-------
Exhibit D
VOA of Ambient Air on Tenax®
NOTE: When a cartridge is not being loaded, a
placed in the loading position.
artridge is
4.3.4.6 Direct nitrogen flow to the side where! th4 Tenax® cartridge
will be loaded and allow the system to equilibrate fbs: ?0 miriuces
before loading cartridges with the generated/te£tv*«j:mosjJhe_res.
4.3.4.7 Divert the nitrogen flow to the
for loading cartridges and insert the Te
chamber.
ate
4.3.4.8 Start the stopwatch and immediately dir
atmospheres gas flow through the ca
4.3.4.9 Calculate the time neede
follows:
t = (G/P) x
NOTE: Base the calculation_only on the compoum
has the highest or lowest
4.3.4.10 At the calculatec
gas flow away from the cartrfts
4.3.4.11 Handling the cartridgeXvit*
and return it to its culture tube>
following informatipiH—-Cl) projectN
followed by a number indicc
date.
4.3.4.12 For
cartridge us
ermeation tube
'pcocks to direct
imwipe®, remove the cartridge
the tube, then label with the
r; (2) standard mixture
of loading; and (3) the
the amount loaded onto a
F2)]
4.3.4.13 Deliver
the quali
permeation tubes to the GC/MS for use in
December, 1991
Page D-27
-------
Exhibit D
VOA of Ambient Air on Tenax®
5 GC/MS ANALYSIS OF VOLATILES FROM TENAX® CARTRIDGES
5.1 Summary
5.1.1 i'nis section includes a description of <.
associated procedures for GC/MS tuning, charact
the GC/MS calibration procedures, and analysisspf
cartridges and QC samples.
lance of
5.1.2 The analytical system is comprised
spectirorr -r set in -he full scan mode.
automatic, repetitive analysis and progr^
target compounds. The Contract Requir
from 1 to 50 ng in the full scan mode
about 5 percent RSD. Concentration of Ixjmpou;
installed calibration table is reported
program.
5.1.3 The relative response factor (RRF) from the carvt^nui^ig calibration
standard analysis is used to calcua
Secondary ion quantitation is allo1
interferences with the primary fon.\ If
performed, document the reasons in. th
secondary ion cannot be substitute
relative response factor is calculat
GC equipped with a mass
up for
data for the
^imits (CRQL) range
precision of
upon a previously
ited data reduction
the sample.
sample
ion quantitation is
SDG tfar/atlvrr--/The area of a
vth)6 airea of a primary ion unless a
ng/the secondary ion.
5.1.4 Quantitation is
mass or primary ion J
selected for each cot
and lack of potentij
Currently used masses
secondary ions.
5.2 Apparatus and
NOTE: Considerable var^i
in terms of instrument coi
responsible/for verif)
results. /Sec>irOfr~6~-4iscu*
be met.
integration >of the SICP of a quantitation
the compound. This mass has been previously
;ed\on its spectral uniqueness, intensity,
knowq/coeluting compounds.
7T-5 for both primary and
iterferenck
ire listd
Table^
rom
ira
that
;es spe
one laboratory to another is expected
Therefore, each laboratory must be
Jieir""i>articular system yields satisfactory
c performance requirements which must
5.2.I/ Sampling/Preconcent^atfipn System
Sample Desorpt/ioW/Injection Unit: Designed for thermally
a Tei}ax® sampl/e cartridge (glass or stainless steel) for
sample t^ansferxAnto/a suitable GC/MS system for analysis. The
configuration of Che thermal desorption unit should permit the
enclosure and f^apid he'ating of the Tenax® cartridge from room
December, 1991
Page D-28
-------
Exhibit D
VOA of Ambient Air on Tenax®
temperature to approximately 250°C while purging with T&u inert gas
(helium) into a cryogenically cooled (liquid nitr/genO trap. The
cryogenically cooled sample must then be rapidly/heared to a
preselected temperature (200-250°C) and a helium ga4 supply allowed to
sweep the sample from the trap onto the gas chromato^isaDhic column. A
schematic diagram of a typical thermal desorption7>'6*lujne of tubing and
must be minimized
helium cat
gas.
5.2.1.3 Sample cartridge: Sampling cas^tridges/consist of 13.5 x 100
mm borosilicate glass with polished-flat end surfaces. One end is
etched with an I (inlet) and the other with alKE (ejJiO- Stainless
steel cartridges (12.7 mm OD x 100 mm long) may aiso bemused. (see
Figure D/VT-1). Cartridges/musTr-~£it-4jjto the thermaTx4esorption unit.
5.2.1.4 Glass fiber filter
5.2.1.5 Forceps.
5.2.1.6 Lint-free tissues: (e.g.\
5.2.1.7 Filter holder: Stainless steNjl
inch diameter fi]
5.2.1.8 Cotto:
5.2.2 GC/MS Sys/em
aluminum (to accommodate 1
nax® cartridges.
5.2.2.1 The G(J)'MS system/should be capable of subambient temperature
programming, exhibrBvunitSaass resolution up to 400 amu, and be
capable of^sr.aoning a J&^300 amu region every second. Equipped with
data sy*£em for ir}»V-1 coating. The GC column inlet should be
to/10°C and subsequently increased rapidly to
is/can be most readily accomplished using a GC
subambient cooling capability (liquid
r approaches such as manually cooling the
December, 1991
Page D-29
-------
Exhibit D
VOA of Ambi en t Air on Tenax®
inlet of the column with a cotton swab containin,
be acceptable.
liquid nitrogen may
5.2.2.3 The specific GC column and temperature program employed will
be dependent on the specific compounds of irrcer/estx,.^ Appropriate
conditions are described in Table D/VT-2. /In /generaT>a nonp-alar
stationary phase (e.g., SE-30, OV-1) temperature-programme^ fromOO to
245°C at 4°/min will be suitable.
5.2.3 Data System
5.2.3.1 GC/MS analysis is based on/a
and relative abundances of target
on the hard disk of the GC/MS co;
identification of each chromatogra:
software that allows searching any
specified mass and plotting such ion abun
number. This type 'of plot is defined as
(SICP). Software must also be available that a
abundance in any SICP between
Also, for the non-target
allows for the comparison o^f simple"
spectra. The 1990 (or more recent) re
of Standards and Technology (NlST^
as the reference library. The db^ta
all data files that have been edi
The retention time
seconds of the library ret
level for relative a6uiJ
percent of the/expected aopniiance*
qualifying te
the analyst J^o determine /the/areas'
compound shj
subjective
problems can
inspection of the^paantit
concentrat
f retention times
lifiers are stored
>plied for
e computer must have
ile for ions of a
rsus time or scan
Current Profile
tegrating the
be
time or scan^vjiumber limits.
be available that
reference library
National Institute
ectral Library shall be used
must be capable of flagging
'nually by laboratory personnel.
to be within ±6
he compound. The acceptance
•ined to be within ± 20
.k that fails any of the
a are manually examined by
for/the flag and whether the
While this adds some
as detect^
analysis, computer generated identification
by an experienced operator. Manual
y.ve results is also performed to verify
acted range.
5.3 Reagents
5.3.1 /Ni/rogen gas: certified 99.995 percent.
5.3,/2 KeJ-ium: certified ^9.9^95 percent, with regulator.
5.3.3 N^at s^aqdards: chemical compounds to be used as standards.
5.3.4 Spectrog5tade mfeOTianol: distilled in glass.
December, 1991
Page D-30
-------
Exhibit D
VOA of Ambient Air on Tenax®
5.3.5 Spectrograde acetone: distilled in glass.
NOTE: Individual chemicals to be used for standard
standards, must have a manufacturer's determined p
better. Purity should be checked by "MR or direc
chemical received by the laboratory is checked b
into a GC, using a 50-m SE-30 WCOT glass capill,
column and FID. The resulting chromatogram is
peaks. If such peaks are observed and amoun
the standard peak, the standard is unacceptable/
5.4 Standards
well as isotopic
>98 percent or
Each
:ion dian alic '.ot
>ondeoHcrossvi inked)
5.4.1 The procedures for the preparation c/f calibration standards are
described in more detail in Section 4./ ThS>s section/presents three
procedures for generating known concervfrisationsv.©/ targeted VOCs for direct
injection into the GC/MS for calibration, &r for deposition on Tenax® for
calibration of the entire GC/MS analytical sys^fe^m. cNpte that direct
injection is allowed only for a continuing calibration standard.) They
are: (1) use of flash vaporization technique for loasd^ng pargeted VOC
standards upon Tenax® tubes; (2$ pre"p~orrstio_nof known concentrations
utilizing static dilution botttesj^-andCS) use~^f—^erjEeation tube system
for generating known concentratrojis\pf\70C-s£andards on/Tenax®.
5.4.2 The Contractor must provide'"all^tajidaj'ds to be used with this
contract. The Contractor must be able tb/ve/ify that the standards are
certified. Manufacturer's' certificates, of Analysis must be retained by
the Contractor and presejteetKupon reques
5.4.3 Neat standard,
weight may be used
the stock solutio:
5.4.4 Alterna
equivalency is
Tenax® may be store
5.4.5
ercent or greater. The
'ate the concentration of
dards may be used if
an EPA audit procedure. Standards on
re than two weeks.
Jards containing the target compounds at
iry stock standards.
.nee Check Standard
concent
d solution of BFB in methanol at a
allow injection of 50 ng of BFB under the
will
December, 1991
Page D-31
-------
Exhibit D
VOA of Ambient Air on Tenax®
5.4.7
solution
every
evaporated.
levels
optimized instrument parameters. Prepare fre
six months, or sooner, if the solution has
5.A.6.2 Calibration Standards
Prepare five calibration standards
for each component as outlined in Tabl
5.4.6.3 Internal Standard Spiking Mixtu/e
Prepare an internal standard spiking mixture^ containing
perf luorotoluene (PFT) , 1,2-dich^oroyenzene-«a4, /knd 1,4-
difluosobenzene at a concentration .chat will allow deposition of
100 ng of each internal standard oathe TanaxBlb~romoe~thajie
1
(LCS)
spiking mixture containing
ene-d4 at a
of 100 ng of each
idges. The amount of
must be the same for all
e spiked onto the sample
Lking Mixture
Containing all of the
sition of 100 ng of each
1,2-dichloropropane
tetrachloroethylene
1,1,2-trichloroethane
trichloroethylene
Cartridges
ge inside the Kimax® tube with a glass wool
'ing transport. For deuterated standards ,
cap with the symbol, "D*".
December, 1991
Page D-32
-------
Exhibit D,
VOA of Ambient Air on Tenax®
NOTE: The scar (*) indicates chat deuterated standards have been
loaded onto the cartridge. This symbol will als
-------
Exhibit D
VOA of Ambient Air on Tenax®
10
.45
000 to A50
10 amu/se
x 100
5.5.3 Mass Spectrometer
Mass range
Scan time
El condition
Mass scan and detector mode
Routine tuning
Preamp sensitivity
Emission current
Electron multiplier voltage
Mass filter
Filter
Total Ion Current sensitivity
Resolution
Display
Response
5.6 Instrumental Analysis
5.6.1 Initial Start-Up
5.6.1.1 Prior to instrument
purge flows (through the desorpt
GC/MS are set at approximately
If applicable, the ipj-eetoj: sweep
5.6.1.2 After t
condition the
range
and
sample analysis, helium
and carrier gas flow to the
and 1-2 mL/min, respectively.
set at 2-4 mL/min.
em Components are assembled,
!nufacturer.
5.6.1.3 The
manufacture
amu, the sc
exceed one
conditions for the
5.6.1.
set -according to the
range should, be from 35 to 300
ye at least five scans per peak and not to
Table D/VT-2 outlines general operating
its tern.
stem has been set up, the user should
idard op^r/ting procedure describing the
instrument being used.
to the mass-flow controllers and set line
gases:
60 psig
40 psig
30 psig
December, 1991
Page D-34
-------
Exhibit D
VQA of Ambient Air on Tenax®
5.6.1.6 Flow rates for the thermal desorption and/GC /system should be
established according to instrument requirements
5.6.1.7 Turn on the master power switch to the^ ch
manitold temperature to 105 ± 5°C, and set sou(rc
temperature to 260°C.
natograph, se:
5.6.1.8 Turn on the power to the thermal desorption unit^and setxthe
temperatures for the valve, trap, and transfer line on the vernier
dials on the control box of the thermal/desorption unit
manufacturer's specification. Typical /values are:
Valves
275°C
Trap
Line
250°C
210°C
5.6.2 Thermal Desorption of Tenax® Adsorbent Tul
5.6.2.1 Initially, the thermal desTrrptienunit is co^ and the Tenax®
cartridges are placed inside whaie^flowing;KeTlra»-£hrough them. This
allows oxygen to be purged Dsom^the trap7 reducing oxidative
degradation of Tenax®. Then,\Juring thji tHermaT"~a^sorption cycle,
helium gas continues to flow through the Cartridge to purge the
organic vapors on the Tenax® intoXthe/liquid nitrogen capillary trap.
5.6.2.2 After the d€gorp€ion has been completed, the six-port valve
is rotated and the'temp_erature on the\apfilary loop is rapidly raised
(greater than 1001°C/minKNthe^ carrier gas tnen introduces the vapors
onto the high resolution Gu columnNsThe apnded-phase fused silica
capillary column jls tempeiyatur>*prograhwad from 40"C (5 min hold) to
240°C at 4°C/toin/and held/at/the up^pe^r 1/mit until all target
compounds ejXate.
5.6.2.3 The column is" programmed to a temperature that will allow the
elution of all of tfeesorgahic compounds while the mass spectrometer is
scanning^—Dataware recorded oy^the computer for subsequent
processing. Quantisation rs^erfibrmed by the' method of relative
responsexfactorS>vWhere the proportionate system responses for analyte
and/stanaard are desermrced prior to the analysis of the sample and
this relative system KfispWse is used to determine the quantity of
compound present on the\ sample cartridge.
hand
device .
or similar
following /outlines typical steps associated with sample
iately prrior to thermal desorption using the NuTech
as a guideline to follow when using this
December, 1991
Page D-35
-------
Exhibit D
VOA of Ambient Air on Tenax®
the desired
5.6.2.4.1 Remove the sealed paint can contai
Tenax® cartridge from the freezer.
NOTE: Use the freezer in the laboratory designated for cartridge
storage ONLY for this purpose. Inadvertenty6frarage "6f containers
of solvent in this freezer will result in contamiha^ion^af all
c rtridges stored in the freezer and wi^ll /compromises-she analysis,
since organic solvents are frequently/^fca^get compounds tox. ^N
quantitative analysis. Verify that/the/laboratory personneINa^r/e
not involved in any process which exposes open containers of
organic solvents, as organic solvent ^apor wLtk. contaminate a
Tenax® cartridge exposed to this/atmosphere /In cmly a few seconds,
thus compromising the quantitative/and/or guaLltative assay.
5.6.2.4.2 Open the sealed lid^iaf the^-pai'ntyCan, using a flat-
bladed screwdriver, beverage can opener, oy other convenient tool
for this purpose.
NOTE: The cartridge will be in a stainless
Teflon-lined screw cap..
5.6.2.4.3 Remove a single
the paint can and replace\in
cap of the desorption
5.6.2.4.4
forceps.
Remove the cartridg<
NOTE: DO NO'
compounds p
compromise
touched,
instrume
with a
e from the~^»aint can. Seal
zer, ^n*~ufelease the Teflon
the shipping tube using
HANDS ! Organic
be sufficient to
rtridge is inadvertently
circumstances in both the
ook.
5.6.2.4.5
chamber .
initiat
cartridge immediately into the desorption
jon cap of the desorption chamber , and
eight-minute desorption cycle. During
owing through the desorption
At the end cSf tfte eight-minute desorption cycle, turn the
unit valve \o the INJECT mode. The following steps are
tic on some commercially available instruments.
Start the <2C temperature program;
In:t
-------
Exhibit D
VOA of Ambient Air on Tenax®
f
5.6.2.5.3 Turn on data acquisition system; ane
5.6.2.5.4 Turn off the trap after it has he^te^C to 250°C.
5.6.2.6 Turn the thermal desorption unit val
remove the Tenax® cartridge. At the end of
recycle and cool to 30°C, and the data
automatically after all compounds have elu
5.6.2.7 Repeat this procedure for each
ax® cartridge.
5.6.2.8 Data from GC/MS runs are normally procea£e-d by the data
system in an automated program which/looates the/compounds of interest
in the data set, quantifies those compounds f017 which calibration data
are available, and prints a report/ A^typicaV^ re/port will present the
quantification parameters and resurts^for tho^se compounds identified
and quantifiable. The report will typrsally li^t those compounds
which were searched for in the sample, indicate wh4^h ones were not
found, print the identifying characteristics and quantification
results for those which were found, and present comment^ for the
operator's benefit, such as/thec?ttetia__which cause
-------
Exhibit D
VOA of Ambient Air on Tenax®
5.6.2.10.4 Peak identification:
5.6.2.10.5 Peak selection:
As determi
laborato
5.6.2.11 The automated procedure begi
two retention time markers (perfluorot^6lui
d4). If the early eluting standard
message is printed and the procedur
eluting internal standard is not fVund
number calculated from the library
a default value.
the
1.S partitioned
er of
attempting to locate the
-dichlorobenzene-
ted, a warning
If only the late
uses the scan
for this standard as
NOTE: Alternatively, the operator may specij
internal standards and then initiate the remainde
procedure. The procedure cycles—through the compound
list attempting to locate
ident?4f
ibers- for the
e automated
in the library
5.6.2.12 If one or more peak;
target compound, the resulting
scans in increasing distance from\th^
The mass spectra in the partitioned^lis
the library entry fop-the^target coi
weighted purity, f£t and r
search for a
partitioned to order the
'cenfter of the search window.
are sequentially compared to
in order to the mass
5.6.2.13 If
the above test;
target is a s/ng
qualitative
group, all
qualitative fi
no peaks are found^
filters,
rs ar
of
fails
person ski
confirmation.
spectrutir'aT!~--the peaiCyfcaximum passes either of
procedure attempSs^tp quantify the peak. If the
compound, yonly^el^e fi?st peak to p'ass the
is inrooessed further. If the target is an isomer
jct/ed b the search are processed through .the
that pass these filters are quantified. If
or pass through the qualitative
is placed in the report.
these criteria does not
absence of the compound in the sample.
orNlow levels of the compound of interest may
,o rail outside of the acceptance range. It is
acceptable values for fit/purity and
questionable identification. If the absence
id is of crucial importance and the DS procedure
•mp^und, manual inspection of the data by a
terpretation of GC/MS data is necessary for
December, 1991
Page D-38
-------
Exhibit D
VOA of Ambient Air on Tenax®
period shall be as
5.8.2 Frequency
5.8.2.1 Prio
standards, t
standard ma:
through the
conditions requ
given in Exhibit E?
5.7 Analytical Sequence
The GC/MS analytical sequence for each 12-hour
follows:
5.7.1 Instrument Performance Check (BFB);
5.7.2 Initial or continuing calibration;
5.7.3 Laboratory Method Blank;
5.7.4 LCS;
5.7.5 Field Blank;
5.7.6 <20 field samples; and
5.7.7 Performance Evaluation (PE) Sample"
5.8 Instrument Performance Check
5.8.1 Summary
Instrument performance chVck\md ma^s ,^tan3afTi£zation of the MS
system is performed according tx> manufacturer's instructions and
relevant information from the user-prepared SOP. The mass calibration
and resolution of the GC/MS system\are (verified by the analysis of the
instrument performapee~ci»ejck standai
pples, blanks, or calibration
that a given GC/MS meets the
'ia. This is accomplished
iromofluorobenzene (BFB). The instrument
acquisition of the BFB mass spectrum are
used for analysis must be checked for performance
twelvexb$'ur period of operation, whichever is
e technical acceptance criteria for BFB as
Also, whenever corrective action which
instrument performance check for BFB (e.g.,
ir, column replacement, etc.), the
ck must be verified immediately irrespective
y performance check requirement.
December, 1991
Page D-39
-------
Exhibit D
VGA of Ambient Air on Tenax®
5.8.3 Procedure
5.8.3.1 Prepare a 25 ng//iL solution of BFB in/me tJ^anol. Prepare
fresh BFB solution every six months or sooner/if the^splution has
degraded or evaporated.
NOTE: The 25 ng/nL concentration is used
volume. The laboratory may prepare a 50,
fiL injection volume is used.
5.8.3.2 Inject 50 ng BFB into the GC/MS.
a 2 /i
solution of
if
5 8-3-3 Set time and parameters fc
initiate data acquisition by foll^
manual.
the acquisition of the data and
rinffxinstructicms in the operator's
5.8.3.4 The instrument parameters (e.g.^iens vlxltages, resolution)
should be adjusted to give the relative ion abundances shown in Table
D/VT-3 as well as acceptable resolution and peaK^ahape^ If these
approximate relative abundances~TraHnat_be achieved/She ion source or
quadrapoles may require cl4anipg^according~~to--«aoufacturer' s
instructions. The Contractor nh^stolTtain the required relative ion
abundances for BFB before pro\eed^ng wi^h ^gample—analysis.
5.8.4 Technical Acceptance Criteria
5.8.4.1 Prior to rt
standards, the Laboratory
the mass spectra/ io/rf*"aBlindai
performance cheyck ^olutior
5.8.4.2 The /nsrument
once at the /beginning o
standards ara^to
rfdrmanbe
-------
Exhibit D
VGA of Ambient Air on Tenax®
5.9 Initial Calibration
5.9.1 Summary
5.9.1.1 Prior to the analysis of samples and/require^blanks and
after the instrument performance check standiird/g/, ion source
cleaning or repair, column\replasement, etcT)7—•or^if the continuing
calibration standard acceptaxice\crite~ria7have not Wen met.
5.9.2.2 If time remains in th£
acceptance criteria for the init
analyzed. If time does not remain^
the acceptance criteria-€^r the ini
sequence shall commence wit
performance stan
5.9.3 Procedure
5.9.3.1 Ve
criteria in
time
.in
analysis
5.9.3.2 The GC
parameter, aqi.ilalent
period after meeting the
ration, samples may be
12-hour period after meeting
alibration, a new analytical
f the instrument
ets the instrument performance
alibra
using temperature and flow rate
in section 5.5.
standards containing all the target
Tenax® tubes as outlined in Section 4 and at
Table D/VT-4. To each of these tubes, add
iternal standards and surrogate standards at
according to section 5.6.
December, 1991
Page D-41
-------
Exhibit D
VOA of Ambient Air on Tenax®
5.9.4 Calculations
NOTE: In the following calculations, the area/response is that of the
primary quantitation ion unless otherwise statfed.
/ r ^
5.9.4.1 Relative Response Factor: Calculate tzne relative "be^ponse
factors (RRF) for each target and surrogate^ compound totfee
appropriate internal standard using the fo^ijTowing equation:
RRF =
EQ. D/VT^-5
where: RRF= relative response
Ax = area of the primar/^ icfe, for tt
measured;
A1S = area of the primary ibH^for'th?
C1S = amount of internal standai
Cx = amount of the compound in
ng
ampound to be
internal standard;
md
tion standard,
;alib
5.9.4.2 Mean Relative Res$ons£^Factor:Caieulatethe mean RRF (RRF)
for each compound by aver aging \he~^7ai«es obtained~§t the five
concentrations using the following equa^ioy^T
EQ. D/VT-6
relative respons fa\tor;
cmpound; a
5.9.4.2.1
from the
surrogate
ation (%RSD): Using the RRFs
the XRSD for all target and
following equations:
EQ. D/VT-7
RRF
EQ. D/VT-8
Ward deviation of initial response factors
(p/e"r compound);
jlative response factor at a concentration
Level; and
mean of initial RRFs (per compound).
December, 1991
Page D-42
-------
Exhibit D
VOA of Ambient Air on Tenax®
5.9.4.3 Relative Retention Times (RRT): Calculate tjie RRTs for each
target and surrogate compound over the initial calibration range using
the following equation:
RRT =
RT,
EQ. D/VT-9
is
where: RTC = retention time of the targfe^ fa surrogateXc^pmpolmd;
and
RTIS — retention time of the ijtfter/nal standard.
25.9.4.4 Mean of the Relative Retention/Times (BSS^: Calculate the
mean of the relative retention times/(R^T) for riach7analyte target and
surrogate compound over the initia}/ cayLibratiop range using the
following equation:
RRT =
RRT
n
EQ. D/VT-10
where: RRT = mean relatiyeretention time for^fche target or
surrogate orimpouna—§«t_each initial oaQ.ibration
standard;
RRT -= relative retention tiBe—jfor^^the target or surrogate
compound at e\ch
5.9.4.5 Tabulate the area response lf) /6f the primary ion (see Table
D/VT-5) and the corresponding concentration for each compound and
internal standard.
5.9.4.6 Mean Ar/a Re'spolvse \t) for Int*
mean area respc
initial calibi
fo
range/usir
jrnar
Jthe
n
Standard: Calculate the
'andard compound over the
equation:
EQ.. D/VT-11
where: Y -
mearv^area
.area
irnal
>tanoaxd.
Percent Area\Res
ich/calibration level\
;ing equation:
ce^sponse; and
the primary quantitation ion for the
for each initial calibration
onse .Change (%ARC): Calculate the %ARC at
each of the internal standards using the
December, 1991
Page D-43
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Exhibit D
VOA of Ambient Air on Tenax®
A - 7
X 100
EQ. D/VT-12
where:
%ARC
percent area response
area response of the
concentration level;
mean area response
the entire calibratio.
where: RT = mean retention time; and
RT - retention time for the internal^
initial calfBtstionstandard.
er
5.9.4.8 Mean of the Retention Times /RT)/ For Internal Standard:
Calculate the mean retention time (RJT) for each/internal standard over
the initial calibration range using/th^ following^equation:
EQ. D/VT-13
for each
5.9.4.9 Internal Standard R\ten^ISn~Tiae Shift (RT37: Calculate the
RTS between the RT of each internal staiwiarQ^at—fcaSn concentration
level and the RT for that inteisnalXstajidal'a over the entire
calibration range using the follte>wing/ej.nternal standard at a
roncentrajCion/''Ie\
5.9.4.10 Tabulatexjjeak/height or area responses against concentration
for each compound anoSant/rnal standard. Table D/VT-5 contains
primary quantitative ionsv^p be used for each target and surrogate
compound ajnd_internaFvs^andai
5.9.4/11 iafcaijial standard r&sp/nses and retention times in all
standards must bes*evalu^ted during or immediately after data
acquis/tion.
5.9 '
jchnical Acceptance Criiteria
5.>x5.1 >11 initial oalipration standards must be analyzed at the
concervt^tiorN^evels/and/frequency described in this section on a
GC/MS sysbsm meet
BFB instrument performance check criteria.
December, 1991
Page D-44
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Exhibit D
VOA of Ambient Air on Tenax®
5.9.5.2 The %RSD for all target and surrogate compounds in the
initial curve must be less than or equal to 30.0/per/cent. Up to two
compounds may exceed the maximum %RSD criteria;/the^ ZRSD for those
compounds, however, must not exceed 40.0 percent.
5.9.5.3 The RRT for each of the target and,
each calibration level must be within ±0.0$
relative retention time (RRT) for the co:
5.9.5.4 The %ARC at each calibration
of the mean area response (Y) over th
each internal standard.
5.9.5.5 The retention time shift Ifor
at each calibration level must be/wit
mean retention time (RT) over the
internal standard.
5.9.6 Corrective Action
he/internal standards
seconds compared to the
ation range for each
5.9.6.4 If the
not met, inspect
clean the^-lon .japurce ,
actio
urroeate compounds at
units^er. the^snean
ve* must be within ±40
inftial calibration range for
5.9.6.1 If the retention
more than 20 seconds from
calibration range, the chroi
malfunctions, and corrections"
5.9.6.2 If the %RSD of the RRFs
±30.0 percent, initial calibration
is within the QC li
5.9.6.3 If the
percent of the
spectrometric
made as appr
corrective
internal stanSifrd changes by
entire
must pe. inspected for
ic/initial curve is not within
wiards are rerun until the %RSD
tandard is not within 40
a (Y), the mass
r malfunction and corrections
Narrative all inspection and
alibration technical acceptance criteria are
for problems. It may be necessary to
e column, or take other corrective
technical acceptance criteria.
£ion acceptance criteria MUST be met before
ance evaluation (PE) samples, or required
samples or required blanks analyzed when
ia have not been met will require analysis
ank cartridges (if available) at no
[ency .
December, 1991
Page D-45
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Exhibit D
VOA of Ambient Air on Tenax®
Results of the
srnal standard
5.9.7 Documentation
Reporting requirements are listed in Exhibit
initial calibration are reported on Form V-AA'
area and RT shall be tabulated on Form VII-
5.10 Continuing Calibration
5.10.1 Summary
5.10.1.1 Prior to the analysis of Camples and/beguired blanks and
after tuning criteria have been met,/thar initial; calibration of each
GC/MS system must be routinely chec/fced/by analyzing a continuing
calibration standard to ensure that th^^instrXuneift: continues to meet
the instrument sensitivity and linearityTfe^q»ir^nents of the method.
5.10.1.2 The continuing calibration standard,
(CAL 3) standard, shall contain all the target
compounds, and internal standards.
5.10.1.3 All sample results
from the continuing calibra
is the mid level
ds, surrogate
the RRFs obtained
5.10.2 Frequency
5.10.2.1 A check of the calibrators
every 12 hours on a^JJG/HS^system thl
5.10.2.2 The cotfti
injection of tb
criteria for B,
analyzed.
5 .10. 3 Procedu:
e must be performed once
met the tuning criteria.
e starts with the
meets the ion abundance
ibration standard may be
Analyze the
met the tuningand ma
proceduafeunderThsjrrumeri
5.10.4
In the followin
ry quantitation i
tandard (CAL 3) in a GC/MS system that has
tion criteria following the same
sis, section 5.6.
calculations, the area response is that of the
less otherwise stated.
5 . lOvA. 1 Relative Reapo
respons^factb^: (RRF/ f
equation
e Factor (RRF): Calculate a relative
each target compound and surrogate using the
'.4.1.
December, 1991
Page D-46
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Exhibit D
VOA of Ambient Air on Tenax®
5. 10. A. 2 Percent Difference (%D) : Calculate the pferoknt difference
in the RRF of the daily RRF (12 -hour) compared to/the/mean RRF in the
most recent initial calibration. Calculate the /D for each target and
surrogate compound using the following equatior
RRF. -
%£> = -
D/VT-15
where: %D
RRF,.
RRF,
percent difference;
RRF of the compound in
standard; and
mean RRF of the compound
calibration.
5.10.5 Technical Acceptance Criteria
5.10.5.1 The continuing calibration standard
concentration level and frequency describeJKin
system meeting the BFB instrument performance
ist be analyzed at the
section on a GC/MS
leek criteria.
5.10.5.2 The %D for each t4rgef~ltni~6ucroga.te compoxhwd RRF in a
continuing calibration sequenc^-nmstbe witKltr-^XLO percent of the
initial calibration mean RRFxin^order^tD^proceed wiph the analysis of
samples and blanks. Up to two. compound^ may excSBn the maximum %D
criteria; the %D for those compounds^, Jaow^ver, must not exceed 40.0
percent.
5.10.5.3 Corrective Acl
\ V /
5.10.5.4 If the/ret
more than 20 seconds from
standard, the /hrotaatograpj
malfunctions ,/ana correct
ne _for anyxintarnal standard changes by
contijming (12-hour) calibration
lie systemsmuat be inspected for
required.
5.10.5.5 Ir"-the canj^inuing calibration technical acceptance "criteria
are not met, ins>^ct the ^system for problems. It may be necessary to
clean the ion sourcevchange the column, or take other corrective
actions tp—«e-et^the contcmuingx^alibration technical acceptance
criterj
/—-\ x
^.bration acceptance criteria MUST be met
performance evaluation (PE) samples, or
d. Any samples or required blanks analyzed
tion criteria have not been met will
•nal sample or blank cartridges (if
1 cost to the Agency.
December, 1991
Page D-47
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Exhibit D
VOA of Ambient Air on Tenax®
5.10.6 Documentation
Reporting requirements are listed in Exhibvfc B/ Results of the
continuing calibration are reported on Form V)/-AAVT;\Jnternal
standard area and RT shall be tabulated on Fe
5.11 Blank Analysis
5.11.1 Summary
5.11.1.1 To monitor for possible lab^rat/fery con&Smination, laboratory
method blanks are analyzed with each/SDC? at leasr once in a 12-hour
analytical sequence. All steps in /che/analyticral /procedure are
performed on the blank using all r/eageTi^s, standards, equipment,
apparatus, glassware, and solvents^th^at wlnt^/a by used for a sample
analysis.
5.11.1.2 A field blank is designed to detec^x^otenbial sample
contamination during the handling and shipping pr^xcess^of a field
sample. The Tenax® cartridg'e~u5e-d-as__afield blank^isyst be associated
with the actual sampling process^; therefore-;—dogblank cartridge is
opened with the other cartrldges^re^ealfid, and carried through the
same handling process as thos\ used to samtf/le~~~aTnb-i«it air.
5.11.1.3 A laboratory method bl>
Tenax® that has not left the
spiked with the same^ameunt of surrc
standard and carriea throujs
sample.
5.11.1.4 The
sample is ad
with associ
is an unused, certified
The blank cartridge is
compounds and internal
tical procedure as a field
tandards that are added to each
samples must be analyzed
5.11.2 Frequency
5.11.2.1
field
shal
zed once per sample delivery group. A
g with each batch of <20 samples and
re analytical procedure.
bex analyzed after the calibration standard(s)
\lyzed.
ally concentrated sample is encountered, an
ormed immediately after the sample analysis.
ank cartridges with the same amount of internal
December, 1991
Page D-48
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Exhibit D
VOA of Ambient Air on Tenax®
standards and surrogate compounds and using the s
as the field samples.
5.11.3.2 Analyze the blanks following the sam;
under section 5.13, "Sample Analysis".
5.11.4 CaIculations
piking technique
edure outlined
The blanks are analyzed similar to a/ff&ld sample and
equations in section 5.13.4 apply. / /
5.11.5 Technical Acceptance Criteria
NOTE: If the most recent valid cal/brtion is
internal standard area responses and RTSsin
against the corresponding internal
the mid level (CAL 3) standard of the initial
initial calibration,
lank are evaluated
re/L responses and RTs in
libration.
5.11.5.1 All blanks must be analyzed at the fteauerifcy^described in
section 5.11.2 on a GC/MS sYS£emmeeting the BFB instrument
performance check and initi/al caTiBraeioji^or continuing calibration
technical acceptance critei
5.11.5.2 The percent recover
the blanks must be between 80
5.11.5.3 The area response for eac
±40 percent of areaxfelp&nse of the
calibration.
the surrogate compounds in
ient.
tin the blank must be within
the most recent valid
5.11.5.4 The
be within ±20.
calibration.
Jterition time Tor ea^sh of \ne internal standards must
seconds between—the bTsml^ and the most recent valid
5.11.5.5 TheNjlank^auyt n6t contain any target analyte at a
concentration grfe«^ter than its CRQL and must not contain additional
compounds with elutbsn characteristics and mass spectral features that
would inperfHre-^ith idfeRtific^ion and measurement of a method
analyt^at its CRQt^ The to^l |tevel of analytes in the blank other
than/the/s'urroga>6£s arH internal/standards must not exceed 10 ng.
5.11.6,
syste
ensure t1
reagents, g
blanks do not meet the technical
'ontractor must consider the analytical
1. It is the Contractor's responsibility to
erences caused by contaminants in solvents,
other sample storage and processing hardware
December, 1991
Page D-49
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Exhibit D
VOA of Ambient Air on Tenax®
ines in gas
problem, the
.d appropriate
;e further sample
ol
that lead to discrete artifacts and/or elevated
chromatograms be eliminated. If contamination
source of the contamination must be investigate
corrective measures MUST be taken and documer
analysis proceeds.
5.11.6.2 All samples processed with a
(i.e., contaminated) shall be flagged wit
5.11.7 Documentation
Reporting requirements are listed ii( Exhibitf B7 Blank results are
reported on Form I-AAVT. and the associated sajfiple4 are summarized on
Form II-AAVT. Internal standard a4easa,nd RT jfihajfl. be tabulated on
Form VII-AAVT.
5.12 Laboratory Control Samples (LCS)
5.12.1 Summary
ntrol sample designed
the analytical
ts the LCS
5.12.
The LCS is an internal^la'
to assess the capability or\th
method listed in this Exhibi
compounds.
5.12.2 Frequency
. The LCS must
sequence, and co;
5.12.3 Procedure
5.12.3.1 P
at a concen'
5.4.6.5, and t!
of 100 ng each
blanks.
once per 12-hour analytical
in the SDG.
itaining all the LCS compounds
for each compound according to section
and internal standards at a concentration
ne spiking technique as the samples and
ng the same procedure described in
dual compound recoveries of the LCS using
December, 1991
Page D-50
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Exhibit D
VOA of Ambient Air on Tenax®
LCS % .Recovery
Concert Cra tion
reported
Concentzation
x 1,
spited
5.12.A.2 Field sample calculations in sectio
LCS in monitoring the area and retention tim<
standards.
5.12.5 Technical Acceptance Criteria
NOTE: If the most recent valid calibr^
internal standard area responses and
against the corresponding internal
the mid level (CAL 3) standard of
5.12.5.1 The LCS must be analyzed""
initial or continuing calibration, and
criteria at the frequency described in sect
5.12.5.2 The percent recove,
the LCS must be between 80
5.12.5.3 The percent recove*
within the percent recovery
EQ. D/VT-16
apply to the
e internal
5.12.6 Correcti,
5.12.6.1 If
standards are not mi
It may beja»&»ssary to
corrective
crit
of each of the su
is an initial calibration,
rare evaluated
iponses and RTs in
ration.
system meeting the BFB,
£hnical acceptance
.2.
;ate? compounds in
mpounds must be
tent.
5.12.5.4 The area response chan
valid calibration for each of the
±40 percent.
5.12.5.5 The repfen
valid calibrati
±20.0 seconds.
n the LCS and the most recent
,al standards must -be within
;he LCS and the most recent
standards must be within
acceptance criteria for the internal
calculations and instrument performance.
the instrument or take other
et the technical acceptance
lay not submit data from an SDG until all the
iteria are met. LCS contamination from
,CS analyzed not meeting all the technical
quire analysis of additional LCS cartridges
:he Agency.
criteria MUST be met before any field
December, 1991
Page D-51
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Exhibit D
VOA of Ambient Air on Tenax®
samples, performance evaluation (PE) samples, oryfeqt/ired blanks are
analyzed. Any samples or required blanks analyzed ichen the LCS
technical acceptance criteria have not been met/wiO require analysis
of additional LCS cartridges at no additional/cost tb\the Agency.
/ /^ -
5.12.7 Documentation
Reporting requirements are listed in
Control Sample analysis data are report
standard area and RT shall be tabulate
5.13 Sample Analysis
5.13.1 Summary
Prior to the analysis of samples,^Bhe appropriate GC/MS operating
conditions are established, instrument pefc£prmarl&e check standard is
analyzed, and the GC/MS system is calibrated>xThe eantents of the
sample cartridge is desorbed, preconcentrated, ahd subsequently
analyzed by GC/MS under condTEiitms—in__section 5.5. ^Sy/ldelines for
qualitative and quantitative analysis are~"TJi*eu&sed in sections 5.14
and 5.15.
bit B. Labora
on Form III-AAVT. In
Form VII-AAVT.
5.13.2 Frequency
5.13.2.1 If time remains in the
calibration is perforjuesLsamples
a continuing calibration sbandard.
period in which an initial
analyzed without analysis of
5.13.2.2 If time cjoes no
injection of tne itistrume
initial calibration is p
check standard apd the
analyzed bei
5.13.3 Procedure
n theM/-hour period since the
performafcs^check standard in which an
foi?med7v'both ^He instrument performance
ntirming caTiferation standard must be
na£ysis may begin.
5.13. 3-i^ Analyze^ftamplesNinder
section 5^-5—and^accor^j1^ to
outl/lne0 in sectichi 5.i
iie instrument conditions provided in
'GC/MS instrumental analysis procedure
5/13./G.2 Upon introduction of the cryofocused sample onto the column,
JC/MS system is opara
mge r*^m 35 to 300 amu.
chromatogY&£hic peak gnoi
identific.
library spS
so that the MS scans the atomic mass
At least five scans per eluting
Ld be acquired. Scanning allows
compounds in the sample through searching of
December, 1991
Page D-52
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Exhibit D
VOA of Ambient Air on Tenax®
5.13.3.3 Each analytical run must be checked for /saturation. The
level at which an individual compound will saturate /he detection
system is a function of the overall system sensitivity and the mass
spectral characteristics of that compound. Wh^n aCsample is analyzed
that has saturated ions from a compound, this/analysrsxmust be
followed by a blank analysis. If the blank .analysis is nc^t free of
interferences, the system must be decontaminated. Sample arta^ysis may
not resume until a blank analyzed is founc
interferences.
5.13.3.4 Secondary ion quantitation
sample matrix interferences with the
quantitation is performed, document/the/reasons/
5.13.4 Calculations
5.13.4.1 The equation below is used fb^calcu^ating concentrations.
EQ. D/VT-17
where: Xa -
aowed only when there are
rmary ion/Xlf secondary ion
he SDG Narrative
compound
area of the
measured;
area of the ch
internal
amount of the
5.13.4.2 Su
percent rec
e compound to be
ion for the specific
'standard spiked into the
om the analysis of the
rd or the mid level (CAL
calibration.
): Calculate the surrogate
tion:
EQ. D/VT-18
I-—-—_., —^ermihed by analysis, ng; and
juanrvty addeJisjro sample/blank, ng.
^sponse Change (%ARC): Calculate the change
jinternal standard by comparing with the most
sing the following equation:
December, 1991
Page D-53
-------
Exhibit D
VOA of Ambient Air on Tenax®
- A
where:
%ARC
AC
percent area
area response
calibration
area response
X 100
response
of the,
and
of
EQ. D/VT-19
valid
5.13.4.4 Internal Standard Retention
shift in retention time between the
recent valid calibration standard
using the following equation:
RTS = RT,
20
where: RTC -
retention time of
calibration; and
retention time of
RT =
5.13.5 Technical Acceptance
NOTE: If the most recent va'
internal standard area respons
against the corresponding inte
the mid level (CAL 3) standard of'
5.13.5.1 The fie^sample
the BFB tuning, /mi
technical acce
5.13.2.
.nitial calibration,
syin the sample are evaluated
.rd area responses and RTs in
calibration.
on a GC/MS system meeting
.tinuing calibration
incy described in section
5.13.5.2
±20.0 second
most recent va"
5.13.5.3
±40
5.1,
ho.
pe
5.13.5.6
the sample mu
internal standard must be within
time of the internal standard in the
the internal standards must be within
calibration.
t be desorbed and analyzed within the contract
jhave a laboratory method blank meeting the
criteria of less than 10 ng of total VOCs
recovery of each of the surrogate compounds in
«7een 80 and 120 percent.
December, 1991
Page D-54
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Exhibit D
VOA of Ambient Air on Tenax®
5.13.5.7 All target compound concentrations must/hot/exceed the upper
limit of the initial calibration range and no compound ion (excluding
the compound peaks in the solvent front) may sajaira>ce the detector.
5.13.6 Corrective Action
5.13.6.1 If the on-column concentration oi
exceeds the initial calibration range,
that are out of range.
any compoufjo. in Smv sample
fsults for the comrftaunds
5.13.6.2 Internal standard responses ,and/retention times must be
evaluated during or immediately after/da/a acqui^Tfcion. If the
retention time for any internal stantiarel change/ bymore than 20
seconds (0.33 minutes) from the latrest/continuAng/(12-hour)
calibration standard or mid level ACAL>i) standa/d if samples are
analyzed in an initial calibration analytbs^l sequence, the GC/MS
system must be inspected for malfunctions, and^corrections made as
required.
5.13.6.3 If the SICP area
than ±40 percent between th samp]
calibration, the GC/MS system
corrections made as appropriate":
internal stand^d changes by more
the most recent valid
be inspec£e~d--€a£_malfunction and
5 . 13 . 6 . 4 When target compounds
quantitation limits (CRQL) , but
criteria, report the concentration
CRQL is 5 ng and a jeotlcetrtration of
"2J."
witt
ng
acceptance criteria.
contract required
ra meet the identification
a "J." For example, if the
is calculated, report as
5.13.6.5 If t
surrogates and' i
surrogate and' i
It may be nf[ces
corrective
standard technic"
5.13.6.6
to hayi
and
the,
5.13.7 DoculB«itat
Reporting
;hri"ical"^cepta\>ce criteria for the
•kers-are nbfe-aiet, check calculations,
'andard solv±ioitfs, and instrument performance.
'ecaXibrate the instrument or take other
s to meet the surrogate and internal
e^ds to analyze more than one (1) sample
comp^aunds^within the initial calibration range
d ions^ncft saturating the detector (excluding
front), contact Sample Management Office
he Region for instructions.
:Ot meet technical acceptance criteria must
tents are listed in Exhibit B. Sample analysis
December, 1991
Page D-55
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Exhibit D
VOA of Ambient Air on Tenax®
data are reported on Form I-AAVT;
be tabulated on Form VI I-AAVT.
5 . 14 Performance Evaluation Samples
5 . 14 . 1 Summary
Internal stand/rd /area and RT shall
the
5.14.1.1 The performance evaluation (PE) /s«Brples will assisT
Agency in monitoring Contractor performance/ The laboratory
be informed as to which compounds are cyonta/ined in the PE samples or
the concentrations.
5.14.1.2 The laboratory will receiyi R£ samples' otC Tenax® adsorbent
tubes from the Agency. The sample^ will come dritn instructions
concerning the desorption procedure\requir^d/f or/the PE samples . Add
internal standards and surrogate compobqds to t^ie PE sample, following
procedures in Section 4.
5.14.1.3 In addition to complying with the PE saw^le ^fcchnical
acceptance criteria, the lab'SrattH-y.jgill be responsibJ^i for correctly
identifying the quantifying^ the
-------
Exhibit D
VOA of Ambient Air on Tenax®
5.14.5.2 The PE sample must be analyzed with a me
the blank technical acceptance criteria.
5.14.5.3 The percent recovery of each of the
the sample must be between 80 and 120 percent
5.14.5.4 The retention time for each inte
sample analysis must be within ±20.0 secon
the internal standard in the most recent
5.14.5.5 The %ARC for each of the
analysis must be within ±40 percent
calibration.
5.14.5.6 The results of analysis
provided in the performance evaluatl
and accuracy criteria in comparison wit
outlined in Section 6.
5.14.6 Corrective Action
5.14.6.1 If the PE sample
internal standard and surrogS
standard solutions and insti
recalibrate the instrument or take \th0r
to meet the technical acceptance\riteri/.
blank that met
standards in the PE sample
t valid
e target compounds
must meet precision
results, as
eria for the
alculations,
tay be necessary to
action procedures
5.14.6.2 If duplic
PE sample must be
met. If after r
standards are ijtsi
first analysis
laboratory.
within the
and must be
E samples are provided, the
criteria are not
the RTs for all internal
en the problem with the
within the control of the
from the analysis with SICPs
sidered the initial analysis
on all data deliverables.
5.14.6.3 If the relraalysfSxpf the PE sample does not solve the
problem, i-^e-r-r-J^ie SICP^areas^ar internal standard RTs are outside the
contract limits for-vboth aha^-vse^, then submit the SICP data and
sample dacS" trdTJKbotn^^nalyse&x/Distinguish between the initial
analysis; and the re^analysis on all data deliverables, using the sample
sufifix/es specified in\ExtvLbit B. Document in the SDG Narrative all
ivfepe/ction and corrective kctions taken.
\ )
no other FE Sykmple cartridges are provided for
the' results after flagging the data as required.
)G /narrative, if necessary.
December, 1991
Page D-57
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Exhibit D
VOA of Ambient Air on Tenax®
5.14.6.5 In addition to complying with the PE sample7 technical
acceptance criteria, the Contractor will be responsible for correctly
identifying the compounds included in the PE sample^. The Agency will
notify the Contractor of unacceptable performs
5.14.6.6 If the PE sample is provided witl
technical acceptance criteria MUST be met
reported. Also, the Contractor must demc
performance for compound identification/an<
Contractor fails to meet the PE sample/te<
the Agency may take, but is not limit/d
reduction of the number of samples,
site visit, a full data audit, and/<
analyze a remedial PE sample, and^or
Cure Notice.
5.14.7 Documentation
Reporting requirements are listed in Exhibit
data are reported on Form
be tabulated on Form VIl-j
5.15 Qualitative Analysis
SDG, "PEsamj
sample ota^a ar*
;rate acceptable
quantification.
inical acceptance criteria,
•wing actions:
Lmple shipment,
.aboratory to
such as a
tple analysis
ea and RT shall
5.15.1 Target Compounds
5.15.1.1 The compounds-ij^ted in tf
Exhibit C and in Table D/VT\1
an analyst competent
Responsibility «aniple component and standard component
(pXimary and secondary ion identification).
correspondence of the GC relative retention
onent RRT must compare within ±0.06 RRT
ndard component. For reference, the
run ita tfte same 12-hour time period as the sample.
inteyfemng components prohibits accurate assignment
com>Q/ent/RRT from the total ion chromatogram , the RRT
sing SICPs for ions unique to the component of
December, 1991
Page D-58
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Exhibit D
VOA of Ambient Air on Tenax®
interest.
5.15.1.4 For comparison of standard and sampl
spectra, mass spectra obtained on the Contract
Once obtained, these standard spectra mav
purposes only if the Contractor's GC/MS meet
performance requirements for BFB. These s
obtained from the run used to obtain refer
required.
5.15.1.5 The requirements for qualitat^
of mass spectra are as follows:
re Xrerification by compaJsi/on
Sarg mass si
All ions present in the sta
intensity greater than 10 ^erc/nt (mos/ a
spectrum equals 100 perce
spectrum;
mt
resent
a at a relative
indant ion in the
in the sample
The relative intensities of such i~
percent between the standard and samp
For an ion with an ab_undance of 50 percerf
spectra, the corre
and 70 percent) ;
e abundance
agree within ±20
spectra. (Examp1e:
in the standard
t be between 30
For each internal sta
in the sample extract h\s
percent from the area me
continuing calibration
from the mea«-area measured
either criterion is
improve
ot met,
2 me
the area measured
hanged by greater than 40
measured during the most recent
che\Jc or/by greater than 50 percent
initial calibration. If
al action must be taken to
.uri
,he sample spectrum but not
must be considered and
ing the comparison. All
:he identification criteria must be reported
For all compounds below the CRQL report
lowed by a "J", e.g., "3J."
verified by all of the above
dgement of the mass spectral
intrpretation speb-i^lis^ the identification is correct, then the
Coiitraetor shall report chat identification and proceed with
lantzlf ication.
5.15.2/1\A lib^ry
componentsTxy: the^pu
shall be executed for non- target sample
fose of tentative identification. For this
December, 1991
Page D-59
-------
Exhibit D
VOA of Ambient Air on Tenax®
purpose, the 1990 (or more recent) release of the/NIST Library,
containing 50,000 spectra, shall be used. Computer/generated library
search routines must not use normalization rouclne^that would
misrepresent the library or unknown spectra wWen compared to each
other. Up to 10 organic compounds of greate
not listed in Exhibit 0 shall be tentative
search of the NIST Library. Only after
spectra with the nearest library
interpretation specialist assign a
ncentration
forward
searche
comparisor
the mass spe^E^al
identification.
?le
5.15.2.2 Guidelines For Making Tenta,
Relative intensities of ma
(ions greater than 10 per
be present in the sample
The relative intensities of the
±20 percent. (Example: For an ion
percent of the standard spectra, the coi
abundance must be
Cation:
eference spectrum
abundant ion) should
should agree within
an^>abundance of 50
sponging sample ion
Molecular ions pres«
in sample spectrum;
Ions present in the sample
spectrum should be reviews
contaminatioja-e¥;4.d bevs^ported as unknown. The mass spectral
specialist should^give aaftitioristi classification of'the unknown
compound Jtf^p^&sibleXi.e., unknown aromatic, unknown hydrocarbon,
jrown/chlorinatexl compound). If probable molecular weights can be
distinguished, include them.
-------
Exhibit D
VOA of Ambient Air on Tenax®
located correctly. If the compound identification is
ct, the
computer then performs the quantitative calculation using?' the method of
relative response factors. Data are reported as ng yor yig/tube (since the
entire contents of the tube is introduced into the JGC/nS system, and can
be subsequently converted to ng/m3 if the volume or air sampled is known
to the laboratory.
5.16.1 Target Compound Quantitation
5.16.1.1 Sample quantitation is performed tfy the data
system for all desired ions of all target /compounds. Target compounds
are quantified according to the following/equation
processing
X, ng/m3' =
where: X - target compound air cor
AX - area of ion of analyte,
ngls - mass of internal standard appl
As - area of standard,
RRF = relative re;
V0 - volume of
If the volume of air sampled b
equation becomes:
EQ. D/VT-21
5.16.1.2 The coi
scan number, ti:
5.16.1.3 St
be evaluated
retention ti:
the latest
system must be insp
required-^JXhe—SICP of
evaluat^a for eacn^sample
oratory, the above
EQ. D/VT-22
int) out peak number, m/e,
area and amount.
rfn times in all standards must
data acquisition. If the
ird changes by more than 30 seconds from
lour) calibration, the chromatographic
malfunctions, and corrections made as
il standards must be monitored and
If the SICP area for any
intertfal^CanaarcLcharJges by rt&rX than 40 percent, the mass
speccronretric system,.musX; be inspected for malfunction and corrections
made a.z appropriate. NWhert corrections are made, reanalysis of
duplicate samples analyped\while the system was malfunctioning is
*eces-sary.
5.16.2 ^Risn-Tar^t Compound Qtfantitation
5.16.2.1 Ah\estima*ed /Concentration for non-target components
December, 1991
Page D-61
-------
Exhibit D
VOA of Ambient Air on Tenax®
tentatively identified shall be quantified by the/standard method.
The nearest internal standard free of interferences/shall be used.
5.16.2.2 The formula for calculating concentffations^isthe same as in
section 5.16.1.1. Total area counts (or peal/he/Cgi^ts) fTS^m the total
ion chromatograms are to be used for both ttfe compourJii to
and the standard. A relative response fact^or/(RRF) of ohe (IjHs to
be assumed. The value from this quantita£i>op shall be qualtfej^ed a*
estimated (i.e., flagged "J"). This estimated concentration snoHld7be
calculated for all tentatively identifyed ^compounds as well as those
identified as unknowns.
5.16.2.3 An estimated concentrations sh(buld be /calculated for all
tentatively identified compounds as wesLl as tWose/identified as
unknowns. This estimated concentration must/oe^alculated for all
tentatively identified compounds as we^ij. as thg4e identified as
unknowns.
December, 1991
Page D-62
-------
Exhibit D
VGA of Ambient Air on Tenax®
LITY FOR THE
6 PERFORMANCE REQUIREMENTS FOR DEMONSTRATING METHOD ACCE^TA
ANALYSIS OF AMBIENT AIR
6.1 Summary
6.1.1 Although this method describes the GC/MS
compounds collected on Tenax®, collection on ottfer/adsorbents isX.
acceptable if the performance criteria describedifn this section areNqet.
Specifically, the analyst must demonstrate tha~tN:ollection on an^iternVt
solid adsorbent and subsequent GC/MS analysjte poduce results meeting
these general criteria:
Minimum contract required quanti^at^n limits (X^RQL) listed in
Table D/VT-1;
Replicate precision within 30 percent
Audit accuracy of 30 percent* for targ&t^compbund concentrations
normally expected in ambient air.
* Exceptions are carbon tetra/dhlorTc
which higher audit accuracies
, 1 -trichlol?6ethane, for
3orteo~irT-the-4ISEPA TAMs study.
6.1.2 These criteria were establi>she^susing/historical' data from the
application of TO-10 methodology toNsampleifi from the Toxics Air Monitoring
System (TAMs) and the Urban Air ToxicSt Monit/ring Program (UATMP). The
primary reason to base the acceptability of/analysis method on performance
is to allow systems curr^nTTy-vbeing used\for\the analysis of VOCs in water
to be used for VOCs in/air. Solutions ratt\er\han compressed gas
standards may be used'for^catibration. However/ audit standards must be
humidified gas standards, to mast^clo~se^y res^prfble the air matrix.
Details for the dejfernanation 0f each ofrhe_criteria follow.
6.2 Minimum Contract Ret
/itation Lifiits (CRQL)
The minimum
replicate measurements
the expected jtoeee^ioji linul
seven re
Student's/
CO
6 . 3 Repli
by each laboratory by making seven
.entration of the compound of interest near
:andard deviation computed for the
ind tihis value multiplied by 3.14 (the
•cent confidence for 7 values).
the
relat
There are1
measurement.
effect on the p
ed for this program is the unsigned
'licate measurements of the same sample.
may affect the quoted precision of the
:he compound of interest itself may have some
as the observation that styrene generally
December, 1991
Page D-63
-------
Exhibit D
VOA
Ambient Air on Tenax®
shows slightly poorer precision than the bulk of nonpo/lar/VOCs. The
primary influence on precision is the concentration Leve/ of the compound
of interest in the sample, i.e., the percent relative standard deviation
for a set of replicate values degrades as the concentration approaches the
detection limit. A conservative measure of preciSion^Vas otvfcaj.ned from
replicate analysis of Tenax® samples from the TAJls tfetworfcx. Thrs^is the
source for the 30 percent figure of merit for overall replica^ precision
given above.
6.4 Audit Accuracy
Audit Bias is defined as the relative/difference/between the
measurement result and the nominal concentration of/the/audit spiked
compound, i.e., [(True - Found x lOOJ/Truev. Audi/standards will be
supplied to the participating iboratori^s, the^se/audlt standards
analyzed, and the results judged against cr-iteria ba4ed on historical
data.
December, 1991
Page D-64
-------
Exhibit D
VGA of Ambient Air on Tenax®
Compound
Table D/VT-1
Target Compound List for Volatiles Collected or
and Contract Required Quantitation Limit
CAS RN
75-6
104-51-8
56-23-5
108-90-7
Benzaldehyde
Benzene
Benzonitrile
Bromobenzene
Bromochloromethane
l-Bromo-3-chloropropane
Bromoethane
Bromotrichloromethane
n-Butylbenzene
Carbon Tetrachloride
Chlorobenzene
2 -Chlorobutane
l-Chloro-2,3-epoxypropane
2-Chloroethoxyethene
Chloroform
1-Chloropropane
2 -Chloropropane
3-Chloro-l-propene
m-Chlorotoluene
o-Chlorotoluene
p-Chlorotoluene
1,2-Dibromoethane
D ib romome thane
1,2-Dibromopropane
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,3-Dichlorobutane
1,4 -Dichlorobutani
2,3-Dichlorobutine
c is -1,4 -Dichl^ro-
3,4-Dichlor
1,1-DichloroetWane
1,2-Dichloroe/hane
l,l-Dich*oro
l,2-DichIb
-------
Exhibit D
VGA of Ambient Air on Tenax®
Table D/VT-1
(continued)
Target Compound List for Volatiles Collected/on Tens
and Contract Required Quantitation Li
Compound
100-
630-20-
79-43-5
127-18-4
Ethylbenzene
(l-Methylethyl)benzene
1-Methyl-4-(l-methylethyl)benzene
Pentachloroethane
1-Phenyle thanone
Styrene
1,1,1,2-Tetrachloroethane
1,1,2,2 -Tetrachloroe thane
Tetrachloroethylene
Tetrahydrofuran
Toluene
Tribromomethane
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethylene
1,2,3-Trichloropropane
1,3,5-Trimethylbenzene
m- and p-Xylenes
o-Xylene
December, 1991
Page D-66
-------
Exhibit D
VOA of Ambient Air on Tenax®
Table D/VT-2
Typical Operating Conditions for a GC/MSy
Thermal Desorption Unit - NuTech Model 320, Tekraan Hoc
xor equivalent
Helium @ 1.2 mj
8 minutes
25°C
150°C
10 mL/min,
200 °C
30°C
0.1 minute's
48C/min to
240eC
0.1 minutes
Purge gas (prior to desorption)
Desorption cycle
Initial desorption temperature
Final desorption temperature
Thermal desorption unit purge
Gas Chromatographv
Injection/Detector temperature
Initial column temperature
Initial hold time
Program (ramp rate)
Final hold temperature
Final hold time
Maximum oven temperature
Carrier gas
GC/MS interface
Sample injection to MS
Column
Mass Spectrometer -
Mass range
Scan time
El condition
Mass scan and detector modi
Routine tuning
Preamp sensit^:
Emission cu
Electron
Mass filt
Filter
Total la
Resolution
Display
Response
3/sec at 250°C
jet
'd OV-1 glass capillary
:thyl silicone (50 m x 0.3
film thickness) Scientific
SE-30 glass capillary
:hyl silicone (50 m x 0.5 mm,
ckness),or equivalent.
ectron Impact (El)
1 sec-10 min over entire range
70 eV
Follow manufacturer instruction for select
selective detector (MS) and scan mode
nofluorobenzene (BFB)
-0.45
1000 to 1500
10 amu/sec
x 100
1
Normal
TIC
Fast
December, 1991
Page D-67
-------
Exhibit D
VOA of Ambient Air on Tenax®
M/e
50
75
95
96
173
174
175
176
177
Table D/VT-3
Required BFB Key Ions and Ion Abundance
Ion Abundance Criteri
8.0 to 40.0 percent of m/,
30.0 to 66.0 percent o
base peak, 100 perce
5.0 tO 9.0 percent/of
less than 2.0
50.0 to 120.0 percent of m/e"
4.0 to 9.0 jf5reen£_o_f_ m/e 174
93.0 to Wt ~~~
NOTE: All iorN^bundaR^es mus£ b£ normalized to m/z 95, the nominal base peak,
even though the iotksabunaajK:«s of/m/z 174 may be up to 120 percent that of m/z 95.
December, 1991
Page D-68
-------
Exhibit D
VOA of Ambient Air on Tenax®
Table D/VT-4
Composition and Concentration (ng, on column/in
of Calibration Standards
Compound
benzaldehyde
benzene
benzonitrile
bromobenzene
b romochlorome thane
1-bromo- 3 -chloropropane
bromoethane
bromotrichloromethane
butylbenzene
carbon tetrachloride
chlorobenzene
2-chlorobutane
1-chloro-2,3-epoxypropane
2-chloroethoxyethene
chloroform
1-chloropropane
2-chloropropane
3-chloro-1-propene
m-chlorotoluene
o-chlorotoluene
p-chlorotoluene
1,2-dibromoethane
dibromomethane
1,2-dibromopropane
1,2-dichlorobenzene
1,3-dichlorobenzene
1,4-dichlorobenzene
1,3-dichlorobutane
1,4-dichlorobutane
2,3-dichlorobutane
3,4- dichloro -1 -^butene
cis-l,4-dichl
1,1-dichlor
1,2-dichlo
Cal 1
Cal__5
December, 1991
Page D-69
-------
Exhibit D
VGA of Ambient Air on Tenax®
Table D/VT-4
(continued)
Composition and Concentration (ng, on colt
of Calibration Standards
Compound
Cal 1
1,1-dichloroethene
1,2-dichloropropane
1,3-dichloropropane
1,2-dimethyIbenzene
1,4-dioxane
l-ethenyl-4-chlorobenzene
ethylbenzene
(1-methylethyl) benzene
l-methyl-4-(l-methylethyl)benzene
pentachloroethane
1-phenylethanone
styrene
1,1,1,2-tetrachloroethane
1,1,2,2-tetrachloroethane
tetrachloroethene
tetrachloromethane
te trahydro furan
tribromomethane
1,1,1-trichloroethane
1,1,2-trichloroethane
trichloroethene
1,2,3-trichloropropane
1,3,5-trimethylbenze
toluene
xylene, m- and p-
xylene, o-
December, 1991
Page D-70
-------
Exhibit D
VOA of Ambient Air on Tenax®
Table D/VT-5
Target Compound List for Volatiles Collected on
with Characteristic Ions (Primary and S/cor
Cartridges
•ry)
Compound
Benzene
Bromobenzene
Bromochloromethane
1-Bromo-3 -chloropropane
Bromoethane
Bromotrichloromethane
n-ButyIbenzene
Carbon Tetrachloride
Chlo robenzene
2 -Chlorobutane
l-Chloro-2,3-epoxypropane
2 -Chloroethoxyethene
Chloroform
1-Chloropropane
2-Chloropropane
3-Chloro-l-propene
m-Chlorotoluene
o-Chlorotoluene
p-Chlorotoluene
1,2-Dibromoethane
D ib r omome thane
1,2-Dibromopropane
,2-Dichlorobenzene
,3-Dichlorobenzene
,4-Dichlorobenzene
,3-Dichlorobutane
,3-Dichlorobutane
1,4-Dichlorobutane
cis-l,4-Dichloro-2-butene
3,4-Dichloro-l-bu
1,1-Dichloroetj
1,2-Dichloro
1,1-Dichlor/eti
1,2-Dichlo.
Primary Ion
December, 1991
Page D-71
-------
Exhibit D
VGA of Ambient Air on Tenax®
Table DAT-5
(continued)
Target Compound List for Volatiles Collected on/Tena>
with Characteristic Ions (Primary and/6ec/
Primary Ion
Compound
1,3-Dichloropropane
1,4-Dioxane
Ethylbenzene
l-Ethenyl-4-chlorobenzene
(1-Methylethyl) benzene
1-Methyl-4-(l-methylethyl)benzene
Pentachloroethane
1-Phenyle thanone
Styrene
1,1,1,2-Tetrachloroethane
1,1,2,2-Tetrachloroethane
Tetrahydrofuran
Tetrachloroethylene
Tribromomethane
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethylene
1,2,3-Trichloropropane
1,3,5-Trimethylbenzene
Toluene
Xylanes, o-, m-, and p-
December, 1991
Page D-72
-------
Exhibit D
VOA of Ambient Air on Tenax®
Table D/VT-6
Typical Compounds Used in Response Factor (RF) Detei
Specific Mass Loading onto Spiked Carl
Compound
Benzene
Chloroform
1,1,1-Trichloroethane
Carbon Tetrachloride
1,2-Dichloroethane
Trichloroethylene
1,1,2,2-Tetrachloroethane
Chlorobenzene
Tetrachloroethylene
Ethylbenzene
o-, m-, and p-Xylenes
Styrene
o-Dichlorobenzene
p-Dichlorobenzene
December, 1991
Page D-73
-------
Exhibit D
VGA of Ambient Air on Ter.ax®
Figure D/VT-1
Common Designs of Adsorbent Cartrigeys
Cartridge
mm OD x
mm Lena)
(a) Glass Cartridge
1/2" to
i/r-
R*dudn«
Union
[ultibcd Adsorbent Tube
December. L991
Page D-74
-------
Exhibit D
VOA of Ambient Air on Tenax®
Figure D/VT-2
Typical Desorption GC/MS Configuration
December, 1991
Page D-75
-------
Exhibit D
VOA of Ambient Air on Tenax®
Figure D/VT-3
Flash Evaporation Unit
A*— HALF,
P •« /HELIUM FLOW
AJON ULTRA-TORR 5/8 in.
ION (bored ouC to 16.5
. 5 mm)
TENAX ADSORBENT CARTRIDGE
December, 1991
Page D-76
-------
Exhibit D
VOA of Ambient Air on Tenax®
Matheson
8-5BD
Regulator
Figure D/VT-4
Permeation Tube System for
Generating Standard Gas Atmospheres
500 iccm
Exhaurt Line
ray Teflon-Plug
^/ Stopcodci
N«edlt Valves
Mixing Chamber
Permeation Chamber
Jacket
Thermostat, Heiter. and
Circulating Pump
Carrie.r.Gas Line:
Thermostat Fluid Lines
December, 1991
Page D-77
-------
Exhibit D
VOA of Ambient Air on Tenax®
Figure D/VT-5
Tenax Cleanup Schematic Diagram
ASSIGN NUMBEf
TO TENAX
BATCH
SOXHLET
EXTRACTION
• Logbook
• Cha)n«of*Custody
Methanao/Pent
Extraction
is/hour
THERMAL
DESORPTION
• Hallum flow
• Descrb for
CARTRtaGE
PACKING
tub*
Star* in cte*n room
In en* gallon cans
Rafrlgarat*
until us*
Compute logbook and
Chaln-of-Custcdy Form
D«»iceat*
• Vacuum ov«n
100° C
overnight with
Nitrogen Flow
/ Jt
SIEVING
TENAX
f
-4-
December, 1991
Page D-78
-------
Exhibit D
VOA of Ambient Air on Tenax®
Tenax Batch No.:
Virgin Recycled^
No. of cartridges:
Figure D/VC-6
Tenax Cleanup Worksheet
Proj<
(check one) Recy(
SIEVING/PACKING
Sieve (40/60)
Packing
CLEANUP
Teflon
Teflon line
Date:
Hours:
imp trap:
(hours):
rent through Act. C:
Date:
Date:
Date:
Date:
12345
Date
Hours
lowrate
EXTRACTION
No. of Soxhlet units (circle one)
Methanol extraction:
Pentane extraction:
DRYING
Nitrogen chamber
Vacuum oven:
December, 1991
Page D-79
-------
QUALITY ASSURANCE/QUAL\TY\ONTRO
December, 1991
-------
EXHIBIT E
QUALITY ASSURANCE/QUALITY CONTROL REQUI
TABLE OF CONTENTS
Page No.
SECTION 1 INTRODUCTION
SECTION 2 QUALITY ASSURANCE PLANS
SECTION 3 STANDARD OPERATING PROCEDURES .././... ./>. E-7
SECTION 4 CHAIN-OF-CUSTODY /./...././ E-14
SECTION 5 DOCUMENT CONTROL >^ . >\ / . / E-17
SECTION 6 ANALYTICAL STANDARDS REQUIREMENTS . -\. . ^x. E-21
SECTION 7 METHOD SPECIFIC QA/QC REQUIREMENTS . . . 7XNV, . r> E-27
r——-^ ^/
SECTION 8 REGIONAL DATA REVIEW /. w^. • T^T—r-_^^^^ E-33
SECTION 9 LABORATORY EVALUATION SAMfcLES\. . . / :/T~~r~-^^/. E-34
SECTION 10 GC/MS TAPE AUDITS \. \/. / E-36
SECTION 11 ON-SITE LABORATORY-EVALUATIONS \ . \ E-37
SECTION 12 QUALITY ASSUR/NCEx-DMA TREND ANALYS^XS .\ E-40
J \ ^^^^ V
SECTION 13 DATA MANAGEMENT^ ... J .... ^v^- E-42
SECTION 14 REFERENCES / . . . /. / . . /">-*/ E-44
December, 1991
-------
SECTION 1
INTRODUCTION
1.1 Quality assurance (QA) and quality control (QC) are/incegral parts of
EPA's Contract Laboratory Program (CLP). The CLP QA pr/5gra4 consists of
management review and oversight at the planning, implementat]LlxK and
completion stages of environmental data generation aotiv^ftTies. tbxensure that
data provided are of the quality required. The CLP/^C/prograifrx^nc hides those
activities required as part of data generation to ^Qsyre that theMataa^e of
known and documented quality.
1.2 During the planning of an environmental d
activities focus on defining data quality obj
designing a QC system to measure and documen
generated. During the implementation of th<
activities ensure that the QC system is fu:
deficiencies uncovered by the QC system are
environmental data are generated, QA activitie"
of data obtained to determine its suitability to
remedial decisions.
ollection program, QA
ti^es and £*iteria, and
qualit^ of data that will be
collection effort, QA
ing effectively, and that the
corrected. After
locus ctfi assessing the quality
forcement or
dent:
/to
1.3 The purpose of this Exhibit is
and the processes by which the CLP <
-------
Exhibit E
VOA of Ambient Air on Tenax®
1.6 Necessary components of a complete QA/QC program inclidde/internal QC
criteria that demonstrate acceptable levels of performance, a(s determined by
QA review. External review of data and procedures is ac/compJlished by the
monitoring activities of the National Program Office, tyegi«(nal data users,
Sample Management Office, NEIC, and EMSL/LV. Each e?
accomplishes a different purpose. These reviews are,
sections of this Exhibit. Performance evaluation sampl4s provide ahvexternal
QA reference for the program. A laboratory on-sit< evaluation s>s£em rs^also
part of the external QA monitoring. A feedback
the various review functions to the contract laboratories through
communications with the Administrative Project/Off/cers (APOs) and Technical
Project Officers (TPOs).
1.7 This 'Exhibit is not a guide to constructing QA pro^ec/t plans, QC systems,
or a QA organization. It is, however, an ^xpl'anat ion/of /the QC and QA
requirements of the CLP. It outlines someNs^imuliKS/andards for QA/QC
programs. It also includes specific items thats^are required in a QA Plan and
by the QA/QC documentation detailed in this contra^r. DfeJAvery of this
documentation provides the Agency with a complete daczt^packa-ge which will
stand alone, and limits the need for contact with the CohtxactcJr or with an
analyst, at a later date, if some a>s/pect--x>f~»Etje_analysis is>«estioned.
.Contractor
aeets the
data comparison,
1.8 To ensure that the product deli
requirements of the contract and to
the Agency requires the following from^he^Con/ra^tor.
1.8.1 Development and implementation\f a OA program, and documentation
of the key elements of that-QA program through a written QA Plan, as
described in Section 2/of this
libit.
1.8.2 Preparation j/f
Procedures (SOPs)
adherer
ascribed/in Sectior
/Standard Operating
or this Exhibit.
1.8.3 Adherence/ to
specified in thexcontfJ
analytical methods-and associated QC requirements
1.8.4 Verification o
purity of nea^jnatferials al
from privat^chemical>sfeouses.
the
_al standards and documentation of the
rity and accuracy of solutions obtained
1.8.7 Subm
review.
analysis of laboratory performance evaluation
nee to corrective action procedures.
laboratory evaluations, including
procedures.
all/raw^data and pertinent documentation for Regional
December, 1991
Page E-2
-------
Exhibit E
VOA of Ambient Air on Tenax®
1.8.8 Submission, upon request, of GC/MS tapes and
documentation for tape audits.
1.8.9 Submission for Agency review of all originaly
generated during sample analyses.
applicable
December, 1991
Page E-3
-------
Exhibit E
VOA of Ambient Air on Tenax®
SECTION 2
QUALITY ASSURANCE PLANS
2.1 The Contractor shall establish a QA program wi
providing sound analytical chemical measurements.
incorporate the QC procedures, any necessary corr
documentation required during data collection as
assessment measures performed by management to
production.
2.2 As evidence of such a program, the Con
Quality Assurance Plan (QAP) which describ
implemented to achieve the following:
2.2.1 Maintain data integrity, validity,
2.2.2 Ensure that analytical measurement system,
acceptable state of stability and reproducibility
2.2.3 Detect problems throug:
action procedures which keep
pare a written
ures that are
2.2.4 Document all aspects of theNjieaJ
data that are technically sound and
2.3 The.QAP must present,
objectives, and specific
quality requirements in
each element shall be i;
be available during
the Administrative P
preparation of a Q<
intained in an
tablish corrective
able.
leryt process in order to provide
.ef ensible.
policies, organization,
to achieve the data
able, SOPs pertaining to
t of the QAP. The QAP must
ion and upon written request by
nformation relevant to the
'M publications"'*'.
2.4 ELEMENTS OF A QU
2.4.1 The
program sh.
2.4
the Contractor's quality assurance
sed irT
policy and Objectives
Personnel
ientf of QC and QA responsibilities; and
December, 1991
Page E-4
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Exhibit E
VGA of Ambient Air on Tenax®
Reporting relationships.
Personnel;
Staff resumes;
Education and experience requireji
Contract; and
Training progress.
Facilities and Equipment;
Instrumentation and bad
Maintenance activities
Document Control;
Laboratory notebook policy;
Sample and dat
documentation
and
Logbook maintenan
and distribution \of
Case file organizati
procedures; and
aures;
ration, and review
roval, review, revision,
Analytical/ Methodol
7 7 / \. F
frequency;
and storage procedures;
jle prejJ&ratiohxprocedures;
fsis pr^sc/edures; and
jaration procedures.
Data Generation);
colle/ctiy6n procedures;
iata f»/lucVlon procedures;
December, 1991
Page E-5
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Exhibit E
VOA of Ambient Air on Tenax®
Data review procedures;
Data reporting and authorization
Data management procedures.
Quality Control Program; and
Solvent, reagent, and adsorbefltsCcheck
Reference material analysi?
Internal QC checks; and
Corrective action and
procedures.
Quality Assurance Program Assessing
Data audits;
Systems audits
Performance audit
Corrective action pfbicedtores/ and
QA repor£i«g~^procedures\
December, 1991
Page E-6
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 3
STANDARD OPERATING PROCEDURES
3.1 In order to obtain reliable results, adherence
methodology is imperative. In any operation that
basis, reproducibility is best accomplished throug'
Operating Procedures (SOPs). As defined by the
document that provides directions for the step-
operation, analysis, or action which is commonl
performing certain routine or repetitive tasks/
3.2 SOPs prepared by the Contractor must b
comprehensive, up-to-date, and sufficient!
results by qualified analysts. All SOPs,
reflect activities as they are currently per
addition, all SOPs must:
3.2.1 Be consistent with current EPA regulations
contract's requirements; ~
3.2.2 Be consistent with inst
manuals;
3.2.6 Describe the corre
analytical ce"sultsao^*ipt mee
analytical
epetitive
p execution of an
fcepted as the method foi
'e. , clear,
rmit duplication of
the Agency, must
laboratory. In
s, and the CLP
fie instruction
3.2.3 Be available to the EPA durin-
complete set of SOPs shall be bound
at such evaluations. DurjjifrOn-Site
be asked to demons trata/the ap
3.2.4 Provide for
complete to record
3.2.5 Describe
reported by the
inconsistent resul
te Laboratory Evaluation. A
and available for inspection
ons, laboratory personnel may
SOPs;
ion that is sufficiently
required by the protocol;
ing the validity of data
the cause of missing or
3.2.9 Be
sures and feedback mechanism used when
requirements;
and updated as necessary when contract,
iural modifications are made;
eference in usability or evidentiary
work stations as appropriate; and
December, 1991
Page E-7
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Exhibit E
VOA of Ambient Air on Tenax®
3.2.10 Be subject to a document control procedure whioh precludes the
of outdated or inappropriate SOPs. / /
use
3.3 SOP SPECIFICATIONS AND FORMAT
3.3.1 An SOP is defined as a written narrative s/tep/By^step^xJescription
of laboratory operating procedures including exatapLes otl>aboral
documentation. The SOPs must accurately describe /the actual^procedCctes
used in the laboratory, and copies of the writfterr SOPs shall
to ensure that analytical data produced under thus contract are acce>£a#le
for use in EPA enforcement case preparation/anci litigation. The
Contractor's SOPs shall provide mechanisms/arya documeireation to meet each
of the following specifications and shal^/be/used by/EP^ sa the basis for
laboratory evidence audits.
3.3.2 The format for SOPs may vary demanding-
for which they are prepared. However, at
sections must be included.
3.3.2.1 Title page.
3.3.2.2 Scope and application
3.3.2.3 Definitions.
3.3.2.A Procedures.
3.3.2.5 QC acceptanj
3.3.2.6 Corrective
secondary revie
tjie kind of activity
the following
3.3.2.9 Reference
ing procedures for
ted.
fample forms.
and precautions.
samp
proc
Contrac
and use adequate written SOPs to ensure
• Evidentiary SOPs shall include specific
ocesses as they are performed by the
December, 1991
Page E-8
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Exhibit E
VGA of Ambient Air on Tenax®
3.4.1.1 Sample receipt and logging
3.4.1.1.1 The Contractor shall have written/
and logging in the samples. The procedures
documentation of the following informatiot
Presence or absence of EPA chair
• Presence or absence of airbill*
Presence or absence of EPA
lists;
Presence or absence of
sample containers and 0iei/ condit
Custody seal numbers,
Presence or absence of sample^
Sample tag ID numbers;
Condition of tr
Condition of the
Reports or SAS packing
shipping and/or
Verification of agre
on receiving documents"
3.4.1.2
nonagreement of information
ample containers;
epancies with SMO; and
>
d to describe sample
have a designated sample
for receipt of samples and have written
Ls/her duties and responsibilities.
shall have written SOPs for
:ification of EPA samples throughout the
Contractor assigns unique laboratory
SOPs shall include a description of the
sign the unique laboratory identifier and
o the EPA sample number.
December, 1991
Page E-9
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Exhibit E
VGA of Ambient Air on Tenax®
3.4.1.2.3 If the Contractor usts prefixes/or^suffixes in
addition to sample identification numbers/ tjtfe written SOPs
shall include their definitions.
3.4.1.3 Sample security
The Contractor shall have writt*
the security of samples after log-:
security of the sample storage ar
shall specifically include descriptions of all storage
for EPA samples in the laborat
sample contamination. The SO
authorized personnel who hav
and steps taken to prevent
ie a list of
ire storage areas.
3.4.1.4 Internal chain-of-custody/of
The Contractor shall have "wi^tten S^DPs for the chain-of-
custody consisting of sample idenH£ica"ti«n, chain-of-custody
procedures, sample receiving procedure^. anoNsample tracking
procedures. For more information concerrfine ttyfe chain-of-
custody procedures yee~~5etrti
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Exhibit E
VGA of Ambient Air on Tenax®
3.4.2.1 The Contractor shall have written SOPs for/^preventing sample
contamination, during sample preparation, cleaning/of/glassware,
storage, and analysis.
3.4.2.2 The Contractor shall have SOPs to ensi/re
standards used in sample analysis QA/QC.
3.4.3 Quality Management SOPs
3.4.3.1 The Contractor shall have writt
managerial review of laboratory operati
preparation, laboratory data review/la
The procedures shall include but not
following information:
aceability of
3.4.3.1.1 Data flow and char
3.4.3.1.2 Procedures for measuring
3.4.3.1.3 Evaluation of parameters for
errors.
3.4.3.1.4 Procedures
complete and compliant
ory self inspection system
ocumenting the
3.4.3.1.7 /Dei
actions, /and.
resulting f
3.4.3.
n ot_4jrobl
analtic
l/audit
data review;
(on and accuracy.
systematic
eliverables are
xhibit B.
3.4.3.1.5 Demonstration o
(demonstrated by supervisory
internal PE samples, etc.).
3.4.3.1.6 Fr
quarterly, s
inspection procedure
on personal notebooks,
al audits (e.g., random,
e areas).
identification, corrective
processing. Sequence
QA feedback).
"W ^ /
3.4.3.1.8 Db
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Exhibit E
VOA of Ambient Air on Tenax®
concerning document control and case file preparation/ see Section 5
of this Exhibit.
dat
3.4.3.3 The Contractor shall have written SOP
management and handling, and reporting of
include but not be limited to documenting
3.4.3.3.1 Procedures for controlling
errors.
3.4.3.3.2 Procedures for reviewin,
deliverables and ensuring traceab
sample analysis,
;ocedures shall
^formation:
3.4.3.3.3 Life cycle manageme
and implementing changes to e
hardware, software, and docume
3.4.3.3.4 Database security, backup
including recovery from system failures.
3.4.3.3.5 System maintenance
anges to data and
js.
testing, modifying
systems including
tailing new systems.
procedures
se time.
3.4.3.3.6 Individual ( s Kre'kpons'itrle-; for^system/operation,
maintenance, data integrity a*\d seci/rit
3.4.3.3.7 Specifications fo\ staff /raining procedures.
3.4.3.4 The Contragtor-stiall have written SOPs for laboratory safety.
3.5 HANDLING OF CONFIDI
VTION
conducting/ workunde
sntifal information f
3.5.1 A Contracto,
designated confi
information must/be^iandled^ep/rately ff
under this cont
handling of confide
EPA-
the
Lai infoi
s contract may receive
Agency. Confidential
other documentation developed
this, the following procedures for the
tation have been established.
Jlish
3.5.2 All co
designated
informa
Log. The
only after: it
documents shall
^hall be under the supervision of a
30).
.tion received with a request of
ed as "confidential." A separate locked
re this information and shall be segregated
rmation. Data generated from confidential
fidential. Upon receipt of confidential
e documents into a Confidential Inventory
made available to authorized personnel but
d out to that person by the DCO. The
eturned to the locked file at the conclusion of each
December, 1991
Page E-12
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Exhibit E
VGA of Ambient Air on Tenax®
working day. Confidential information may not be rep
approval by the EPA Contracting Officer. The DCO wil
into the document control system. In addition, this
be disposed of except upon approval by the EPA Cont
DCO shall remove and retain the cover page of any
disposed of for one year and shall keep a record /of
Confidential Inventory Log.
iuced except upon
:er all copies
jrmation may not
Lng Officer. The
iential information
th--
3.6 SOPS DELIVERY REQUIREMENTS
Within forty-five (45) days of contract
SOPs relevant to this contract shall be
Also, during the term of performance of
have been amended or new SOPs which hav$
TPO, EMSL/LV (quality assurance SOPs)
in
set
complete
:o the TPO, SMO and EMSL/LV.
ipies of JOPs which
LI be sent to the
'tiary SOPs).
December, 1991
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 4
CHAIN-OF-CUSTODY
A sample is physical evidence collected from a £
environment. An essential part of hazardous waste
that the evidence gathered be controlled. To ace
sample identification, chain-of-custody, sample
procedures have been established.
4.1 SAMPLE IDENTIFICATION
4.1.1 To ensure traceability of samples wtfile in possession of the
Contractor, the Contractor shall have/a specified/method for maintaining
identification of samples throughout tt
4.1.2 Each sample and sample preparation cont^iner^shall be labeled with
the EPA number or a unique laboratory identifierN^If aXmique laboratory
identifier is used, it shall be cross-referenced to ctie EKJ? number.
4.2 CHAIN-OF-CUSTODY PROCEDURES
Because of the nature of the
samples must be traceable from the^imV tk\& s
they are introduced as evidence in 1<
shall have procedures ensuring that
documented. A sample islander custody
4.2.1
4.3 SAMPLE RE<
custody of EPA
les are collected until
eedings. The Contractor
custody is maintained and
following applies:
,n_your possession, or
locked it up, or
4.2.4 It is i
accessible to
ed secure area (secure areas shall be
only).
lURES
4.3.3 The
be inspected u
representative
designate a sample custodian responsible for
ignate a representative to receive samples
Custodian is not available.
.e /shipping containers and sample bottles shall
the sample custodian or his/her
December, 1991
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Exhibit E
VGA of Ambient Air on Tenax®
4.3.4 The condition of the custody seals (intact/not inottles.
4.3/9.S/ Presence br absence of airbills or airbill stickers.
Airbill or aiVbill sticker numbers.
pice of EPA custody records.
oy absence of EPA traffic reports or SAS packing
lists.
December, 1991
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Exhibit E
VGA of Ambient Air on Tenax®
4.3.9.9 Presence or absence of sample tags.
4.3.9.10 Sample tag identification numbers cro
EPA sample numbers.
4.3.9.11 Verification of agreement or non-
recorded on shipping documents and sample c
4.3.9.12 Problems or discrepancies.
4.4 SAMPLE TRACKING PROCEDURES
The Contractor shall maintain records
handling from receipt to final analysis.
documentation of the movement of samples
designated laboratory storage areas.
-r/ferenced to the
formation
ases of sample
include
les into and out of
December, 1991
Page E-16
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Exhibit E
VGA of Ambient Air on Tenax®
SECTION 5
DOCUMENT CONTROL
The goal of the laboratory document control progr,
documents for a specified Sample Delivery Group (SD
when the project is completed. Accountable docume
laboratories shall include but not be limited to 1
records, sample work sheets, bench sheets, and o
sample or sample analyses. The following docum/nt
ontrol
been established to assure that all laboratory/records are
stored for delivery to the EPA or are available y(p°n recl
prior to the delivery schedule.
5.1 PREPRINTED LABORATORY FORMS AND LOGBOOKS
Contractor w]
tdxassure that all
>e accounted for
b>
chain
to
procedures ti
assembled and
from the EPA
5.1.1 All documents produced by the
to the preparation and analysis of EPA sample
of the EPA and shall be placed in the complete s
(CSF). All observations and results recorded by
preprinted laboratory forms sh
logbooks. When all data from *a SDfi^gre^compile
forms and copies of all SDG-relA^ed\logl
the documentation package.
ch are directly related
the property
yery group file
the^laborytory but not on
permaneift laboratory
original laboratory
intries shaZl be included in
into
5.1.2 'The Contractor shall identify\the
laboratory documents which is directly\rele
analysis of EPA samples
ivity recorded on all
ted to the preparation and
5.1.3 Pre-printed
laboratory and be d£te<
responsible for peyrfo
performed.
5.1.4 Logbook
person responsible
performed.
fokms shall c\mt
(montWd
ing the act
Tye
ity
,n the name of the
gned by the person
ie time an activity is
perTo
dated (month/day/year) and signed by the
ning the activity at the time an activity is
5.1.5 Logfco'ok entrie>x§hall Bfes.in chronological order. Entries in
logbooks .Awith^EEe-^xceptSon of rhsjrrument run logs and extraction logs,
shall ijfclu4e only oneX^DG per page.
5.1.6/ P^ges in both bound\ and-unbound logbooks shall be sequentially
numherec
5.1.7 li^strumfeiat run log/ shall be maintained so as to enable a
reconstruction orthe run sequence of individual instruments. Because the
laboratory musb^RrovicVe/coyies of the instrument run logs to the EPA, the
December, 1991
Page E-17
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Exhibit E
VGA of Ambient Air on Tenax®
laboratory may exercise the option of using only laboratory or EPA sample
identification numbers in the logs for sample ID rather than government
agency or commercial client names to preserve the confidentiality of
commercial clients.
5.1.8 Corrections to supporting documents and raw d^fca^shailxbe made by
drawing a single line through the error and entering the
information. Corrections and additions to supporting docume
data shall be dated and initialed. No information shall be obli
rendered unreadable. All notations shall be/recorded in ink. Uj
portions of documents shall be crossed out.
5.2 CONSISTENCY OF DOCUMENTATION
5.2.1 The Contractor shall assign a
for the organization and assembly of
5.2.2 All copies of laboratory documents
5.2.3 Original documents which include information
one SDG shall be filled in the
shall be placed in the other CS
following information on the coj
officer responsible
ORIGINAL IS FILED IN CSF
The Contractor shall sign and
5.2.4 Before relea
shall assemble and
records, lab benc
relevant data to
sample delivery
5.3 DOCUMENT NUMBERING
5.3.1 In
analysis
serializ:
lete and legible.
to more than
The copy(s)
shall record the
to the copy(ies).
de
document control officer
^on on sample tags, custody
t logs, and other
to each particular sample or
:ent throughout the CSF.
countability of thfe completed
in aFshall be inventoried and assigned a
d in Exhibit B, Section 2.
d number (For example: 75-2-0240).
records, re
attempted
be inventoried.
o each sample delivery group, including
ass spectra, chroma tograms , screening
cods, re-analysis records, records of failed or
records , library research results, etc., shall
December, 1991
Page E-18
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Exhibit E
VOA of Ambient Air on Tenax®
5.3.3 The Document Control Officer (DCO) shall be responsible for
ensuring that all documents generated are placed in the CS£ for inventory
and are delivered to the EPA. The DCO shall place th
-------
Exhibit E
VGA of Ambient Air on Tenax®
5.5.3 A copy of the transmittal letter for the CSF wi^l t>fe sent to the
NEIC and the SMO.
5.5.4 The Document Control form is used to document thfe receipt and
inspection of shipping containers and samples. The Contractor shall
submit one (1) original FORM AADC-1 for each shij
5.5.5 The Contractor shall sign and date the
examine the shipping containers, record the
seals and their conditions.
5.5.6 The Contractor shall note any probl
the instructions explained in Exhibit B,
5.5.7 The Contractor shall submit a c
each SDG package.
t Control Form with
es and follow
eet.
December, 1991
Page E-20
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Exhibit E
VGA of Ambient Air on Tenax®
SECTION 6
ANALYTICAL STANDARDS REQUIREMENTS
The U.S. Environmental Protection Agency will not/supply
reference standards either for direct analytical measurable
purpose of traceability. All contract laboratorie
prepare from neat materials, from cylinders of co
NIST Standard Reference Materials or NIST/EPA api/ra
material, or purchase from private chemical supply
lytical
or EQT the
be re^uirec
sed gases
d certified refe^erice
ouses those standarc
necessary to successfully and accurately perfo/m
protocol.
6.1 PREPARATION OF CHEMICAL STANDARDS FRO*
ie analyses required in this
NEAT HIGH/TURITY BULK MATERIAL
6.1.1 A laboratory may prepare their chsmicat^-s^arwfards from neat
materials. Commercial sources for neat chemical standards pertaining to
analytes listed on the TCL are given in Appendix C of^he "Quality
Assurance Materials Bank: Analytical Reference Sta~ndards>5v,Seventh
Edition, January 1988. Laboratotigsshould obtain tnexhighest purity
possible when purchasing neat ohemicaT~5tsBdaj:ds; standards purchased at
less than 98% purity must be daeumwttedas to yHy~~a—feigtjer purity could
not be obtained.
6.1.2 Neat chemical standards must\be
used in the preparation of standard
chemicals is essential in order to saf
sfrigerated when not being
Proper storage of neat
them from decomposition.
6.1.3 The purity of
chemical supply housy
the concentration
laboratory's resp<
that the purity
confirmation, v\
compound>can sometitaes^be misrepresented by a
ince\knc|wledge of purixy is needed to calculate
olutifact<>T:xfor impurity when weighing neat
materials £n the preparation ofxsoluvion standards is:
und
ft. of pure compound
. percent purity.
100
Eq. E-l
whereXvxweigfr&spf pure compound" is that required to prepare a specific
volume 0^4 solbtiiLon stan/lard^ of a specified concentration.
December, 1991 Page E-21
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Exhibit E
VOA of Ambient Air on Tenax®
6.1.4 Mis-identification of compounds occasionally oocuris and it is
possible that a mislabeled compound may be received from/a chemical supply
house. It is the contract laboratory's responsibility/to have analytical
documentation confirming that all compounds used iri th4 preparation of
solution standards are correctly identified. Identification confirmation,
when performed, should use GC/MS analysis on at /lea^-^wo different
analytical columns, or other appropriate technique/
6.1.5 Calculate the weight of material to
volume taking into account the purity of thja
concentration. A second person must veriJ
calculations. Check balances for accurac
All weighing should be performed on an
0.1 mg and verified by a second person,
solute should be compatible with the
be used; the solute should be soluble.
solvent. In the case of a multicomponentT"
not react with each other.
6.1.6 Log notebooks are to be kept for all weighingNand dilutions. All
subsequent dilutions from the p£imSry--fi£andard and the calculations for
determining their concentrations aretp berec^frded^and verified by a
second person. All solution st^ndariils~~aTe—to be refrigerated when not in
use. All solution standards are\:o be clearly/laBSied/as to the identity
of the compound or compounds, concentra^ioyn, /date prepared, solvent, and
initials of the preparer.
6.2 PURCHASE OF CHEMICAL
ighed out for
[pound and the desirfe
'& accuracy of the
f standard weights.
!ce to the nearest
solve/t vised to dissolve the
the standard is to
.onreactive with the
lution/ the components must
6.2.1 Solutions of
Contractors provid
6.2.1.1 Con
documentati
purchase:
ds can be purchased by
iteria.
standard a
below) . The
ain the following
the standard solutions they
confirmation of the neat material ;
t material ; and
^quantitative documentation that the solution
according to the following section.
jst purchase standards for which the quality
?lly and analytically by a method of the
y this can be demonstrated is to prepare and
high standard, a low standard, and a
/concentration (see sections 6.2.1.3 and 6. 2.1. A
must then demonstrate that the analytical
December, 1991
Page E-22
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Exhibit E
VOA of Ambient Air on Tenax®
insistent with the
^e by the
ffhis is achieved,
Nation of the
of the low and
The standard
ration.
results for the high standard and low standard are
difference in theoretical concentrations. This i
Student's t-test in part 6.3.1.3 which follows.
the supplier must then demonstrate that the con
target standard lies midway between the concen
high standards. This is done by the Student'
is certified to be within 10 percent of the
6.2.1.3 If the procedure above is used, t
that the following have been achieved.
• Two solutions of identical concent/ati/on must be prepared
independently from neat materials/: An aliqup^Nif the first
solution must be diluted to the /intended concentration (the
"target standard"). One aliquot is taken /ronr the second solution
and diluted to a concentratioi/ teri^percent greater than the target
standard. This is called the "THEh sfcan4arjiJ". One further
aliquot is taken from the second sbiution a{nd diluted to a
concentration 10 percent less that thexw standard, target,
standard; and
ts for each solution must be
Eq. E-2
Eq. E-3
The valu<
analyses of
standards are
varia;
and
represent the results of the six
rd. The means of the low, target, and high
Mx, M2, and M3, respectively. The
t, and high standards are designated
Additionally, a pooled variance,
Eq. E-4
If
/10.00
calculatia
5t of Vp is less than one percent of M2, then M22
ted as the value of Vp in all subsequent
December, 1991
Page E-23
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Exhibit E
VOA of Ambient Air on Tenax®
The test statistic must be calculated:
TEST STATISTIC
If the test statistic exceeds 2.13
demonstrate a twenty percent differe
standards. In such a case, the sta:
The test statistic must be calcul/
\M2 -
TEST STATISTIC =
If the test statistic exceeds 2.13, the
demonstrate that the target standard concent
between the high and Ic
are not acceptable.
The 95 percent confidence1
standard must be calculate
INTERNAL FOR LOW STAND.
INTEJ
Eq. E-5
ed to
etween
s are not acceptable
STANDARD = M,±(2.13) (—£)
Eq. E-6
.as failed to
s midway
the standards
.n result of each
Eq. E-7
Eq. E-8
Eq. E-9
Theseintfervals m
fai
ference
If overlap is observed, then
nonstrate the ability to discriminate
di^ferenc£vsjtn/ concentrations. In such a case, the
standards are^spt acceptable. In any event, the laboratory is
responsible for tshe quality of the standards employed for analyses
ider this contract.
6.3 REC
iSTII
STANDARDS FROM/
EPA STANDARDS REPOSITORY
Solutio^ns of analytiyal /reference materials can be ordered from the
U.S. EPA Chemifca.1 Sta>i4ards' Repository, depending on availability. The
Contractor can plkise an oBxier for standards only after demonstrating that
December, 1991
Page E-24
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Exhibit E
VOA of Ambient Air on Tenax®
chese standards are not available from commercial vendoi
solution or as a neat material.
either in
6.4 DOCUMENTATION OF THE VERIFICATION AND PREPARATION OF CHEMICAL STANDARDS
It is the responsibility of each laboratory t«f mainta^ki the necessary
documentation to show that the chemical standards they^-have visaed in the
performance of CLP analysis conform to the requlrenfents pr«vious"i^- Lsted.
Weighing logbooks, calculations, chromatogramsVsniass spectra\^tc, whether
produced by the laboratory or purchased from/en»mical supply hou
be maintained by the laboratory and may be ^ubiect to review during
on-site inspection visits. Documentation csf standards preparation may be
required to be sent to EPA for verification at contrac^compiiance. In
those cases where the documentation is suppctrtive of the analytical
results of data packages sent to EPA, s/uch/documenjcat^n is to be kept on
file by the laboratories for a period<
December, 1991
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 7
METHOD SPECIFIC QA/QC REQUIREMENT:
7.1 This section outlines the minimum quality control
necessarv to satisfy the analytical requirements as
deterain. ion of the volatile organic compounds lisi
procedures in Exhibit D for samples of ambient air'
section is not intended as a comprehensive qualitc-pntrol
rathe:- .s a guide to the specific QC operations/that must
analysis of volatiles using this method. The laboratory is expected to
address these operations in preparing the qua/ity/ass- rancVjjlan and Standard
Operating Procedures discussed in Sections 2/an hgtrh o£
preparing Tenax® cartridges for
Lysfs, the laboratory is required to analyze by
&m each batch of prepared Tenax® cartridges,
^less than 10 ng. If the total VOCs exceed
irtridges shall be rejected.
7.2.1.2 Tfor actepTralile batches, "fihe/laboratory is also required to spike
each cartridge with lOOsng dach of PFT, l,2-dichlorobenzene-d<,, as
internal sjcandards, and bXnze\ie-d6i chlorobenzene-d5, and 1,4-
as the\5uHf°§ate compounds.
7.2.2
cormance Checking/ the Mass Spectrometer and Ion Abundance
Patt*
7.2.2.1 Prior^fco ini^ia'ting any data collection activities involving
samples, blanks, orx^tandards, it is necessary to establish that a given
December, 1991
Page E-26
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Exhibit E
VOA of Ambient Air on Tenax®
GC/MS system meets the instrument performance criteria/specified in
Exhibit D. The purpose of this instrument performance chfeck is to ensure
correct mass calibration, mass resolution, and mass ;craasmission. This is
accomplished through the analysis of bromofluorobenzen^ (BFB).
7.2.2.2 The required frequency of BFB analysis
each GC/MS system) is described in detail in E
7.2.2.3 The key ions produced during the ana
respective ion abundance criteria are given
3.
7.2.2.4 The documentation includes Form
bar graph spectrum for BFB analysis.
7.2.3 Initial Calibration of GC/MS for
Prior to the analysis of samples and
instrument performance criteria have been
initially calibrated utilizing target compound
compounds.
Blanks and after
system must be
A) and surrogate
7.2.4.5 Relative
Exhibit D.
7.2.4.6
printout/for,.
mass sp/ect
7.2.4 'Internal Standard Calibra
7.2.4.1 The GC/MS may be calibr
Tenax® tubes, and calculating cone
factor '(RRF) method.
7.2.4.2 Calibration s
are prepared as outl
7.2.4.3 The Ten,
internal markers
7.2.4.4 The t
(aards spiked onto
ns/by the relative response
target compounds of interest
known concentrations of
escribed in Exhibit D.
Scribed in Exhibit D.
Actors (RRFs) are calculated as described in
7.2.5
on inc^Uides jForm VII-AAVT, a GC/MS data system
.of eactNsjolatile calibration standard, and the
and surrogate compound.
on for Target and Surrogate Compounds
has been calibrated, the calibration must
2)/hour time period for each GC/MS system.
December, 1991
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Exhibit E
VGA of Ambient Air on Tenax®
7.2.5.2 The standard is to be analyzed according to tjrie procedures and at
the frequency given in Exhibit D.
7.2.5.3 The continuing calibration of the GC/MS system^is evaluated on
the basis of the magnitude of the response factors' and tnexpercent
difference between the average RRF of each compound /rbmthe^initial
calibration and the RRF of that compound in the/conrinuingXcalior^ation
standard. The minimum response factors of eacH^cjXrnpound in the^conbxjuing
calibration and the percent difference must
Exhibit D. Allowance is made for any two v
meet these criteria. The minimum or RRF o
greater than or equal to 0.010, and the
than or equal to 30.0 percent for the co
acceptable.
the criteria giv&Q in
fie compounds that
two compounds must be
ace must be less
ition to be
7.2.5.4 The documentation included Fo
printout for the analysis of the volatile
mass spectrum of each target surrogate compourJ
7.2.6 Internal Markers and Surrogate Standards and
C/MS data system
standard, and the
7.2.6.3 The rete;
each internal m
analyses.
7.2.6.1 The response of each
standards, samples, and blanks
analytical results, because the qv
compounds by these procedures is
added immediately prior to analysis.\ v /
7.2.6.2 The specific
standards are given i
standard is spiked
300 ng.
in all calibration
n of reliable
on of volatile
se of internal standards
1 markers and surrogate
,1 marker and surrogate
a>level of approximately
cted/ion current profile (SICP) of
must be monitored for all
7.2.6.4 The area response of ""each internal marker and surrogate standard
from the SICPand__Che re tendon tla»e of the internal marker and surrogate
standard ar£x"evaluateoNfor stabilitySaccording to the procedures in
Exhibit D/ Th€-aTwkvof the intertte4Aarker and surrogate standard in a
sample must/hot vary byxmorV than 40 percent from the area of the same
internal marker and surro&ate\standard in the associated continuing
calibration standard. LikewisV the retention time of an internal marker
and surrogate standard must) be Iwithin 30 seconds of its retention time in
the etantinultig calibrationyfeta/idard, as described in Exhibit D.
7.2.6.5 Req\iireme>*ts for/an/lysis of samples when internal marker and
surrogate stano^ds d&xtfot ^eet specifications are given in Exhibit D.
December, 1991
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Exhibit E
VOA of Ambient Air on Tenax®
7.2.6.6 The documentation includes Form III-AAVT and t
system printout for the analysis of each sample, blank
standard.
7.2.7 Method Blank Analysis
7.2.7.1 A method blank is a certified clean Ten
desorbed with a volume of helium carried througj
procedure. The volume of helium must be appro^maftely equal
associated with the blank. The purpose of a .method blank is to
the levels of contamination associated with/the/processing and
samples.
GC/MS data
rix spike, and
lume
analy*
7.2.7.2 A method blank shall be analyzes! onte evei
GC/MS system, as described in detail in/Exhibit D.
12/hours on each
7.2.7.3 For the purposes of this protocol, arKa/cep/fcable method blank
must contain less than or equal to the Corrbisact Required Quantitation
Limit (see Exhibit C) of any single target comp^nd/^ar. less than 10
ng/cartridge for total VOCs, whichever is less.
roprij
7.2.7.4 If a method blank exce/ds
Contractor must consider the a:
of the contamination shall be
actions taken and documented before ffcirther/s,
requirements for reanalysis of asso
7.2..7.5 The documentation includes Fofcm IV/AAVT for the blank analysis
and a GC/MS data system-printout for the\ana\ysis of the method blank.
for contamiiR^t ion 'above, the
pntrol. The source
e corrective
sis proceeds. The
are given in Exhibit D.
fl.es
7.2.8 Surrogate Cc
ries
of the/thr
7.2.8.1 The recoWri
from the analysis/of/each sample/bla:
the surrogate compourids is
sampling and des
spots in transfer imes are oj
recovery of these compot
7.2.8.2 The' surrogate^
for samplying^
7.2.8.
ac cor din,
the rfual
surrogate c
steps ou
compounds are calculated
matrix spike. The purpose of
'aluate the^erformance of the Tenax®
Poor purging efficiency, leaks, and cold
ly a few of the potential causes of poor
mpounofi are
dded to each Tenax® tube prepared
scribed in Exhibit D.
tnte surrogate compounds are calculated
ir» Exhibit D. The recoveries must be within
ivfen in Exhibit D. If the recovery of any one
'de A:hese limits, the Contractor must follow the
December, 1991
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Exhibit E
VOA of Ambient Air on Tenax®
7.2.8.4 The documentation includes Form IX-AAVT, and
printout for the analysis of each sample, blank, and
7.2.9 Performance Evaluation (PE) Samples
7.2.9.1 Performance and method evaluation sampl
the Agency in monitoring Contractor performance
be informed as to which compounds are containe
concentrations.
7/MS data system
spike.
to assist
ill not
or\the
7.2.9.2 The Laboratory shall extract, analyze/ and report the results of
the PE sample once per sample delivery group,/if available.
7.2.9.3 The laboratory will receive PE,
the Agency. The samples will come wi
desorption procedure required for the
internal markers and surrogate compounds t"
procedures in Exhibit D.
les on/Ten^x® cartridges from
oncerning the
Laboratory must add
.the PE Cample, following
in^ructipns
samp
7.2.9.4 Each laboratory must extract and concentrate
the procedure described in Exhi#Tt~TT~f<»«^eh£se target
Exhibit C, Table 1.
7.2.9.5 The laboratory must meet\the\folloylnj
acceptance criteria as detailed in\xhit*it
sample using
iunds listed in
Le technical
\ V /
7.2.9.5.1 The PE sample must be analyzed on a GC/MS system meeting
the BFB tuning, initia*~salibration\ano\continuing calibration
technical acceptance criter^i
7.2.9.5.2 The
blank that meegs
7.2.9.5.3 Tfle
within accepS^able
nple mfcstl'it>e~''p^er>areo\a/nd analyzed with a method
blank/technicai"5ic£eptance criteria.
Scoyery for e^cti of the surrogates must be
Us a"s outlined in Exhibit D.
7.2.9.5.4 The areaNr^espo'h&e change between the PE sample and the most
recent caljjaration stahda^d analysis for each of the surrogate
s tandarvdsmus t
\ \
covery for each of the target compounds must
ecftsion and audit accuracy, as outlined in
December, 1991
Page E-30
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 8
REGIONAL DATA REVIEW
8.1 Contract laboratory data are generated to meet the specific needs of the
Regions. In order to verify the usability of data for tKeXmtemiftd purpose,
each Region reviews data from the perspective of end-user, bas«d upb>
functional aspects of data quality. General guidelines for
been developed jointly by the Region and the NatLtfrlsu: Program
Region uses these guidelines as the basis for data ^valuation. Individus
Regions may augment the basic guideline review /process with additional review
based on Region-specific or site-specific cono4rnE. Regi/Shal reviews, like
the sites under investigation, vary based on/The/nature of zhe problems under
investigation and the Regional response appropriate to/the/specific
circumstances.
8.2 Regional data reviews relating usability "bf.the da£a to a specific site
are part of the collective assessment process. Th"»y complement the review
done at the Sample Management Office, which is designted to itieritify
contractual discrepancies, and the review done at EMSL/Lvxwhich is designed
to evaluate Contractor and method p<6rf3rliran6£^These individual evaluations
are integrated into a collective r^yiewjthat isnecBssaryfor program and
laboratory administration and managements ancTTnay^be used to^iake appropriate
action to correct deficiencies in the
December, 1991
Page E-31
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 9
LABORATORY EVALUATION SAMPLES
9.1 Although intralaboratory QC may demonstrate Cor
performance that can be tracked over time, an external/perforirtance evaluation
program is an essential feature of a QA program.
Contractor and method performance, Contractors participate in
comparison studies conducted by the EPA. Results from the analysis of
laboratory evaluation samples will be used by /he /EPA to verify the
Contractor's continuing ability to produce ac£eptzable analytical data. The
results are also used to assess the precisian arid accuracy^of the analytical
methods for specific analytes.
9.2 Sample sets may be provided to particip^ting^^Gontr^ctors as frequently as
on an SDG-by-SDG basis as a recognizable QC saiitp^.e of Imown composition; as a
recognizable QC sample of unknown composition; orn<^t rec^sgnizable as a QC
material. The laboratory evaluation samples may be s&Bt either by the
Regional client or the National Prog^am^ Of f ice, and may bexusedy' f or contract
action.
9.3 Contractors are required to ana^yzk the s
package and all raw data within the contract
re,
>lesand return the data
ifuiired^turraround time.
9.4 At a minimum, the results are eval
quantification, and sample contamination.
quantification of target
population statistics. E
evaluation sample to com'
particular sample. No
sample are not specifi
to use the NIST/EPA.
maximum number of
a minimal response
contractually described"
integrated into the
a frict
listed/in
/mass spe.ctr
coi
jectral
compound identification,
ontAdence intervals for the
are based\pn imported values using
adjust the scoresx>n any given laboratory
r unariticipate^l difficulties with a
c^jopounds spiked into the
,t. Contractors are required
tentatively identify a
raction that are present above
of these compounds based on
nterpretation procedures is evaluated and
the
com
li&r
ids in eacr
tification
evaluates
prc
9.5 A Contractor's resuT&&xon theNl.abor^tory evaluation samples will
determine the/Coivei'Sctoi^s pebformanceXae follows:
9.5.1 /6o Response is req\ire>d for a score of 90 percent or above.
a score of 75 toj 891 the Contractor shall describe the
;) and the corrective action(s) taken in a letter to the APO,
within & days of receipt of notification from EPA.
9.5.3 For a scb« les's/thah 75, the Contractor shall be notified by the
APO or TPO concerning the/remedy for its unacceptable performance. The
December, 1991
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Exhibit E
VGA of Ambient Air on Tenax®
Contractor may expect, but EPA is not limited to, the fallowing actions:
reduction of the number of samples sent under the confctac^, suspension of
sample shipment to the Contractor, a site visit, a full data audit,
analysis of remedial PE samples, and/or a contract s4nc/tion, such as a
Cure Notice.
ctive action
act
NOTE: A Contractor's prompt response demonstrating/t
has been taken to ensure the Contractor's capab/liity to m
requirements will facilitate continuation of fu^l/sample
December, 1991
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 10
GC/MS TAPE AUDITS
10.1 Periodically, EPA requests from Contractors the7 G
corresponding to a specific Case in order to accomplis
Generally, tape submissions and audits are requested for the fol
reasons:
Program overview;
Indication of data quality problems fronEMSL/Ly; Sm.0, or Regional
data reviews;
Support for on-site audits; and
• Specific Regional requests.
10.2 Depending upon the reason for an audit, the tapes^&pm a^ecent Case, a
specific Case, or a laboratory eva]jtfii£lon-&am|>le may *>e reqvte^ted. Tape
audits provide a mechanism to assess adherenceto~~coBtr^ctual requirements and
to ensure the consistency of data rapor\e3^STr--fehe hardcopywith that generated
on the GC/MS tapes. This function provides ext«ra£"~fiRmitOTing of Program QC
requirements and checks adherence of the Contractor to internal QA procedures.
In addition, tape audits enable EPA to e\alua/e ^he utility, precision, and
accuracy of the analytical methods.
10.3 The GC/MS tape shalL/includeNraw data aHd qWntitation reports for
samples, blanks, laboratory evaivatiim samplesXinrtial calibrations,
continuing calibration,/and/BFB astocliaTe^with ohet Case requested. The
specific requirements ^or/submissions o£ GC/MS^tapes are discussed in Exhibit
B.
10.4 Upon request 6f the
required tapes and all
within seven (7) days of nt
Lst^ative Project Officer or EMSL/LV, the
iocumentation shall be submitted to EPA
December, 1991
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Exhibit E
VGA of Ambient Air on Tenax®
SECTION 11
ON-SITE LABORATORY EVALUATIONS
11.1 At a frequency dictated by a contract laboratory
Administrative Project Officer, Technical Project
representative will conduct an on-site laboratory
laboratory evaluations are carried out to monitor
meet selected terms and conditions specified in
process incorporates two separate categories:
and an Evidentiary Audit.
/ua
lance, the
authorized
11.2 QUALITY ASSURANCE ON-SITE EVALUATION
11.2.1 Quality assurance evaluators yhspeSst the £onlzractor's facilities
to verify the adequacy and maintenanceiaf instrumentation, the continuity
of personnel meeting experience or education requij-ements, and the
acceptable performance of analytical and QC pria^edure^. The Contractor
should expect that items to be monitored will include but^not be limited
to the following items:
Bench sr?
Review of the
proced
Size and appearance of\th<
Quantity, age, availabili
of instrumentation;
Availability, appropriateness,N
Staff qualifi$
Reagents, st
Standard /ret
mce and performance
tilization of SOPs;
ersonnel training programs;
facilities;
data;
cical logbook maintenance and review, and
r's sample analysis/data package inspection
evalua<^6n, various documentation pertaining
ic Contractor is integrated in a profile
the evaluation. Items that may be included
.aboratory evaluation sample scores,
.1 QA materials, GC/MS tape audit reports,
December, 1991
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Exhibit E
VOA of Ambient Air on Tenax®
11.3 EVIDENTIARY AUDIT
11.3.1 Evidence auditors conduct an on-site laboratory/evaluation to
determine if laboratory policies and procedures are' in/place to satisfy
evidence handling requirements as stated. The ev^dence^dit is comprised
of the following three activities.
11.3.1.1 Procedural Audit
The procedural audit consists of review/and examination
standard operating procedures and accompanying documentation forthe
following laboratory operations:
Sample receiving;
Sample storage;
• Sample identification;
Sample security;
• Sample tracking (
Analytical project
11.3.1.2 Written SOPs Audit
The written SOPs
written SOPs to
following labor
sample identif^dat^bn
to completion
and assembly
11.3.1.3
The analytica
examination_pf the
audito
tion of analysis); and
sembly.
veview and examination of the
te and complete for the
eiving, sample storage,
le tracking (from receipt
project file organization
Iden
:t File Evidence Audit
file evidence audit consists of review and
project file documentation. The
:o determine:
document inventory;
e file;
acy of the document numbering system;
'sample activity;
of activity recorded on the documents; and
December, 1991
Page E-36
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Exhibit E
VOA of Ambient Air on Tenax®
Error correction methods.
11.4 DISCUSSION OF THE ON-SITE TEAM'S FINDINGS
The QA and evidentiary auditors discuss their findings with the
Administrative Project Officer (APO)/Technical Project Officer (TPO) prior
to debriefing the Contractor. During the debriefing^ ^tiie au&i^ors present
their findings and recommendations for corrective actionsTiecessaf chefirrcti^g or^withi^the time agreed
upon between the APO/TPO and the Contractor,
11.5.2 If the Contractor fails to
resolve the deficiencies discussed in fche
may expect, but the Ageney—rs-jiot limited
reduction of the
suspension of
a follow-up
ipriate corrective action to
ori-site reports, a Contractor
to\ the following actions:
the contract;
analysis of rem<
Cure Notice.
actor;
t; and
tples and/or contract sanction, such as a
December, 1991
Page E-37
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 12
QUALITY ASSURANCE AND DATA TREND ANAL'
addition, QC prescrlrtjed/ in
y used by the Agency to
y and Etxjeram data quality
iplisheo/by/entering data into
12.1 Data submitted by laboratories are subject to
aspects: compliance with contract-required QC, usabifli
package evaluation. Problems resulting from any o
determine the need for a GC/MS tape audit, an on-
and/or a remedial laboratory evaluation sample. /I
the methods provides information that is continua
assess sample data quality, Contractor data qu4l
via data trend analysis. Trend analysis is
a computerized data base. Statistical reports/that evaluate specific
anomalies or disclose trends in many areas/ iricluding/the/following, are
generated from this data base:
Laboratory Control Sample;
• Blanks;
GC/MS Instrument Performan>
Initial and Continuing Calib
Other QC and Method Parameters.
12.2 Program-wide statistic
to observe the relative perTormanc
against its peers. The repoi?es-a>re
laboratories . The resuVts /of many\ o
overall evaluation of
determine if correcti;
indicated in order
12.3 Contractor perf
techniques to detect
levels of QC, and to provide
which may not
12.4 As a
information' neded to estabrfcsh
analytica
vast empiricl data set producera.
itn^^he results augmen
rank laboratories in order
using a given protocol
ntify trends within
'analyses are included in
and are reviewed to
ratory evaluation is
s of the contract.
/er/time is monitored using these trend analysis
^Contractor output from required or desired
swarning of Contractor QA/QC problems
.results of an individual'case.
performance^
Program, the data base provides the
rformance -based criteria in updated
ry criteria have been previously used. The
contract laboratories is carefully
ng theoretical and research-based
is a continuously monitored set of QC and
performance criteria specifications of what is routinely achievable and
expected of envirohmentalxcJiemLstry laboratories in mass production analysis
December, 1991
Page E-38
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Exhibit E
VGA of Ambient Air on Tenax®
of environmental samples. This, in turn, assists the Agency^in meeting its
objectives of obtaining data of known and documented qualicy.
December, 1991
Page E-39
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Exhibit E
VOA of Ambient Air on Tenax®
SECTION 13
DATA MANAGEMENT
13.1 Data management procedures are defined as procedures s
acquisition or entry, update, correction, deletion,
computer readable data and files. These procedures
and contain a clear definition for all databases a
resubmit deliverables. Key areas of concern inc
(including personnel and security), docuraentati
quality control.
13.2 Data manually entered from hard-copy
error rates estimated. Systems should prev>
out-of-range data and alert data entry pe
entry error rates must be estimated and re
reentering a statistical sample of the data e
discrepancy rates by data element.
erations,
.edifying the
curity of
ten form
te or
tion^
'and
ontrolled and the
orrect or
's. In addition, data
thly basis by
calculating
13.3 The record of changes in the form of corrections ahdupdktes to data
originally generated, submitted, aiyC^~~r^tubjiiitted must be^dgcumented to
allow traceability of updates. DocumeoEation mus~C~~i«cJjide the following for
each change:
Justification or rationale
Initials of the person making the
must be implemented and—reviewed byN
the source generat
13.4 Li
systems
deliverable
utilization
or changes. Data changes
son or group independent of
Change document
original deliv
Resubmitted
part of the
resubmission
inspected;
The
delivi
Do
Lab
ioed acCxo/ding to the schedule of the
les must be reinspected as a
inspection process prior to
'deliverable, not just the changes, must be
e changes to originally submitted
ges may be requested by laboratory auditors.
es must be applied to computer software
to be used to generate and edit contract
e thoroughly tested and documented prior to
December, 1991
Page E-40
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Exhibit E
VGA of Ambient Air on Tenax®
A software test and acceptance plan including test requirements, test
results and acceptance criteria must be developed,/followed, and
available in written form. / /
/ /
System changes must not be made directly to production systems
generating deliverables. Changes must be made/first'So a development
system and tested prior to implementation. "^
Each version of the production system willda^tinland quality
control; and
Data and system security, b
December, 1991
Page E-41
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Exhibit E
VGA of Ambient Air on Tenax®
SECTION 14
REFERENCES
14.1 Fisk, J.F. and Manzo, S.M. "Quality Assurance^/Qualitsv Control in
Organics Analysis", Proceedings from the Water Pollujfioty^SQntrolxpederation
Meeting, May 1986.
14.2 Office of Monitoring Systems and Quality
Protection Agency, "Interim Guidelines and Speci/£i
Quality Assurance Project Plans", QAMS-005/80,/TJec^mber 1980.
14.3 Office of Solid Waste and Emergency esjonse,
Protection Agency, Test Methods for Evaluating/Solid
SW-846, November 1986.
U /S. .Environmental
Third Edition,
14.4 Laidlaw, R.H., "Document Control and cbain of Custody Considerations
for the National Contract Laboratory Program," Quality Control in Remedial
Site Investigations: Hazardous and Industrial SolidSjaste^Testing, Fifth
Volume, ASTM STP 925, C.L. Perket, ed., American Society^srat^ry7
Agency, Manual of Analytical Methods^or
and Environmental Samples, EPA-600/8-86k-03"
Environmental Protection
he A.njCLydis~~o£~~£&s tic ides in Humans
ie/1980.
14.6 Environmental Protection Agency, NSuideiines Establishing Test
Procedures for the Analysis o£-Eollutants UhderNthe Clean Water Act; Final
Rule and Interim Final RuLeand Proposed Rule\, 4S CFR Part 136, Federal
Register, Vol. 49, No. 209. ,/pp-s^323\-43442, Od^obeY 26, 1984.
14.7 Health Effects/Research
Agency, Manual of Analytical Qua..
Compounds In Human and Ejwiroi
EPA-600/2-81-059, ,
moratory, Tk^S-^nvironmental Protection
Lty/Control for/Pesticides and Related
\ta.J Samples^Second Revision,
14.8 Environmental Monit-or ing ^Systems Laboratory, U.S. Environmental
Protection Agency,_Analytical>Refer^ce Standards and Supplemental Data: The
Pesticides and^Ifidustr7al>ChemicaSs^ Repository, EPA-600/4-84'-082, October
1984.
14.9 American Chemical Soblet\ Committee on Environmental Improvement, and
SubcommitjZee An EnvironmentalVnalytical Chemistry, "Guidelines for Data
Acquisition &nd Data Quality Evaluation in Environmental Chemistry",
Analytical Che^wLstry, Volume 5i, Number 14, December 1980.
14.10 Moore, JvM. an&^J>earscfn, n .G. "Quality Assurance Support for the
Superfund ContracbsLabora^Xy program", Quality Control in Remedial Site
Investigation: Hazar<3
-------
Exhibit E
VGA of Ambient Air on Tenax®
ASTM STP 925, C.L. Perket, ed. , American Society for Testin^and Materials,
Philadelphia, 1986.
December, 1991
Page E-43
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December, 1991
-------
EXHIBIT F
EVIDENTIARY REQUIREMENTS
TABLE OF CONTENTS
SECTION 1 SAMPLE CHAIN-OF-CUSTODY
1.1 SAMPLE IDENTIFICATION
1.2 CHAIN-OF-CUSTODY PROCEDURES
1.3 SAMPLE RECEIVING PROCEDURES
1.4 SAMPLE TRACKING PROCEDURES
SECTION 2 DOCUMENT CONTROL PROCEDURES
2.1 PREPRINTED LABORATORY FORMS AND LOGBOOKS
2.2 CONSISTENCY OF DOCUMENTATI'
2.3 DOCUMENT NUMBERING AND INVENTOEX PROCED
2.4 STORAGE OF EPA FILES
2.5 SHIPPING DATA PACKAGES AND CS
NO.
SECTION 3
3.1
3.2
STANDARD OPERAT.
SPECIFICATIONS
STANDARD OPERATING/lPROCEfcURflS,
HANDLING OF C/NFTOENTIAL INFO]
10
12
December, 1991
-------
Exhibit F
VOA of Ambient Air on Tenax®
SECTION 1
SAMPLE CHAIN-OF-CUSTODY
A sample is physical evidence collected from a facfi
environment. An essential part of hazardous waste invest
that the evidence gathered be controlled. To accomp
sample identification, chain-of-custody, sample rec
procedures have been established.
1.1 SAMPLE IDENTIFICATION
1.3
from • *
fforc is
llowing
eking
1.1.1 To assure traceability of samples/while in pesss^ssion of the
Contractor, the Contractor shall have a specified me/cho^ for maintaining
identification of samples throughout th/ lafcoratoi
1.1.2 Each sample and sample preparatibr^concaaner shall be labeled
with the EPA sample number or a unique laboratory identifier. If a
unique laboratory identifier is used, it shall oexcrossxreferenced to the
EPA sample number.
1.2 CHAIN-OF-CUSTODY PROCEDURES
theXdata
1.2.1 Because of the nature o:
of EPA samples must be traceable
until they are introduced as evidenc
Contractor shall have procedures ensuring
maintained and documented.
Lne
in
d, the custody
ie tj/me/fche samples are collected
proceedings. The
'th/t EPA sample custody is
1.2.2 A sample is mider^coistody if the fa.lloVj.ng applies:
1.2.2.1 It is in/your possession.
1.2.2.2 It is /.n /our view/after beiitgs4j/your possession.
1.2.2.3 It was'^tD your~vp6ssession and you locked it up.
1.2.2.4 It is in a desl^gnateiKsecure area (secure areas shall be
accessible jKfaunt&sized pet«pnnelXpnly).
SAMPLE
1.3.1
for r
esignate a sample custodian responsible
1.3.2
samples in
condition of
esignate a representative to receive
he/sample custodian is not available. The
containers and sample bottles shall be
December, 1991
Page F-l
-------
Exhibit F
VOA of Ambient Air on Tenax®
inspected upon receipt by the sample custodian or his/her .representative.
1.3.3 The condition of the custody seals (intact/ytot /Intact) shall be
inspected upon receipt by the sample custodian or
1.3.4 The sample custodian or his/her represei
the presence or absence of the following documei;
sample shipment:
1.3.4.1 Airbills or airbill stickers.
1.3.4.2 Custody seals.
1.3.4.3 EPA cus tody records.
1.3.4.4 EPA traffic reports or SAS pi
1.3.4.5 Sample tags
~ er
1.3.5 The sample custodian or
date all forms (e.g., custody
and airbills) accompanying the
sign and
acking lists,
.mple receipt.
1.3.6 The Contractor shall contact"^SMO ta/re^olve^rr^crepancies and
problems such as absent documents, confiicttlng; information, broken
custody.seals, and unsatisfactory sample condition (e.g., leaking sample
bottle).
1.3.7 The Contractor shall refc^rd
problems on Teleph
1.3.8 The following/ information
the sample custodian/or his/tv
and inspected:
ion of discrepancies and
corded on Form AADC-1 by
:e as samples are received
1.3.8.1 Conditio
1.3.8.2 P
and/or s
lipping container.
condition of custody seals on shipping
snumbers, when present.
nple bottles.
of airbills or airbill stickers.
ai/bilA sticker numbers.
December, 1991
Page F-2
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Exhibit F
VOA of Ambient Air on Tenax®
1.3.8.7 Presence or absence of EPA custody records.
1.4
1.3.8.8 Presence or absence of EPA traffic reports
lists.
1.3.8.9 Presence or absence of sample tags.
1.3.8.10 Sample tag identification numbers cr/
sample numbers.
1.3.8.11 Verification of agreement or non?
recorded on shipping documents and sample/coj/tainersx
1.3.8.12 Problems or discrepancies.
SAMPLE TRACKING PROCEDURES
packing
EPA
The Contractor shall maintain records doc
handling from receipt to final analysis. The recor
documentation of the movement of samples and prepared
designated laboratory storage areas.
11 phases of sample
include
and out of
December, 1991
Page F-3
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Exhibit F
VGA of Ambient Air on Tenax®
SECTION 2
DOCUMENT CONTROL PROCEDURES
The goal of the laboratory document control program^is tbxassure that
all documents for a specified SDG will be accounted for /hehxrtie pisoject is
completed. Accountable documents used by contract Vaboratories^hallXnclude
but not be limited to logbooks, chain-of-custody re
bench sheets, and other documents relating to the/sample or sample
The following document control procedures have been/established to assure^that
all laboratory records are assembled and stored/for delivery to the EPA or are
available upon request from the EPA prior to phe ^delivery/schedule.
2.1 PREPRINTED LABORATORY FORMS AND LOGBOC
2.1.1 All documents produced by the Cbqtracbar whach are directly
related to the preparation and analysis of E£A samples shall become the
property of the EPA and shall be placed in thesftQmplebe^sample delivery
group file (CSF). All observations and results rebardediyjc'the
laboratory but not on preprintecL-iaboratory forms shalS^be Centered into
permanent laboratory logbooks. /WhenaHr^Ata^frpm a SDG are compiled,
all original laboratory forms and swpi^sof aliSUGT^alated logbook
entries shall be included in the\doc\tmentatT9n naskage.
2.1.2 The Contractor shall identify
laboratory documents which is direct!^
analysis of EPA samples.
ie/act:ivity recorded on all
related to the preparation and
2.1.3 Pre-printed Laboratory^orms shal\ contain the name of the
laboratory and be dazed Xmon^hydaV/year) andysigned by the person
responsible for per/ormlng the )activity-v§t thX/time an activity is
performed.
2.1.4 Logbook/entrees shall
the person responsible ror /per,
activity is performed
dated (month/day/year) and signed by
forming the activity at the time an
2.1.5 Logbpefc—entries sh
logbooks, vith the exce>^ion o
shall incXude^-6nTy~>ne SDG\er pa£
chronological order. Entries in
nstr;bment run logs and extraction logs,
2.1.6 / P/ges in both
numbe/ed,
id unbound logbooks shall be sequentially
the
the
Instrument run log's snail be maintained so as to enable a
the run,4equence of individual instruments. Because
laboratory mustxgrovfde /copies of the instrument run logs to the EPA,
laboratoryms^ exet«ise/the option of using only laboratory or EPA
December, 1991
Page F-4
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Exhibit F
VOA of Ambient Air on Tenax®
sample identification numbers in the logs for sample ID/:
government agency or commercial client names to preserve
confidentiality of commercial clients.
2.1.8 Corrections to supporting documents and ra»fr da%a shall be made
by drawing a single line through the error and entering tnexcorrect
information. Corrections and additions to supporting dbcumenfcs^and raw
data shall be dated and initialed. No informat/on/shall be\obliterated
or rendered unreadable. All notations shall b.eXrgcorded in ink-^ Umlsed
portions of documents shall be crossed out.
2.2 CONSISTENCY OF DOCUMENTATION
2.2.1 The Contractor shall assign a d^ci
responsible for the organization and
2.2.2 All copies of laboratory documet
legible.
bnt control/officer
Ly of th4 QSF.
;s shsiY be/complete and
2.2.3 Before releasing analytical results, the TlBQumentxeontrol
officer shall assemble and cross^ctieck the informatioi^xm sample tags,
custody records, laboratory bench shee"E3~7-~pet£onal and instrument logs,
and other relevant data to ensure Khat^data pertalrttng-io each particular
sample or sample delivery group is c^nsistenT? thtojughouv the CSF.
2.3 DOCUMENT NUMBERING AND INVENTORY
2.4
2.3.1 In order to provide document a\coui(t;ability of the completed
analysis records, each iCSnTTnva CSF shall bexinventoried and assigned a
serialized number as described Da Exhibit \, Section 2.
CSF # - Region -
nent
2.3.2 All doc
bench sheets, m
preparation recor'
analysis, custody re
inventoried.
2.3.3
ensuring
and are
plasti
document
STO:
llized n)omBer(Flx^ exantple: 75-2-0240).
relevant c6 eacfN§DG,/including logbook pages,
s s>e^tra, >chrcraiatograms, screening records, re-
re>snj(lysiis records, records of failed or attempted
rds, library research results, etc., shall be
The Contrac
location.
(DCO) shall be responsible for
generate/a are placed in the CSF for inventory
The DCO shall place the sample tags in
:ure E-l of Exhibit E is an example of a
nta.i.u EPA laboratory documents in a secure
December, 1991
Page F-5
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Exhibit F
VGA of Ambient Air on Tenax®
2.5 SHIPPING DATA PACKAGES AND CSF
2.5.1 The Contractor shall document shipment of deli'werabies packages
to the recipients. These shipments require custody/sea&s on the
containers placed such that they cannot be opened ywithout'iiamag ing or
breaking the seal. The Contractor shall document whatN^s seh<, to whom,
the date, and the method (carrier) used.
2.5.2 The Contractor shall purge the CSF
appropriate EPA Region 180 days after the r
arable to the
submission.
2.5.3 A copy of the transmittal letter
NEIC and SMO.
2.5.4 The Document Control form is
inspection of shipping containers and
submit one original FORM AADC-1 for each
2.5.5 The Contractor shall sign and date the
examine the shipping containers, ^.record the presence
custody seals and their conditio
2.5.6 The Contractor shall
follow the instructions explained
1 be sent to
2.5.7 The Contractor shall submit
with each SDG package.
the receipt and
ontractor shall
present)
ice of
samples and
g-In Sheet.
:ed Document Control Form
December. 1991
Page F-6
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Exhibit F
VOA of Ambient Air on Tenax®
SECTION 3
STANDARD OPERATING PROCEDURES
The Contractor must have written standard operating p^
for receipt of samples, maintenance of custody, sample/ identi
storage, tracking the analysis of samples, and asse
3.1 SPECIFICATIONS FOR WRITTEN STANDARD OPERATI!
3.1.1 An SOP is defined as a written nartfati
description of laboratory operating proce
laboratory documentation. The SOPs must
procedures used in the laboratory, and oopi^s of
be available to the appropriate laborapory/personn;
are necessary to ensure that analytical- datS
are acceptable for use in EPA enforcement^case
litigation.
(SOPs)
ition, sample
data.
DCEDURES
e step-by-step
including examples of
cibe the actual
tten SOPs shall
These procedures
under this contract
operation and
3.1.2 The Contractor's SOPs shall provide mecharti^ms ahd documentation
to meet each of the following specifications and shalt-^e used by EPA as
the basis for laboratory evidence audits":—Ihe^ContractorNnust have
written standard operating proc
Sample receipt and log
Sample storage.
3.1.2.1
and logbooks.
data control systems.
.nageriai/review of laboratory operation and
contractually-required quality assurance
each individual data package.
ata handling, and reporting.
December, 1991
Page F-7
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Exhibit F
VOA of Ambient Air on Tenax®
3.1.2.12 Chain-of-Custody.
3.1.2.13 Document control, including Case file pr«
3.1.3 The Contractor shall have a designated
responsible for receipt of samples and have writ^
his/her duties and responsibilities.
3.1.4 The Contractor shall have written S0?s
in of the samples. The procedures shall in<
documenting the following information:
3.1.4.1 Presence or absence of EPA c
3.1.4.2 Presence or absence of air
3.1.4.3 Presence or absence of EPA Traf
lists.
orms.
stickers.
s or SAS packing
3.1.4.10 Verifi
receiving doc
3.1.4.11 Resolutio'
3.1.4.12 T
upon rece
but not be limited
3.1.4.4 Presence or absence of^custody seals on sh:
containers and their conditioi/
3.1.4.5 Custody seal numbers,
3.1.4.6 Presence or absence of s
3.1.4.7 Sample tag ID numbers.
3.1.4.8 Condition
3.1.4.9 Conditio
and/or sample
tion
;reement of information on
(ems or discrepancies with SMO.
nn.s used to describe sample condition
,hal\ have written SOPs for maintenance of the
n and shall demonstrate security of the
reas. The SOPs shall specifically include
as for EPA samples in the laboratory, and
ontamination. The SOPs shall include a
list of ati^hori^ad personnel Who have access or keys to secure storage
areas.
December, 1991
Page F-8
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Exhibit F
VGA of Ambient Air on Tenax®
3.2
3.1.6 The Contractor shall have written SOPs for trac
performed on any particular sample. The tracking SOP
following:
ig the work
include the
3.1.6.1 A description of the documentation used/to record sample
receipt, sample storage, sample transfers, sampl/ preparations, and
sample analyses.
3.1.6.2 A description of the documentation,
calibration and other QA/QC activities.
to record ihfitrume
3.1.6.3 Examples of the document format/ anfl. laboratory documentation
used in the sample receipt, sample storage,/sample ^ratjsfer, and sample
analyses.
3.1.7 The Contractor shall have written iJQPs for maintaining
identification of EPA samples throughout^the -laboratory.
3.1.8 If the Contractor assigns unique laborktQry identifiers, written
SOPs shall include a description of the method useoN^o assign the unique
laboratory identifier and cross-j?e£ej:ence to the EPA sample/number.
3.1.9 If the Contractor uses\Dre-ftst*s^orsuffixe^~ii»--a/ddition to
sample identification numbers, tne widttenSDPs/shall include their
definitions. The Contractor shall\havte writttetr SOPs3escribing the
method by which the laboratory maintXins\sa'mp]^es under custody.
3.1.10 The Contractor
assembly of all documen
and managerial review
basis. The procedure's
pages, sample tracking
printouts, raw dat
documents having /ef<
submission to EPt
inventory procedu
shall have writcen SfoPs for organization and
relating to eacb EPA Case, including technical
Documentk shall beNfiled.on a Case-specific
fst ertfiura thiat all ck>cuments including logbook
Lecords ,) cHromatographiV charts, computer
laries,/corpes^ondertee-j and any other written
ence to/the/Case ase c/mpiled in one location for
system must include a document numbering and
3.1.11 The Contractor shall fia^e written SOPs for laboratory safety.
3.1.12
used in
Contractor^shall
p/eparing
written SOPs for cleaning of glassware
.nalWing sam>ies under this contract.
TWe Contractor snsll \iave SOPs for traceability of standards
HANI
jrn aample analysis QA/DC.
KG OPvqoNFIDENTIAL ZNFC
3.2.1 A Con
-------
Exhibit F
VOA of Ambient Air on Tenax®
doc,
EPA-designated confidential information from the Agenc
information must be handled separately from other
under this contract. To accomplish this, the folio
the handling of confidential information have been
3.2.2 All confidential documents shall be und<
designated Document Control Officer (DCO).
Confidential
tation developed
edures for
Lished.
3.2.3 Any samples or information received
confidentiality shall be handled as "confid<
file shall be maintained to store this
segregated from other nonconfidential inf<
confidential samples shall be treated as,
confidential information, the DCO logs
Confidential Inventory Log. Tl. Lnfo
authorized personnel but only a:• ?r it
by the DCO. The documents shal. be returne
a request of
ll." A separate
;ion and shall be
;ion. 9^*> generated from
fidential. /Upon receipt of
documents/into a
aade available to
out to that person
locked file at the
conclusion of each working day. Confidential "tHformabipn may not be
reproduced except upon approval by the EPA Contracting Or^cer. The DCO
will enter all copies into the document control systeiJh^In/addition,
this information may not be disposed"of-~excej>tupon approval by the EPA
Contracting Officer. The DCO shal^h-^ejiiove andreTcaitft--Che cover page of
any confidential information disposed ofTor^one^year ana shall keep a
record of the disposition in the Confidential /nventory Log.
December. 199L
Page F-10
-------
December, 1991
-------
EXHIBIT G
GLOSSARY OF TERMS
Aliquot - A measured portion of a field sample taken for analysis.
Analysis Date/Time - The date and military time (24-biourclocsiO of the
introduction of the sample, standard, or blank into/th ahalysis^ystem.
Analysis Group - An analysis group is a set of noSao^e than twenty^anaty^ical
sair.rles (as defined below) for the purpose of merh&ri Quality Assurance/Quality
Control (QA/QC), such that the QA/QC required by Exhibits D and E are,
minimum, prepared and analyzed at a frequency/ofyonce per twenty analytical
samples.
Analytical Sample - Any solution or media/Introduced /nto7 an instrument on
which an analysis is performed excluding^rnstrament ^calibration, initial
calibration verification, initial calibration blahto( continuing calibration
verification and continuing calibration blank^xNote ^tje following are all
defined as analytical samples: field samples, dujJi4.catev>«amples, laboratory
control sample (LCS), and performance evaluation
•\STM Type II Water - Distilled wa
^mho/cm at 25°C. For additional
"Standard Specification for Reagent
Autozero - Zeroing the instrument at t'
to running, a standard blank with the abs"
Background Correction - A teetiriltj^e to compJ
contribution to the instr/ument sigr
uctivity
Batch - A group of sam
Breakthrough volume
will be initially
Calibration - The estab
absorbance, emission i
standards. Cali
this document
that method.
Calibrati
analyst
curve).
the same"
of Ttess than 1.0
JTM D1193-77,
It is equivalent
for variable background
.ete\mination of trace elements.
intens
h point a particular component
fronTthe Tenax® sample cartridge.
an analytical curve based on the
ther measured characteristic of known
er for the various methods included in
methdd^of interest for a definition specific to
of known standard solutions used by the
trument (i.e., preparation of the analytical
jected to the preparation method but contain
arations to be analyzed.
December, 1991
Page G - 1
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Exhibit G
VOA of Ambient Air on Tenax®
Case - A finite, usually predetermined number of samples collected over a
given time period from a particular site. Case numbers arie assigned by the
Sample Management Office. A Case consists of one or more/Sap(ple Delivery
Groups.
Coefficient of Variation (CV) - The standard deviatio:
arithmetic mean.
Continuing Calibration Standard - A standard solution
to be used to verify the stability of the instr
the instrument performance during the analysis
calibration standard should have a concentrati
calibrated range. Analytical standard run
every 12 hours, whichever is more frequent,
analytical system.
the middle of the
al sansL les or
libration of the
Contract Required Quantitation Limit (CRQL
acceptable under the contract Statement of
more) times the standard deviation of seven replf
blank.
Control Limits - A range within whi
to be compliant. Control limits
if exceeded, or advisory, requiring
lyst
time^nd
Correlation Coefficient - A number (r)
dependence'between two variables (e.g.,
dependent they are the closer the value
least squares line.
Cryogen - A liquified ga
cryogenic trap of the ai
(bp - 195.8 CC).
el of quantitation
defined as 3.3 (or
ses of the method
;ults must fall
corrective action
flagged.
ates the degree of
trtion - absorbance). The more
Determine -on the basis of the
tmperatures in the
cryogen is liquid nitrogen
Data System - For t
the continuous acqu
the chromatographic pr$
Day - Unless othe
DDI - Deionized
Deuterated
isotope t;
quality stssw
computer system that allows
tout of time vs intensity data throughout
hall mean calendar day.
cals which contain deuterium (hydrogen
tydrogen); used as tracers for system
December, 1991
Page G - 2
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Exhibit G
VOA or \mbient Air on Tenax®
Field Blank - Any samp" submitted from the field identif
Field Sample - A portion of material received to be ana
in single or mu]f- _e containers and identified by a u
s a blank.
that is contained
EPA Sample Number.
Holding Time - The elapsed time expressed in days from
the sample by the Contractor until the date of its
In-House - At the Contractor's facility.
Initial Calibration - Analysis of analytical s
different specified concentrations; used to defi
range of the response of the analytical ins
Interferents - Substances which affect th<
interest.
Internal Standards -Compounds added to every
known concentration, prior to analysis. Internal s"
basis for quantitation of the target analysis.
f receipt of
Laboratory - Synonymous with Cont
Laboratory Control Sample (LCS)-
specific compounds and subjected to
to monitor method and contractor perfo
Laboratory. Method Blank (LMB)^_Aclean unv
and performing the same analytical
cartridge never leaves
Laboratory Receipt Da
Contractor's facilit
sample Traffic Repo
receipt).
;iards for a series of
^earity and dynamic
garget compounds.
e compound of
, sample at a
are used as the
concentration of
ire/ analytical procedure in order
analyzed along with
e field samples. The LMB
le is received at the
's delivery receipt and
(validated time of sample
Linear Range - The concents^tion^-range over which the analytical curve remains
linear. The range of the ins^&rumervtNsfor a specific compound, as determined
using calibratLe»n^stan3aT«4s. Tnexuppervlimit of this linear range (determined
at each analysis)-is—the higitest corteencration calibration standard that has a
determined valufiTwithinrQX of\the known value.
Mass Spec
standard/qu,
"noise
ied as the inability to detect the internal
.presence of high levels of mass spectral
December, 1991
Page G - 3
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Exhibit G
VGA of Ambient Air on Tenax®
Matrix - The predominant material of which the sample to be,-analyzed is
composed.
Megabore® Column - One of two types of capillary column
narrow bore, for the analysis of target compounds unde
the other being the
contract.
Method Detection Limit (MDL) - The chemical concentr/ti
signal, due to an analyte, which is equal to the s
standard deviation of a series of measurements on
method blanks. In practice, a method detection
higher than an instrumental detection limit. T\/ie
metals is t 99 times the standard deviation of
Of course, all spectral background techniques/
integration times must be utilized as when
MS-SCAN - The gas chromatograph (GC) is c
where the instrument is programmed to acqui
and to disregard all others.
derft t 99 times tit
east seven s«parat
will be
thod detection
method blank analyses.
ive and the same
e analyzed.
Narrative (SDG Narrative) - Portion of the data packag^e^whichxincludes
laboratory, contract, SDG and samplenumber identificationvand?descriptive
documentation of any problems encoyntered^~rn-piacessing the samples, along
with corrective action taken and pxx>bl-e«urjesolution"? €eaplete SDG Narrative
specifications are included in Exhibit
selective detector
target compounds
Narrow-Bore Capillary Column - One of
the wide-bore (Megabore®) capillary colt
under this contract.
Performance Evaluation
EPA for Contractor analy,
Protocol - A compilat}
sample receipt and h
deliverables, and
Qualitative Accuracy
identify compounds.
Quantitative A]
measure the
Reconstruc
represent,
total io;
Sample \^A sample^of Known composition provided by
bjf EPA to evXlua\e Contractor performance.
V
.followed with respect to
data reporting and
columns, the other being
:he analysis of compounds
of an analytical system to correctly
analytical system to correctly
d compound.
C) - A mass spectral graphical
|Chieved by a gas chromatograph; a plot of
time.
December, 1991
Page G - 4
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Exhibit G
VGA of Ambient Air on Tenax®
Recovery - A determination of the accuracy of the analytic
comparing measured values for a fortified (spiked) sampl^
spike values. Recovery is determined by the following
rocedure made by
inst the known
ion:
%Recovery = measured value
spiked value
x 100%
Relative Response Factor (RRF) - A measure of the
response of an analyte compared to its internal
Factors are determined by analysis of standards/an^
calculation of concentrations of analytes in
the following equation:
RRF =
C;
Ais
area of the characteristic
concentration;
internal standard; and
compound of interest.
where: A
C
is
x
Resolution - Also termed separati
chromatogram, calculated by dividi:
peaks by the peak height of the smal
100.
Retention Time (RT) - The time to elute a
chromatographic column for a^sp^cific carrier
time the chemical is injected into
concentration appears at/the/'de'&e.ct
peaks on a
between the
multiplied by
chemical from a
flow rate, measured from the
until its maximum
Retention Time Window / Retention /time windbw^is determined for each compound
of interest and is the tfme f rom /inj ee'tibrvto eHition of a specific chemical
from a chromatographac qolumn. yrhe/window is-^determined by three injections
of a single component stahdard /over a 24-hour period as plus or minus three
times the standard devlba.tion'Wr' t#e absolute retention time for that: compound.
Rounding Rules - If_the figurexfoll&wirig those to be retained is less than 5,
the figure is dropped" atrd^the reNfcainea*vf.igures are kept unchanged. As an
example, 11.443 ig-H?e«nded o&f to
se to be retained is greater than 5, the
ast retained figure is raised by 1. As an
ff to 11.45.
followirt
and
round
following
If
'se to be retained is 5, and if there are no
December, 1991
Page G - 5
-------
Exhibit G
VOA of Ambient Air on Tenax®
figures other than zeros beyond the five, the figure,-§. is dropped, and
the last-place figure retained is increased by one iT i^ is an odd
number or it is kept unchanged if an even number. /As /an example, 11.435
is rounded off to 11.44, while 11.425 is rounded pff/to 11.42.
If a series of multiple operations is to be per/formed
divide, multiply), all figures are carried thcou;
Then the final answer is rounded to the proper number o
figures.
See forms instructions (Exhibit B) for e
Run - A continuous analytical sequence consi
associated quality assurance measurements a
subtract,
lations.
Sample - A portion of material to be analyzed
multiple containers and identified by a un
d samples and all
'is contract.
contained in single or
iber.
Sample Delivery Group (SDG) - A unit within a sampSLe Casfexthat is used to
identify a group of samples for delivery. An SDG is^^groupxpf 20 or fewer
samples within a Case, received overaperiod of up to PKcalendar days. Data
from all samples in an SDG are due /concu?r«Rtly_.An SDG iscWfined by one of
the following, whichever occurs fi^st:
Case; or
• Each 20 samples within a
Selected Ion Current Profile
number for ions of a specified ma
Standard Analyy
target compo
Each 14-day cale«dar-vj>eriod dur3
received, beginning wit
or SDG.
ich samples in a Case are
first sample in the Case
Sample Number (EPA Sample/Number) /- A unique^identification number designated
by EPA for each sample. /The EPA/Sample Number appears on the sample Traffic
Report which documents iQformatjran /m that
- A plot of ion abundance vs time or scan
Static
concentr
cylinde
Cal
tical/Metermination made with known quantities of
ine response factors.
f an analytical system with known
obtained from a source such as gas
stock solutions.
December, 1991
Page G - 6
-------
Exhibit G
VOA of Ambient Air on Tenax®
Stock Solution - A standard solution which can be diluted,
standards.
:o perive other
Surrogates (Surrogate Standard) - Compounds added to eperj/blank, sample,
matrix spike, matrix spike duplicate, and standard; used to^svaluate
analytical efficiency by measuring recovery. Surrogate^>are brbniinated,
fluorinated, or isotopically labelled compounds no^/exjoected^tp beNietected in
environmental media.
Target compound - The compound an analysis see
interest.
Tent.. /ely Identified Compounds (TIC) - Corn-
are not target compound; . internal standard;
peaks are subjected to mass spectral libra
identification.
determine; the comp
in samples that
andards. Up to 10
tentative
Time - When required to record time on any deliverable/item, time shall be
expressed as Military Time, i.e., a 24-hour cloc
Traffic Report (TR) - An EPA sample identification fornT^COl6^?011*1 by
sampler, which accompanies the samp(Te~~lh«iiig^shipment to tn"fe\Xaboratory and
which is used for documenting sample c.on;dition~ait*-5?acfii£t by the laboratory.
Twelve-Hour Time Period - The twelve\(12\ hourytime^peTiod/for GC/MS system
tuning, standards calibration (initial\pr xxmpinuang calibration) begins at
the moment of injection of the BFB analysis\rhat/the laboratory submits as
documentation of compliant tune. The tim^perjlod ends after 12 hours has
elapsed according to the sys£em-^elock.
Validated Time of Sample/Re
received at the Contra
receipt and Sample Tr
s facUit-
Report.
5R) - The aateXon which a sample is
recorded/on the shipper's delivery
Volatile Compounds
by the analytical
thod
compounds with ntrenfal vapor pressures > 0.1 mm Hg
this document.
December, 1991
Page G - 7
-------
ATTACHMENT V
-------
USEPA CONTRACT LABORATORY/ PROG:
SEMIVOIATILE ORGANICS
-------
SEMIVOLATILE ORGANICS ANALYSIS
OF AMBIENT AIR
TABLE OF CONTENTS
PREFACE
EXHIBIT A SUMMARY OF REQUIREMENTS FOR SEMIVi
OF AMBIENT AIR
B-l
C-l
OF SEMIVOEATILE ORGANIC
ANALYZED BY
(GfJ/MS) D-l
EXHIBIT B REPORTING AND DELIVERABLES REQUI
EXHIBIT C TARGET COMPOUND LIST
EXHIBIT D ANALYTICAL METHOD FOR THE\DE'
COMPOUNDS (SVOCs) IN AIR O
GAS CHROMATOGRAPHY/MASS SPEC1
EXHIBIT E QUALITY ASSURANCE/QBAUTY CONTROLXREQ
EXHIBIT F EVIDENTARY
EXHIBIT G GLOSSARY
E-l
F-l
G-l
-------
PREFACE
The purpose of this contract is to provide the U/.S. Environmental
Protection Agency (EPA) with chemical analytical
procedures, and an analysis structure which will generate dataXpf kn
documented quality. This document was developed wi^h/the guidancexpf
Toxics Workgroup to ensure that the needs of regi^ris^., state, and lo
pollution programs are addressed.
The samples to be analyzed are of ambient a/r collected on PUF/XAD-2 at
or in the vicinity of known or suspected hazardaas waste/sites and may contain
potentially hazardous organic and inorganic/naterials ac significant
concentrations. The Contractor should be /warexpf the/potential hazards
associated with the handling and analyses oSsthesex^mpLes. It is the
Contractor's responsibility to take all necess^sy measures and precautions to
ensure the health and safety of its employees. Tne-vContr^aqtor is responsible
for providing a safe working environment and making its^emptopees aware of the
potential hazards of working with and analyzing these samples.
Procedures specified herein
PUF/XAD-2 cartridges and analysis o
quantitation of certain semivolatile
Contractor shall employ safe handling
laboratory practices in the performance
follow the quality assurance and quality c
herein.
The data obtained
the existence and exten
the public, to individi
environment. The dat
requires the stricte
control, and qualit
aration of
ence and
s). The
id generally accepted
requirements and shall
(QA/QC) program specified
be )used by EPA to determine
waste disposal sites to
site cleanups, and to the
criminal litigation which
'tody protocol, document
January, 1992
Revision SVAA01.0
Page i
-------
SEMIVOLATILE OF
OF
JBIENT AIR>
January, 1992
-------
SECTION 1
SECTION 2
2.1
2.2
2.3
EXHIBIT A
SUMMARY OF REQUIREMENTS FOR
SEMIVOLATILE ORGANICS ANALYSIS OF AMBIEN'
Table of Contents
GENERAL REQUIREMENTS
SPECIFIC REQUIREMENTS
Receive and Prepare Ambient Air Sample1
Analyze Samples for the Identification and
Quantitation of Specific
Perform Required Qualitt
Quality Control Procedur
SECTION 3 DETAILED TECHNICAL AND
3.1 Personnel
3.2 Facilities
3.3 Instrumental
3.4 Data Handli
3 .5 Laboratory/Ma
J.,i.uary, 1992
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
SECTION 1
GENERAL REQUIREMENTS
1.1 The Contractor shall employ procedures specified
preparation and analysis of the ambient air samples f
quantitation of the organic compounds listed in Exhib/lt
thi?&xcontract in the
tt*< presence and
1.2 The Contractor shall use proven techniques to/^ttentify and measiAre tfi>
organic compounds presented in the Target Compounia Lyst (TCL) as specir^tejd
Exhibit C. The Contractor shall perform sample .preparation and analysis
procedures as prescribed in Exhibit D, and nteey specified Cample and extract
preservation and holding time requirements.
1.3 For all samples analyzed under this coi/tra£t,
to the QA/QC protocols specified in Exhibi&^E am:
protocols specified in Exhibit F.
Jonttractor shall adhere
by the evidentiary
1.4 Following sample analysis, the Contractor shaliOperforrnxdata reduction
and shall report analytical activities, sample data, arioSqualifcy. control
documentation as designated in Exhibit—E^___Exhibit B contaihs^alA reporting
and deliverables requirements for tpis contract;—incjAximg copies of the data
reporting forms and form instructior
1.5 To ensure proper understanding of
G contains a glossary of terms. When a
explanation, the glossary meaning shall
do not replace or take precedence over spec:
document text.
in this contract, Exhibit
in the text without
tpplio&ble. Glossary definitions
Eic \nformation included in the
yo. m/y contain nazar
1.6 The samples to be
hazardous waste sites a
materials at high conce^ntr/tion leye
potential hazards ass
It is the Contractor's
the health and safety
responsibility to follow
and federal regulations.
jropri*
lfractor\ar,e from known or suspected
.nic and/or inorganic
.ctor should be aware of the
handlihg^ai/d analysis of these samples.
to take all necessary measures to ensure
es. It is also the Contractor's
disposal procedures according to state
or must
1.7 In additi
maintaining th
be used to mjike/hajor
welfare. In addition,
litigation/agafinst potentially
Super fund/legri
fare of the importance of
data generated under this contract, as it may
garding public health and environmental
ed under this contract may be used in
nsible parties in the enforcement of
,'anuarv. 1992
Page A-l
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
SECTION 2
SPECIFIC REQUIREMENTS
For each sample, the Contractor shall perform the//fol/3vowin^\^asks :
2.1 TASK I: RECEIVE AMBIENT AIR SAMPLES ON PUF/$U>-£ CARTRIDGES
2.1.1 The Contractor shall receive and handLe samples under the
of-custody and document control procedures described in Exhibit F.
2.1.2 The Contractor shall provide the r
instrumentation for analyses of the TCL
the quantitation limits specified in Ex,
provides the Contractor with an approp
that shall be used.
2.1.3 The Contractor shall extract samples
within the maximum holding times specified in Exhi1
times are less than the maximum £a£a submission
contract.
2.1.4 The Contractor is advised
contract are usually from known or'
may contain high levels of organic
potentially hazardous nature and of
and should be handled throughout the
appropriate caution. Tbe^Sont^actor
expertise and
lto or lower than
ibit D, EPA
lytical procedures
the extracts
n if these
in this
sha
d under this
aste sites and
'ganic materials of a
tructure and concentration,
fion and analysis with
responsible for all
necessary measures any precautions to ensure tne health and safety of
laboratory employees,
2.2 TASK II:
ANALYZE' SAMPLES FO?
SPECIFIC /COMPOUND?
iJENTI>I€ATION AND QUANTITATION OF
2.2.1 For each staple JfeQe/vedf, the Contractor shall be required .to
perform the sample e^sractionAnd analysis procedures described in
Exhibit D. The documentation chat accompanies the sample(s) to the
Contractor facitrcy—shall iiJiM^cate^s^ecific analytical requirements for
that sample/or set of samples.
analytical procedures that shall be used.
and references for the analysis of
low-to-medium concentrations of
analysis. GC/MS may use automated
the identification of organic compounds,
2.2.3 For tFttexjmrpb^e o$ this contract, a full sample analysis is
defined as analyses foV'all/of the TCL constituents identified in Exhibit
C in accordance with\the nfethods in Exhibit D and performance of related
January, 1992
Page A-2
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
QA/QC as specified in Exhibit D and Exhibit E. Laboratofy-^Control
Samples (LCS) analyses shall be considered a separate mil/sample
analysis. All other QA/QC requirements are cons iderecz an/inherent part
of this contract and are included in the contract sajnple/unit price.
2.2.4 The semivolatile compounds analyzed by GC/M& tachniqbes and
initially identified shall be verified by an analyst/competent^in the
interpretation of mass spectra by comparison of ./rhe/suspect^mass spectra
to the mass spectra of a standard of the suspecps^compound. This
procedure requires the use of multiple intern/1 standards. Two
must be satisfied to verify the identificati
2.2.4.1 Elution of the sample compon
retention time as the standard component
2.2.4.2 Correspondence of the samJ.e cot
component mass spectra.
the same}GC relative
id standard
2.2.5 For each sample analysis, the Contractor'^ihall
spectral library searches of non-target compound si
determine tentative compound identifications as follows
[iduct mass
sonents to
2.2.5.1 For each semivolatJae
shall conduct a search to det^rmi
organic compounds of greatest
standards, surrogate compounds,
Contractor
je the^bsaihleidantity of up to 10
Lonrwhich are not internal
.jfeted in Exhibit C.
2.2.5.2 In performingjearches,
National Institute o-fStarRiards and
spectral library must Jia^usec
NOTE: Substance's
nearest intei
fashion.
Lth responses of
candard are
recent release of the
gy (NIST)/EPA/MSDC mass
sss than 10 percent of the
to be searched in this
2.2.5.3 Only
spectra from the "Hbjrary
interpretation speci
compoundj&ff&s no-fejneet
report
addi
2.3 TASK
.a 1/comparisen of sample spectra with the
earches will the mass spectral
a tentative identification. If the
identification criteria, it shall be
unknowruXThe ma»s spectral specialist should give
Lcatrvjn of thV/unknown compound, if possible (e.g.
hydrocarbon, unknown acid type, unknown
compound) .\ Ir\ probable molecular weights can be
\ould be included.
'ALITY ASSURANCE AND QUALITY CONTROL
2.3.1 All speci
ocedures prescribed in Exhibits D and E shall
January, 1992
Page A-3
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
be strictly adhered to by the Contractor. Records doc
the protocol shall be maintained in accordance with t
procedures prescribed in Exhibit F, and shall be rep
with Exhibit B requirements.
2.3.2 The Contractor shall establish, and use o
QA/QC procedures including the daily or (as req
of standard reference solutions from EPA, MIST
traceable thereto, where available at appropriat
standard solutions designed to ensure that oper
equipment and procedures, from sample recer
quantitation, produce reliable data). Ex
QA/QC requirements.
ring the use of
control
in accordance
ing parameters
rough identification and
ovide specific
bits D and
2.3.3 Additional QA/QC shall be requic|d
i.e., with each Case or Sample Delivery
Laboratory Control Samples (LCS) and Performance Eva
for semivolatile organics submitted to EPA for Osntrac
in the form of verification of instrument parameters
Exhibit E.
more frequently,
'in the form of
uation (PE) samples
analysis, and
as described in
2.3.3.1 EPA has provided tOv th*
of data (Exhibit B). The Con\ra£
completing and returning analys
in this contract and within the
Performance/Delivery Schedule.
Itractor forHreffc&__for the reporting
sKaTJ. be^responstible for
ts in?he format specified
tied in the Contract
2.3.3.2 Use of form>ts~otfeer than
deemed as noncomplifant. SucKdata are
the specified forjnat atnbxadqitional
required.
Designated by EPA will be
^eptable. Resubmission in
the Government will be
2.3.3.3 Computer/generati
data package Os) prsmrided,
This means tha^the
required form, irfe^udirig
header information,
fVrms may^be/Submitted in the hardcopy
~.ha.t the forms are in exact EPA format.
of data elements is the same as on each EPA
>rm numbers and titles, page numbers and
lines.
2.3.4 The Contractor shall provide analytical equipment and technical
expertise ^or-/enTi~~c"btitract\as spec
-------
Exhibit A
Seraivolatile Organics Analysis of Ambient Air
2.3.4.1.2 The computer shall be equipped with
devices for saving all data from the GC/MS run*
storage
2.3.4.1.3 Computer software shall be availa6le/to allow searching
GC/MS runs for specific ions and plotting tjne intensity of the
ions with respect to time or scan number.
2.3.4.1.4 A computer data system must Ke interface^Kto
that allows the continuous acquisition^haa storage, onrnachiii^
readable media, of all mass spectra oota^ned throughout tnfe
duration of the chromatographic program/ The computer must
software that allows searching any /\3C/HS data ,£ile for ions of a
specified mass and plotting such Yon^abundanoes^Versus time or
scan number. This type of plot is defined as an Extracted Ion
Current Profile (EICP) or Selec/edAon Current/Profile (SICP).
Software must also be availablfeitha^Nalloys integrating the
abundance in any EICP between spes4^iedxcime'or scan number
limits. Also, for the non-target comfiounds^^oftware must be
available that allows for the comparisorKpf sample spectra against
reference library spectra. The most recencXeleas^soof the
NIST/EPA/MSDC mass spectpaJ^iibrary shall be us^ad as the reference
library. The data system mustT>e~~capahJ.eof flagging all data
files that have been ed\ted\^naBuaily by laEoTsree^y personnel.
2.3.4.1.5 The GC/MS shall^efeguipofed/with aUTC to MS interface
\ \r * r /
capable of extending a fuseoXsili^ capillary column into the ion
source. The column is to be 5X) meters long by 0.25 to 0.53 mm
I.D. 100% methyl silicone or 5%\$>henyl, 95% methyl silicone
capillary coluima^ore^uivalent.
rac/tor
2.3.4.2 The Con.
capable of reco
s torage. The yoon
under this contract on
manufacture
magnetic tapesxwith
contents (see Exnl
that time, the Contr
days of
Sched
2.3
a magnetic? tape storage device
!g data ^nd"suitab^e for/long—term, off—line
'ractor sjnalL^re
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
and the data system shall have software capable of/removing
background signals from spectra.
2.3.4.5 The Contractor shall have, in—house an;
capable of analyzing Semivolatile organics as
2.3.4.6 The Contractor shall have, in-hous€
standards for all target compounds listed ii
accepting any samples from the Sample Mana^en
Standards provided by EPA for use in the/
Evaluation may not contain all the target compounds and thus shall
not be used for routine analyses unless oir until jZne^w have been
supplemented with commercially available/standard materials.
able, a device
4n Exhibit D.
2.3.5 The minimum functional requiren
and conditions of this contract are listed
designate and use qualified key personnel
The EPA reserves the right to review personnel
experience.
shall
nal
nt's^-inspectio
'o meet the, terms
Contractor shall
these functions.
tions and
2.3.5.1 Proj ect Manager
2.3.5.2 GC/MS Laboratory Sup\rvi
2.3.5.3 Quality Assurance Offic^
2.3.5.4 Systems Manager
2.3.5.5 Program
2.3.5.6 GC/MS
2.3.5.7 Mass,
2.3.5.8 Sampts^repas^fion^Extraction Supervisor ;
2.3.5.9 Sample Prepa^tionyExtraction Specialist;
2.3.5.:
NOTE:
Control/Of
2.3.7 The Contr
extracts, and used
signate a Sample Custodian and a Document
ond within 10 days to requests from data
'mation or explanations that result from
'tivities.
quired to retain unused samples and sample
Containers for a period of 60 days after data
January, 1992
Page A-6
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
submission unless otherwise instructed in Exhibit B or
libit D.
2.3.8 The Contractor shall adhere to the chain-of-custody and document
control procedures described in Exhibit F. Documentation, as described
therein, shall be required to show that all procedures are being strictly
followed. This documentation shall be reported iprthA Comfriete Case File
Purge (Exhibit B).
2.3.9 Sample shipments to the Contractor's fac^H^ty will be schedule*
and coordinated by SMO,. acting on behalf of the^dministrative Prompt
Officer (APO). The Contractor shall communi/cat£ with SMO personnel b)
telephone as necessary throughout the process .of sample scheduling,
shipment, analysis, and data reporting, t
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
that the last sample in the SDG is received.
2.3.13 The Contractor is responsible for identify!
are received, through proper sample documentation
communication with SMO personnel.
SDG as samples
shibit B) and
2.3.14 Each sample received by the Contractor
EPA sample number, and accompanied by a Traffic
the sample number and descriptive information/retarding the sampled. The?
Contractor shall complete and sign the TR, recording the date of samp]
receipt and sample condition on receipt for/ea^h sample container.
'TRs
2.3.15 The Contractor shall submit sign
in an SDG to SMO within three calendar
sample in the SDG. TRs shall be submitted'
an SDG shall be clipped together) with alxSDG
information regarding the SDG, as specified
•pies ol
followi
for all samples
ig Receipt of the last
.SDG/set/ (i.e., all TRs for
/er .Sheet containing
Exhibit B.
2.3.16 EPA Case numbers (including SDG numbers) aiWkEPA^ample numbers
shall be used by the Contractor in^identifying samplesss^ceyved under
this contract both verbally and/in repo~rtsyicar_respondence.
2.3.17 Samples will be routinely^ shipped
through a delivery service. The
sample shipments at any time the
Saturdays and holidays. As necessary\ ttv
responsible for any handling or process!
sample shipments, includiitg~~{yic^-up of s
airport, bus station, pt other carrier sei
geographical area.
Contractor
be~~3va.ilable to receive
flee is operating, including
itractor shall be
Required for the receipt of
at the nearest servicing
/ithin the Contractor's
2.3.18 The Contractor/shall adcept—a^A samples scheduled by SMO,
provided that the/topal numbeir of/samplfe
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
SECTION 3
DETAILED TECHNICAL & MANAGEMENT REQUI
The Contractor shall have the following techni
capabilities:
3.1 PERSONNEL
3.1.1 Project Manager
3.1.1.1 Responsible for all technical/efi
meet all terms and conditions of the
3.1.1.2 Education: Minimum of Ba<
scientific/engineering discipline.
3.1.1.3 Experience: Minimum of three
experience, including at least one year in
3.1.2 GC/MS Laboratory Supervi
3.1.2.1 Responsible for a
laboratory to meet all terms
3.1.3 Quality Ass;
3.1.3.1 Re
data generati
3.1.3.2 Education:
s c i en t i f
the laboratory to
n chemistry or any
aboratory
sory position.
GC/MS
'ontract.
3.1.2.2 Education: Minimum of
scientific/engineering disciplined
3.1.2.3 Experiences
in operating a GC^MS,
position.
degree in chemistry or any
rs of laboratory experience
year in a supervisory
3.1.
overseeing the quality assurance aspects of
Lng directly to upper management.
Bachelor's degree in chemistry or any
nimum df three years of laboratory
least one year of applied experience with QA
n an analytical laboratory.
3.1.4^
computin
procedures),
or /the management and quality control of all
are, software, documentation, and
updating, and performing quality control on
January, 1992
Page A-9
-------
Kxhibit A
Semivolatile Organics Analysis of Ambient: Air
automated deliverables.
3.1.4.2 Education: Minimum of Bachelor's degre/ w^th four or more
intermediate courses in programming, information management, database
management systems, or systems requirements analysis
3.1.4.3 Experience: Minimum of three years' ex^perience^iri dat
systems management or programming includin/g;xij
software used for data management and gen/ra)zion of deliverabj
or
3.1.5 Program Analyst
3.1.5.1 Responsible for the installation,
of software and programs; generatin
quality control procedures on analytical
deliverables.
/
operaytiosi, and maintenance
dating/an/1 performing
atabase^ and automated
3.1.5.2 Education: Minimum of Bachelor's
intermediate courses in programming, informatio^
information systems, or systajngrequirements
^th four or more
nent,
analy*
3.1.5.3 Experience: Minimfc
applications programming incrudii
software used for data managem£
one
and
^ars experr««ce in systems or
r ,of__exper/lence with
[ecationor deliverables.
3.1.6 Gas Chromatography/Mass Spectrometer ftSC/MS) Operator
of BacheSLor\ degree in chemistry or any
3.1.6.1 Education:y-HinO
scientific/engineering
3.1.6.2 Experience/ MinimV
and maintainingGG/MS instj
requirement; 0t im lieu oj
years of exp/riense in oj
ins trumentati*
^f onfexyear Vf experience in operating
cbrvwmction with the education
icationxreqxlirement, three additional
:ing and maintaining GC/MS
3.1.7 Mass Spectral In«
sretel
3.1.8
'.2 Exoerience: »i
>/analvsis of envirp
tmplexPreparation/Ejc
iscipl
Bachelor's degree in chemistry or any
with specialized training in GC/MS.
turn of two years of applied experience with
mtal samples.
ction Supervisor
have a minimum of one extraction specialist
nical efforts of sample preparations and
terms and conditions of the EPA contract.
January, 1992
Page A-10
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
3.1.8.2 Education: Minimum of Bachelor's degree i
scientific/engineering discipline.
3.1.8.3 Experience: Minimum of three years of
experience, including at least one year ~f supe
3.1.9 Sample Extraction/Preparation Specialist
:emistry or any
3.1.9.1 Education:
equivalent.
Minimum of Bachelor's
3.1.9.2 Experience: Minimum of one ye,
analytical laboratory.
f applied experience in an
3.1.10 Technical Staff Redundancy
3.1.10.1 In order to ensure continue
required work as specified by the contra
minimum of one chemist available at all time
person with the following qualifications.
3.1.10.2 Education: Minimi
any scientific/engineering
3.1.10.3 Experience: Minimum
the following areas: GC/MS oper
3.2 FACILITIES
The adequacy of th^ fac_LLitieN
technical staff for accomplishing
EPA contract.
to accomplish the
jLdder shall have a
ck-up technical
degree
3.2.1 Sample Rec
i
Adequate,
chemical resistantxfcjench
handling of EPA samp
3.2.2
lemistry or
experience in each of
.aintenance.
is as important as the
rk as specified by the
-free, well-ventilated work space with
shall be available for receipt and safe
contam
separate!
ratl^r space to maintain unused EPA sample volume
a submission shall be provided.
stored in a refrigerator used only for
les from this contract. Samples must be
onstrated to be free from all potential
iple extracts, and standards must be stored
January, 1992
Page A-ll
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
3.2.3 Sample/Standard Preparation Area
Adequate, contamination-free, well-ventilated' work space shall be
provided with:
3.2.3.1 Benches with chemical resistant tops/.
3.2.3.2 Exhaust hoods.
. . .n
to prepare standard
3.2.3.3 Glove box or isolated area in
materials.
"*.2.3.A Source of distilled or demi
3.2.3 . Analytical balance(s) loc«
change in temperature.
j/c-free water.
raft and rapid
3.3 INSTRUMENTATION
At a minimum, the Contractor-s_h_all have the follow!
operative at the time of the Pre4warxT~51rte--E3£aluation
the full duration of the contract.
3.3.1 100 Samples/Month Capacity
No. of Instrmnent(s)
1
instruments
'ommitted for
NOTE: The Contractor/sh
Voperational) at al
be included in the
Contractor shall
boards to ensure/con'
and turnaround ti
3.3.2 200 Samples/Montf
No. ofxlnstrumentfs
GC/MS system available
These instruments must
Lament. In addition, the
'strument parts and circuit
contract-specified holding
Requirements
Type of Instrument
GC/MS
included in the bidder's inventory of
tractor shall have an in-house stock of
ards to ensure continuous operation to
g and turnaround times.
J.muarv. 1992
Page A-12
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
3.3.3 Instrument Specifications
Further information on instrument specificati
ancillary equipment may be found in Exhibit D at
this contract.
3.4 DATA HANDLING AND PACKAGING
The Contractor shall be able to submit rep,
specified in Exhibit B. To complete this tasy
required to:
3.4.1 Provide space, tables, and copy ma
requirements.
3.4.2 Designate personnel responsible
submission.
3.5 LABORATORY MANAGEMENT CAPABILITY
.nd required
Exhibits in
3.5.1 Technical Staff
Responsible f
sample analysis ,/sa:
instruments.
3.5.2 Project Ma;
Responsib
receipt through
EPA Headquarters
Technica
3.5.3 S
The Contractor shall have ary-acganization with weft-vdefined
responsibilities for each individual irT~Che-«aiiagement system to ensure
sufficient resources for EPA coWrafrt<-sjL_and to malrTrata^a successful
operation. To establish this capability, tK& Contractor/shall designate
personnel to carry out the following rVsponsabiAitiesfor the EPA
contract. Functions include, but ar\ no\ Xim^ted to, the following:
3.5.4
the EPA contract such as
leshooting of all
aspects of EPA contract(s) (from sample
and shall be the primary contact for
Project Officer (APO) and Regional
ng the EPA samples (logging, handling, and
Respotvsible^for oVer^eeing the quality assurance aspects of the
data and repbit^ing Jiirectly to upper management.
January, L992
Page A-13
-------
Exhibit A
Semivolatile Organics Analysis of Ambient Air
3.5.5 Document Control Officer
Responsible for ensuring that all documents generated are placed
in the Complete SDG File for inventory and are keliV^red to the
appropriate EPA Region or other receiver as dejsignated^Hjy EPA.
January, 1992
Page A-14
-------
January, 1992
-------
EXHIBIT B
REPORTING AND DELIVERABLES REQUIREMENT*
TABLE OF CONTENTS
SECTION 1 CONTRACT REPORTS/DELIVERABLES DISTRI
SECTION 2 REPORTING DESCRIPTIONS AND ORDER
2.1 Introduction . . .
2.2 Updated Standard Operating Procedures
2.3 Sample Traffic Reports
2.4 Sample Data Package Summary
2.5 Sample Data Package
2.6 Results of Intercomparison Stxi
Preaward Performance Evaluation
2.7 Complete Case File (CSF) Purge
2.8 GC/MS Tapes \ ' V B"15
2.9 Quality Assurance P.kan (QAP)\ . . . . \ . \ B-15
SECTION 3 FORM INSTRUCTION*^GUIDE/D/^TA REPOR
3.1 Form Instruetions^Guide
3.2 Data Reporting "FQrms
1992
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
SECTION 1
CONTRACT REPORTS/DELIVERABLES DISTRIBU1
1.1 The following table summarizes the contract reporting, and^dej-iverables
requirements specified in the Contract Schedule and ijiclytaes^he distribution
of each deliverable.
NOTE: Specific recipient names and addresses are sfobjpect to change
term of the contract. The EPA APO or SMO will ns/tif/ty the Contractor in
writing of such changes when they occur.
the
Item
No. of
Copies
Daaifer
Schdulesand Daaiyfery
Distribution
(1)
(2)
(3)
Updated Standard Operating
Procedures (SOPs)
45 days affcer contract
X.
Sample Traffic Reports
jfc**3 days after recent
of^TaStr--frainEle in Sampl
\Belivejry
**Sample Data Summary
Package
l4 ciays af/er/reCeiat/of
x / /
las sample in SDG.
**Sample Data Package
including the Performance
Evaluation (PE) Sample
v
35 days aFter receipt of
las\ sample in SDG
X
X
Results of Intercomparison
Study/Preaward Performance/
Evaluation (PPE) Sample
afrcr/receipt of
lastxsampYe in SDG
s s. 7
X.
Complete SDG File
35 days/ after data
receipt of last sample
in SDG.
x.
GC/MS Tapes
Retain for 365 days
after data submission,
or/submit within 7 days
arter receipt of written
request by APO.
As Directed
****Qua/ity assurance Plan
Submit copy within 7
days by written request
by APO.
As Directed
January, 1992
Page B-l
-------
Exhibit B
Seraivolatile Organics Analysis of Ambient Air
Distribution
(1) Sample Management Office
(2) Environmental Monitoring Systems Laboratory-Las
(3) USEPA Region
* Also required in each Sample Data Package.
** Concurrent delivery of these items to all,
*** An SDG is a group of samples within a
seven days or less and not exceeding
in the SDG are due concurrently. (S«
description).
**** see Exhibit E for description.
NOTE: As specified in the Contract Schedule in the
Supplies and Materials), unless otherwi_se_ins true ted by
shall dispose of unused sample voli
earlier than 60 days following subml
Address
(1)
(2)
300 North Lee
Alexandria, V;
USEPA Environmental
P.O. Box 93478
Las Vegas,^
ATTN: Di
er a period of
for all samples
k III, for further
nt Furnished
Contractor
'ontainers no
USEPA. Contract Laboratory Program
Sample Management Office
P.O. Box 818
Alexandria, VA 223
For overnight del/ve
.dress:
3478
.ng Systems Laboratory
ice, use street address:
er
January. 1992
Page B-2
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Contractor with
provide the
(3) USEPA REGIONS:
SMO, acting on behalf of the EPA APO, will provid
the list of addresses for the 10 EPA Regions. S
Contractor with updated Regional name/address l^sts,
throughout the period of the contract and iden
recipients on a case-by-case basis.
NOTE: Specific recipient names and addresses are/sufc
term of the contract. The APO will notify the Cpntyactor in writing of siic
changes when they occur.
Januarv. 1992
Page B-3
-------
Exhibit B
Seraivolatile Organics Analysis of Ambient Air
— - — ^_
SECTION 2
REPORT DESCRIPTIONS AND ORDER OF DATA DELI
2.1 The Contractor shall provide reports and other deliyeraBte^ acceding to
the schedule specified in Section F of the IFB, "SCHEDULE INFORMfc$3X3N>\The
required content and form of each deliverable is de^^ibed in this
2.1.1 All reports and documentation shall be:/
2.1.1.1 Legible;
2.1.1.2 Clearly labeled and completejz in/accorc
in this Exhibit;
ice/with instructions
2.1.1.3 Arranged in the order specified irNt±is section;
2.1.1.4 Paginated; and
2.1.1.5 Single-sided.
2.1.2 If submitted documentation
the Contractor will be required to re
deficiency(ies) corrected, at no addif5
jot confibrm~tQ_^the Above criteria,
ich/Documentation with
to the Government.
2.1.3 Whenever the Contractor is requireckto ^submit or resubmit data as a
result of an on-site labo^fory^fevaluation\r through an APO/TPO action,
the data shall be clearly masked ak "ADDITIONAL DATA" and shall be sent to
all three contractual data/reciplent^_4SMO, EMSL-W, and Region). A cover
letter shall be includted/that describes which daVa are being delivered, to
which EPA Case(s) thfi d^ra pertain, ^arrdvwho rerjpested the data.
2.1.4 Section 3 of th?s\Exhih£t Contains instructions to the Contractor
for properly completing allxdata/reporting forms to provide the EPA with
the required documentaoba^i and Contains the required data forms in EPA-
specified format.
\ >^
2.1.5 Descri^tionsof theNrequirelsents/for each deliverable item cited in
the Contract PBi^oTmanfeB^Delrvery ScnWule (see Section F of the IFB
"SCHEDULE/INFORMATION") arXsp\cified in this Section. Items submitted
concurrently/must be arranged in\ the order listed. Additionally, the
componepfts >of each item must \e Arranged in the order presented herein.
OPERATING /PROCEDURES
2.2.1 The
Operating Procedur
SO
submit updated copies of all required Standard
iat were submitted with the Prebid Performance
January, 1992
Page B-4
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Evaluation (PPE) sample results. The updated SOPs must Address any and all
issues of laboratory performance and operation identified /through the
review of the PPE sample data and the evaluation of Bidder-Supplied
Documentation.
2.2.2 The Contractor must supply SOPs for the fo]
2.2.2.1 Evidentiary SOPs.
2.2.2.2 Sample receipt and logging.
2.2.2.3 Sample and extract storage
2.2.2.4 Preventing sample contaminat
2.2.2.5 Security for laboratory and
2.2.2.6 Traceability/equivalency of standarc
2.2.2.7 Maintaining instrument-records and bound lo>
2.2.2.8 Glassware cleaning.
2.2.2.9 Technical and manageria
data package preparation.
2.2.2.10 Internal review of contract^
individual data packs
2.2.2.11 Sample e/tra^tionNam
reporting.
2.2.2.12 Chaii/-o
preparation.
aboratory operation and
-required QA/QC data for each
handling, and data
trol, including case file
2.2.2.13 Sample
Da
ition/self-inspection system, including:
Hand for data review;
me^^suring precision and accuracy;
for identifying systematic errors;
:hat hardcopy data are complete and
comfHjlant with thy& requirements in Exhibit B;
DemoNFks_trat:ban o/f internal QA inspection procedure (demonstrated
January. 1992
Page B-5
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
quarterly,
by supervisory sign-off on personal noteboo
samples , etc . ) ;
• Frequency and type of internal audits (e/g. I/Vsranc
spot checks, perceived trouble areas);
Demonstration of problem identificati
resumption of analytical process ing /res]
audit (i.e., QA feedback); and
Documentation of audit reports (
response, corrective action, et;
2.2.2.14 Data Handling.
2 . 2 . 2 . 14 . 1 Data Management procedures
procedures that are clearly defined for
used to generate or re- submit deliverables
acquisition or entry, update_^_correction, deleti
security of computer- readable data~~and-_£iles . Key
include: system organiza^on\~w*cJLuding perso
demonstration, operations , \raceabilrty7, apd_quali
.ned as written
and files
>rage, and
'eas of concern
id security,
control.
2.2.2.14.2 Data manually ente'fced ^frofo hardcopy must be subjected
to quality control procedures am} erroi/rates estimated.
2.2.2.14.3 The reetJfcFb>£'changes Oathfc form of corrections and
updates to data siitted, and/or resubmitted
must be documented/^o^tiow jtraceabilicy o£ updates. Documentation
must include pne following £nforra5*4on ^^ each change:
Just/fioation or/rationale"
change;
Initials of'^h^ person making the changes or changes. Data
changeslsu^st be jfaentified when generating the deliverables;
iocumertfcationNnust be retained according to the
schedule or\the ort-cinaiydeliverable;
Resubmitted
the laborato
submission.
X
deliverables must be reinspected as a part of
internal inspection process prior to
intire deliverable and not just the changes
Id;
must be reinsp
TheX^aboratory m/nager must approve changes to originally
de4iv/rables; and
January, 1992
Page B-6
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Documentation of data changes may be reqv.
auditors.
ist&d by laboratory
2.2.2.14.4 Life cycle management procedures/mustNje applied to
computer systems used to generate and edit contract oeliverabies.
Such systems must be thoroughly tested and/dogumehted pr^toj: to
utilization.
2.2.2.14.5 A software test and acceptance>plan including
requirements, test results, and accept4nc/ criteria must be
developed, followed, and available it/written form.
2.2.2.14.6 System changes shall n/t
systems generating deliverables.
development system and tested pr4
2.2.2.14.7 Each version of the product
identification number, date of installatft
operation, and archived.
2.2.2.14.8 System and op«
and maintained for each 53
user's manual and an operai
2,2.2.14.9 Individual(s) resp\nsf
shall be identified:
re/tly to production
made first to a
ation.
will be given an
of last
be developed
include a
Lual.
2.2.2.14.1,
2.3 SAMPLE TRAFFIC REP01
trra±
fair the following functions
Torf-ajrid mainten^nce\including documentation and
entry, data updating and
m securityT backup, and archiving.
ked "Lab Copy for Return to SMO"
receipt information and signed in
sample in the SDG.
SDG sets (i.e., TRs for all samples in an
iwith an SDG Cover Sheet attached.
contain the following items:
January, 1992
Page B-7
-------
Exhibit B
Seraivolatile Organics Analysis of Ambient Air
2.3.3.2 Contract number.
2.3.3.3 Sample analysis price - full sample pric,
2.3.3.4 Case number.
2.3.3.5 List of EPA sample numbers of all s
identifying the first and last samples rece/ve
receipt.
NOTE: When more than one sample is received in the/ftrst or last SDG
shipment, the "first" sample received youla be the/loy»st sample number
(considering both alpha and numeric designations)/ aitd the "last"
sample received would be the highest^amp'be^jiumber /considering both
alpha and numeric designations).
2.3.4 Each TR shall be clearly marked with the SBG Number and the EPA
sample number of the first sample in the SDG. This tuforma^on shall be
entered below the laboratory receinj^_date on the TR. TOfc^TR ^or the last
sample received in the SDG shall )be clea?tr-aarked "SDG -FINAL SAMPLE."
2.3.5 If samples are received at the
the samples on one multi-sample TR ms
In this instance, the laboratory shal]
photocopies of the TR, and submit one ci
2.4 SAMPLE DATA SUMMARY PACI
th mulct-sample TRs, all
ne^es^arily"~be in the same SDG.
le/appropriate number of
each SDG cover sheet.
2.4.1 As specified in /the/DeliveryJSchedule, \ine)Sample Data Summary
Package shall be delivered to SMQ concurrently wtfth delivery of other
required sample data/ The Samplp Da^a^umma>ry-J?ackage shall be submitted
separately (i.e., s^pa^ted by/ubb^r barfci^ c/Lips or other means) directly
preceding the Samp
2.4.2 The Sample Data^Summary package shall contain data for samples in
one SDG of the Case, as
2.4.2.1
2.4.2
tent
1VER
target compound results (FORM I-AASV) and
.nds (FORM I-AASV-TIC).
(ample results (FORM III-AASV).
2.4.2.4\BlanK^ummary CFORtf II-AASV) and tabulated results (FORM I-
AASV) incKtding tentatively identified compounds (FORM I-AASV-TIC).
January, 1992
Page B-8
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
2.5
2.4.2.5 Initial and Continuing Calibration Data
FORM VI-AASV).
2.4.2.6 Internal Standard Area and Retention Ti/i
(FORM VII-AASV).
2.4.2.7 Filter/Adsorbent Cartridge Certificj
(FORM VIII-AASV)
2.4.2.8 Surrogate Recovery (FORM IX-AASV/.
2.4.2.9 Analytical Sequence (FORM X-AASV),
SAMPLE DATA PACKAGE
f-AASV and
Data
2.5.1 The sample data package shall be cbwpleteV/confsecutively paginated,
and shall include data for analysis of all salaries iis^an SDG such as field
samples, blanks, and laboratory control samples.
2.5.2 The sample data package i
2.5.2.1 Cover page.
into five unifc& as/follows:
2.5.2.1.1 This document sha^l b^e cle/rI/ labelecf "Cover Page."
The Cover Page shall contain:\labor/to/y name; laboratory code:
contract number: case number: SRG number; SAS number: EPA sample
numbers in alphanumeric order. sh\win£ EPA sample number cross-
referenced with l^hrcTraTo-i^y ID numbers:Nand comments, describing in
detail any prob^ms^^encoun^ered in processing the samples in the
data package
2.5.2.1.2 Ttfe
verbatim:
Jover Pas
the following statement.
"I certify thatsyt^iis/aata package is in compliance with the
terms and cbsidition^of the contract, both technically and for
completeness , rsjrotnfe^: than the conditions detailed above.
dataxconta^isned in this hardcopy data package has
authorize^i by thexljabo^atory Manager or the Manager's
/deSyirg'nee^ a-s^verrs^ied by cWe following signature."
mervt shall be directly followed by the
atory Manager or his designee with a typed
containing)the signer's name and title, and the date
2.5.2/1^4. InXhe event that the Laboratory Manager cannot validate
.J.inuarv. 1092
Pare B-°-
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
cov/de a detailed
sajnple(s) on the
all data reported for each sample, he/she must
description of the problems associated with
Cover Page.
2.5.2.2 Sample data (Results).
2.5.2.2.1 Sample data shall be arranged iiackets
Analysis Data Sheet (FORM I-AASV, including FORM I-AASV-TIC)
followed by the raw data for semivolatile /samples. These sample
packets should then be placed in increasing EPA sample number
order, considering both letters and^iumb4rs.
NOTE: FORM I AASV-TIC is the tabulated list df tzhe highest
probable match for up to 10 organic compounds that are not
surrogates and internal standards and areNaot .listed in Exhibit C
(TCL). It includes the Chemical Abstracts Se^jlce (CAS) Registry
Number, tentative identification, and estisjatedcojncentration.
2.5.2.
of compel
printout o
the peak.
r^2?2.1.4
d total ion chromat
Laboratory file/ID.
2.5.2.2.1.1 Reconstruc
each sample or sample
2.5.2.2.1.2 RICs must
component, and must contax
ams/(RIC) for
,est nonsolvent
r information:
EPA sample number;
• Date and
GC/MS
to be labeled with the names
Directly out from the peak, or on a
times if retention times are printed over
Report: The complete data system
in&luded ihxflll sample data packages, in addition
'to/the reconstructed ion chromatogram for preliminary
i/entification and/o\ quantitation using either the automated or
hanual data systenh procedures. The complete data system report
lall include all pf ihe information listed below:
sample /number;
of analysis;
January, 1992
Page. B-10
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
• RT or scan number of identified target /omtrounds;
Ion used for quantitation with measured
Copy of area table from data systei/;
• GC/MS instrument ID; and
Laboratory file ID.
2.5.2.2.1.5 In all instances whetfe tKe data system report has
been edited, or where manual integration or/qukntitation has
been performed, the GC/MS operator/shall identify such edits or
manual procedures by initialing a^d dating the changes made to
the report.
2.5.2.2.1.6 Target Compound Mass Spectrar^xFor each sample, by
each compound identified, copies of tnexraw spectra and copies
of background subtracted mass spectra of careet compounds listed
in Exhibit C that are identified in the sampiexand/corresponding
background subtracted /cargetcoBrpw*nd__standard ma"ss spectra
shall be included in t^e dfata-^a^kage. SpeTrtta-must be labeled
with EPA sample number ,\laWjirat<>ry~^ile^DJdapfe and time of
analysis, and GC/MS instrument; ID; /compound names must be
clearly marked on all spect
2.5.2.2.1.7 Tentatively Identified Compound Mass Spectra and
Library Matche^r" FcTtxeach sample, Bv each compound identified,
copies of mass spectra \f organicXcompounds not listed in
Exhibit C, Tentatively Identified Compounds, with associated
best-match/spectra (tHreebestNo(atche«), labeled as above shall
be includ/sd i/n. the dajta p^aekage.
2.5.2.2.2
iVolatile7 Standard DataT"
^\/ /
2.5.2.2.2.1\Initial
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
and quantitation reports (or legible facsimiles) for the
initial (five point) calibration are/labeled according to
2.5.2.2.1.2 and 2.5.2.2.1.4. Spectj
2.5.2.2.2.2 Continuing Calibration:
continuing calibration is performed,
chromatograms and quantitation report
must be put in chronological order,
one instrument is used as follows:
Continuing Calibration Dat/ Sh4et (FOB
Internal Standard Area
VII-AASV); and
id Retention
^I-AASV);
ne Summary (FORM
istrucl
ible
Semivolatile standard(s) re
and quantitation reports (or
initial (five point) calibration
2.5.2.2.1.2 and 2.5.2.2.1.4. Spectra
2.5.2.3 Quality control si
2.5.2.3.1 The quality conti
fo rms:
NOTE: If more than one form is
arranged in chronoj
Blank S
GC/MS
Int
ed ion chromatograms
similes) for the
d according to
not required.
in the following
ary, duplicate forms must be
of analysis or instrument.
2.5.2.3.2
following:
AASV)
\
k (FORM IV-AASV); and
ary (FORM VII-AASV).
ontrol summary shall also contain the
is^necessary, duplicate forms must be
by date of analysis or instrument.
GC/MS Tunind - JBFB data, for each 12-hour period, shall be
arranged in/chronological order by instrument for each
3/MS systf/m utilized;
in/and Mass Calibration - BFB (FORM IV - AASV) ;
Page B-12
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Bar graph spectrum, labeled as in 2.5.2/2. V. 2 and
2.5.2.2.1.4; and
Mass listing, labeled as in 2.5.2.2/1.2/xand 2.5.2.2.1.4.
Blank data shall be arranged in chroj
instrument. The blank data shall
both of the Semivolatile Organics
I-AASV and FORM I-AASV-TIC),
Semivolatile samples.
Laboratory Control Sample
Laboratory Control Samp
<
Reconstructed ion chroma!
or legible facsimile (GC/MS)">
2.5.2.2.1.2 and 2.5.2.2.1.4.
s with
iRM III-AASV); and
.ntitation reports
according to
not required.
2.5.2.4 Raw data.
Blanks;
Duplicates;
or crsjier apparen
cludihc alZ d
valu
2.5.2.4.1 For each reported ^aJ^ife^the Contr3et«c^shall include
all raw data from the instr\unent used~~"Cb origin tlye sample values
(except for raw data for quarterly ver/Lficationsof instrument
parameters). Raw data shall contain/all/instrument readouts used
for the sample results, including tnoser readouts that may fall
below the method quantitation limit. &11 GC/MS instruments must
provide legible hanT copy, of the diXect\real-time instrument
readout (i.e., sJtfripcharts\ printer capesv etc.). A photocopy of
the direct sequential instrument readout n&st be included.
2.5.2.4.2
GC/MS.
ncentration units for
2.5.2.4.3 ^Kganic^xaj/ da2
Page B-13
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Data and EPA sample number for GC/MS ana
sequentially identified on the raw data
All calculations for sample data, inc
coefficient of variation, slope and
fit; and
clearly and
• Time and date of each analysis.
submitted if they contain this
instrument does not automatically
these must be manually entere,
and continuing calibration
as interference check samp
standards.
2.5.2.5 Preparation logs.
These logs must include the following:
Date;
• Standard weights am
ent recovery,
linear
rovide time of analysis,
,ta for initial
blanks, as well
.nge analysis
2.5.2.6 Sample
A legi
submitted
the samples
EPA sample number
designa
2.6 RESULTS
ny signi
cun during pr
Sufficient information p re
samples (e.g., laboratoryvco
to each batch prepared; ami
Comments
reactio
unequivocally which QC
sample, blank) correspond
sample changes or
arktion.
id SDG Cover Sheet shall be
section 2.3 of this Exhibit for all of
The TRs shall be arranged in increasing
snsidering both alpha and numeric
CE EVALUATION SAMPLE ANALYSES
The /epcyrting of analyt:ical\ results for Intercomparison Study/Preaward
Performance Evaluation (PPE)\ sample analyses includes all requirements
specified Hn section 2.4 forlreporting of sample data. The PPE sample
shall Die^carrived through the/ex£c_t same process as an analytical and field
samples.
January, 1992
Page B-14
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
2.7 COMPLETE CASE FILE PURGE
2.7.1 The Complete SDG File package includes all lab/rapory records
received or generated for a specific Case that have ^ot &aen previously
submitted to EPA as a deliverable. These items shall be sinJtoitted to EPA
as a deliverable. These items shall be submitted /along wi
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
provide data which are technically sound and legally
2.9.2 The QAP must present, in specific terms,
objectives, functional guidelines, and specific
to achieve the data quality requirements in this
applicable, SOPs pertaining to each parameter she
referenced as part of the QAP. The QAP must be
laboratory evaluation and upon written request.
January, 1992
Page B-16
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Table B-l
Codes for Labeling Organic Data
Sample
Duplicate Sample /./... XXXXXD
Reanalyzed Sample /./..././..... XXXXXRE
Laboratory Control Sample <^. .^X^- •/• •/ SVLCS##
Laboratory Method Blank >Xi . .^ SVMBLK##
Field Blank >^ . .\. . . SVFBLK##
Standards /. . . .^T~7-^_ ^Y . . . SVSTD###
January, 1992
Page B-17
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
SECTION 3
FORM INSTRUCTIONS GUIDE/DATA REPORTING
3.1 Form Instructions Guide
3.1.1 This section includes specific ins true t
all required forms for semivolatile organics/a
2. Each of the forms is specific to a give
instructions are arranged in the following/or
3.1.1.1 General Information and Heac
3.1.1.2 Cover Page [COVER PAGE -
3.1.1.3 Analysis Data Sheet [FORM I -
3.1.1.4 Tentatively Identified Compounds [FOI
3.1.1.5 Blank Summary [FOE
3.1.1.6 Laboratory Control S"ampi« Data^B^kee^XFORM Jll - AASV]
\ \ / /
and Mass Calibration
-TIC]
3.1.1.7 GC/MS Instrument Performance
[FORM IV - AASV]
3.1.1.8 Initial Cali
3.1.1.9 Continuing CXlib?)s.ti
3.1.1.10 Inter
[FO
>RM V - AASV]
'ORM VI - AASV]
ion Times Summary
AASV]
3.1.1.11 Filte^Adsott^etft Cartridge Certification [FORM VIII - AASV]
3.1.1.12 Surrogate R^BQveryHFORM IX - AASV]
3.1.1.lXAnalyticai>S«quencV^FOR^ X - AASV]
3.l.tf.lVSample Rec£ipt/l>pg-In Sheet [FORM AADC-1]
3./.1A5 Complete SDG F^le \(CSF) Document Inventory Sheet
'd Header Information
3.1.2 G
3.1.2.1 VaUta§ musl
the individual
reported on the hardcopy forms according to
tructions in this Section. For example,
January, 1992
Page B-18
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
results for concentrations of semivolatile organic
must be reported to three significant figures if
than or equal to 10, and to two significant figur
than 10.
jet compounds
tlue is greater
values less
3.1.2.2 All characters which appear on the daz
presented in the contract must be reproduced /by
submitting data, and the format of the forms
identical to that shown in the contract. Nvj^iformation
deleted, or moved from its specified posiirion> without prior
approval of the EPA APO. The names of tWe various fields and
compounds (i.e., "Lab Code," "Pentachlo^roph^nol") must appear as they
do on the forms in the contract.
3.1.2.3 Alphabetic entries made on'
shall be in ALL UPPERCASE letters
the forms/by/the Contractor
,.€.>£ar42re'ssoi~>x6he facility performing the analyses (see Lab Code) .
Ll/2.4.4 The "Case No." is the EPA-assigned case number
associated with the Cample, and reported on the Traffic Report.
L1.2>4sl5 The "SDGf No/." is the Sample Delivery Group (SDG)
nurftfeer. Tbe SDG No/ is the EPA Sample Number of the first sample
received in Che SDG. /When several samples are received together
in the firs£ SDG^shipment, the SDG number shall be the lowest
January, 1992
Page B-19
-------
Exhibit B
Semivolatile Grganics Analysis of Ambient Air
sample number (considering both alpha and numeri^
the first group of samples received under the
designations) in
3.1.2.4.6 The "SAS No." is the EPA-assigne/i nufcber for analyses
performed under Special Analytical Services/(SAS) ^"-tf samples are
to be analyzed under SAS only and reported/on/8ie«e forms, then
enter SAS No. and leave Case No. blank.
according to the "Routine Analytical Sei
an
zed
have additional SAS requirements, list/
on all forms. If the analyses have
"SAS No." blank. Note that some s<
No. while others do not.
Lf ssamples
is" (IFB)
Case No. and
requirements, leave"1
in an SDG may have a SAS
3.1.2.5 The "EPA Sample No." is the/other infoi
of the forms. This number appears e^itherxin th? u
the form, or as the left column of
number of samples. When the "EPA Sampl
triple-spaced box in the upper right cornef^xit s
the middle line of the three lines that compris^
on common to most
er right corner of
zing data from a
entered into the
Id be entered on
,theS
3.1.2.5.1 All samples,/blanEs~r~a»d^standards shal^f be identified
with an EPA Sample Numbeir. >F«o^field sample^—the EPA Sample
Number is the unique identifying numUej: given in J&ie Traffic
Report that accompanied tha\ sample.
3.1.2.5.2 In order to facili^ate^da^a assessment, the following
sample suffixes must be used:
XXXXX
EPA sample number^
XXXXXD
XXXXXRE
3.1.2.5. 3^xSenu^o^la/ilef standards prepared on PUF/XAD- 2
cartridges sKJrll beidantified as SVSTD###, where ### is the
concentration inTsg. (on^xplumn) of the semivolatile standards
OSbSO-OO/^and 200).
Lhe blanfcx./dentifiers, these designations will
other information to uniquely identify
Blanks shall be identified as SVFBLK## and
shall be identified as SVMBLK##. The
unique for each blank analysis within an
characters
possible
SVMBLK01,
t achieve this by replacing the
ernfrnator of the identifier with one or two
rs/ or a combination of both. For example,
for semivolatiles-PUF/XAD-2 blanks would be
etc.
Januarv, 1992
Page B-20
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.2.5.5 LCSs shall be identified as SVLCS##
No." must be unique for each LCS analysis withi:
laboratory must achieve this by replacing the
terminator of the identifier with one or two
numbers, or a combination of both. For
identifiers for semivolatiles-PUF/XAD-2 car,
SVLCS01, SVLCS02, etc.
ie "EPA Sample
''SDG. The
Character "##"
acters or
issible
would be
3.1.2.6 Several other pieces of informatic
Data Reporting Forms. These include Lab
Received, etc. Following is a brief desj/rip
entries.
:ion of each of these
3.1.2.6.1 "Lab Sample ID" is an/opoional laboratory-generated
internal identifier. Up to 12 aVpha/numeric/characters may be
reported here. If the contract^ doeSs^iot Jnavjt a Lab Sample ID,
this field may be left blank.
3.1.2.6.2 "Lab File ID" is the laboratbcv-gefie«ted name of the
GC/MS data system file containing informatiohsperta^ining to a
particular analysis. Up £«Lj.4^alpha-numeric characters may be
used here.
3.1.2.6.3 "Date Received? ik the dape o£_gample
laboratory, as noted on theNTratfic Report (i.e.
should be entered as MM/DD/YY\ \/ /
receipt at the
the VTSR). It
3.1.2.6.4 "Date Extracted" is "fche date the sample was extracted
by the laboratoryx"Tt^sb
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
to be retained by 1 (round up). If the figure following the last
digit to be retained equals 5, round up if the digit/to be retained is
odd, and round down if that digit is even.
3.1.2.8 All results must be transcribed to t
with the specified number of decimal places pha
Exhibit B. The raw data result is to be ro'
of figures in the raw data result exceeds
figures specified for that result entry
not enough figures in the raw data resu
space for that result, then zeros must
the specified number of reporting
specific form. The following exampl
dec:
Raw Data Result
Specif/
the raw data
ar>sdescribed in
only when th~exnuraber
imum numoter of
:hat form. If thfexe are~>
enter in the specif:
ed for decimal places to
for tha"^N:esult for a
prov}
Correct Entry
3.1.3 Cover Page [CO1
3.1.3.1 This fo
within an SDG, afnd
general comments.
Laboratory Ma/ag;
3.1.3.2 Under S
for the EPA sample
required
suffix /These s
alphajuim
Code/co
al
e
5.9
5.99653
95.99653
995.99653
9995.996
99995.9
999995.9
NOTE: 6.3 stands for a maximum
three decimal places.
.900
.997
95.997
5.997
'996.00
99995.9
invalid
significant figures and up to
to\ list all 6>ill^ble samples analyzed
provide'xcer£jtin analytical information and
[so the docijtmaiu: which is signed by the
iori/ze aruKreleAse all data and deliverables
associated w/Lth She SDG.
alphanumeri
applicable.
le No." column, enter up to 7 characters
ncluding blanks and duplicates) for each
Duplicates must contain a "D"
numbe^ss musyt be listed on the form in ascending
the Extended Binary Coded Decimal Interchange
f MAB123A is the lowest (considering both
ctWs) EPA Sample No. within the SDG, it would
EPV Sample No. field. Samples listed below it
quince - MAB124A, MAB12AB, MAB125A, MAC111A,
umbers must be listed in ascending
inuing to the following Cover Page if
January, 1992
Page B-22
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.3.4 Under "Lab Sample ID", a Lab Sample ID (up,
may be entered for each associated EPA Sample No.
is entered, it must be entered identically (for
on all associated data.
3.1.3.5 Under "Comments", enter any problems
technical and administrative, the corrective/act
resolution performed for all of the samples/in;
3.1.3.6 Each Cover Page must be signed,
Laboratory Manager or the Manager's des
the release and verify the contents of
associated with an SDG.
10 characters)
Lab Sample ID
Sample No.)
3.1.4 Analysis Data Sheet [FORM I -
3.1.4.1 This form is used for tabula"
analysis of samples on PUF/XAD-2 cartri
Target Compound List for Semivolatiles as
orting results for
;he compounds in a
ibit C.
3.1.4.6 For
month/day/yea^r )
on the Traffic
(VTSR)].
3.1.4.7
month/
3.1.4.2 This form is used f<
of the target compounds in
control samples, and perfo
3.1.4.3 Complete the header i;
according to the instructions
3.1.4.4 For "Lab Sample^ ID", enter
as listed on the Co
3.1.4.5 For "Cle/nui/'Proc
(Lobar or 610).
icentrations
'aboratory
page of Form I-AASV
ab sample ID for the sample,
b File ID", if applicable.
leanup procedure used
used, enter "NONE".
Extra
thes^mp1e c
fate (formatted
is received'at the laboratory, as recorded
., the Validated Time of Sample Receipt
the date (formatted
fge was extracted.
3.1.4.10
enter "1".
lyz^d," enter the date (formatted
extract was analyzed.
D", "GC Column ID", and "Injection Volume
lupion factor. If no dilution was performed,
January, 1992
Page B-23
-------
Exh
Lt B
Semiv< :ile Organics Analysis of Ambient Air
3.1.4.11 Enter the "Air Sample Volume" corrected
temperature and pressure (STP) in cubic meter (m3)
ambient air sampled is not known, enter "NA".
standard
If the volume of
3.1.4.12 Under the column labeled "Concentration" ifsshe analytical
result is greater than or equal to the Contract Sfequ^red Qbantitation
Limit (CRQL), report the result. If the result/is lowetxthan
CRQL, report the value followed with a "JVonder the "Q" cc
section 3.1.15). For example, if the
the detected level is 3 ng, then enter
"J" under "Q". In this analysis, the
column injected and "ng/m3". Both col
volume of ambient air sampled is
volume of ambient air sampled is not
only the levels in ng injected is rport
an analyte is 5
ider the "ng" column
}L/is expressed in "ng" on-
must be^illed if the
the laXorafcory. If the
iwn to t&e Jiaboratory, then
3.1.4.13 Analytical results must be refJbr^ed te^two significant
figures if the result value is less than lON^Valxlfee greater than or
equal to 10 shall be reported to three significant figures.
3.1.4.14 The requirement fcft reporCtng-j^sults to two^e-r three
significant figures appliesNto 1TORM^i::AASVonT^r---EaLlow the specific
instructions for reporting al\ abtjerresl^.ts/r_aj\_required forms as
described in this Exhibit.
3.1.4.15 For reporting results to\the Agency, the following contract
specific qualifiers are to be used.\ Thefseven qualifiers defined
below are not subjec£-'fo~~m«dification\by\he laboratory. Up to five
qualifiers may be Reported oty Form I-AftSV for each compound. The
seven EPA-defined/qualifiers $o_be used are Xs follows:
U -
J -
Indic
sampl
es/compou
antitatn Jfimit
but not detected. The
corrected for dilution.
Indifc&^es ablestima'ted value. This flag is used either when
estimatinga concentration for tentatively identified
compounds wltare aixl response is assumed, or when the mass
_data ihdlcateXrtie presence of a compound that meets
but the result is less than the
^tion Ifmi/t but greater than zero. For
sample quantitation limit is 20 ng, but a
ng is calculated, report it as "10J".
ation limit must be adjusted for dilution.
Five evidence of a compound. This flag is
atively identified compounds, where the
s based on a mass spectral library search.
all TIC results.
January. 1992
Page B-24
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
B -
E -
This flag is used when the analyte is found/I^ the associated
blank as well as in the sample. It indicates,
possible/probable blank contamination and/wairtis the data user
co take appropriate action. This flag must/be used for a TIC
as well as for a positively identified/targe^ compound.
This flag identifies compounds whose/coneeivCx£tiortsxexceed
the initial calibration range of th6 iristrumenbxfor that
specific analysis. If one or moreSsojdpounds haveaxre spoTis e
that exceed the initial calibration'Jrange, the sample
extract must be diluted and reanalyzed according to the
specifications in Exhibit D. /6.1/such compounds should have
the concentration flagged with ad "E" on yfhfe Form I for the
original analysis. The dilutioia of the Sample may cause some
compounds identified in the/first analysis'to be below the
calibration range in the s4conoNanaly,sis / The results of
both analyses shall be reported on'Wpaii'ate FORM Is. The
FORM I for the diluted sample sha^l hav«^ the "DL" suffix
appended to the EPA Sample Number.
X -
mus
Other specific flag;
results. If used,
description attach
the SDG Narrative.
flag is required, use
five qualifiers are reqi
flag to combine several
"X" flag might combine the
sample.
letters
be required to pfbRerly" define the
described, and such
Sample ISata-SaHmary Package and
If/more than one
If more than
r A sample result, use the "X"
needed. For instance, the
and "D" flags for some
"TabbTsatory-defined Elags are limited to the
"Y", artd "Z". \ \
NOTE: The combination ofjfllgs If6tT or XtfB" is expressly
prohibited. B^ank/contamin'ants-ia<£ fla"gg^d "B" only when they are
detected in tfte sample.
3.1.5 Tentatively. Identi|/ed/6ompounds [FORM I - AASV-TIC]
3.1.5.1 FORM I-AASV>SJC is^
estimated^-eoiioentration
interned standard, and non-1
3.1
ev
;ed for reporting the identification and
10 of the non- surrogate, non-
;et/compounds.
3.1.5.3 Sample"
instructions
AASV—TIC for every sample, performance
analyzed. FORM I-AASV-TIC must be
that requires a FORM I-AASV for target
led dilutions and reanalyses, even if no
information according to the header
3.1.2.
January, 1992
Page B-25
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.5.4 Total the number of TICs found, and enter /this number in the
"No. of TICs Found". If no TICs were found, enter/I0"/(zero).
3.1.5.5 Report tentatively identified compound.? (T&Qs) including "CAS
RN", "Compound Name", "RT" (retention time), and the
concentration (criteria for reporting TICs are g/ven\j.n Exhibit D) .
Retention time must be reported in minutes and .decimal minutes^ not
seconds or minutes and seconds.
3.1.5.6 If in the opinion of the mass s|
specialist, no valid tentative identifi
compound shall be reported as unknown.
3.1.5.7 Under the column labeled
identified in section 3.1.4. If a<
explicit definitions must be include?
Comments section.
3.1.6 Blank Summary [FORM II - AASV]
3.1.6.1 This form summarizes
and laboratory method blank\a:
Form II-AASV is required for
3.1.6.2 Complete the header ii
in section 3.1.2. The "EPA Sampl«
of Form II-AASV shall be the same
when reporting resu
al interpretation
on can be made, the
qualifiers as
are used, their
Page in the
th each field
appropriate
' Form I-AASV.
Form II-AASV as described
tered in the box at the top
entered on the Form I-AASV
3.1.6.3 On the
associated with
identifies the
provided unde
3.1.7 Laborato
3.1.7.1 Form III-A&
analytes
sample numbers
:her information which
ID for each sample must be
iff available.
Data Sheet [FORM III - AASV]
to report the recovery of the spiked
samples (LCS).
rmation according to the instructions
time the LCS was analyzed.
"Spiked," enter the spiked concentration
in ng^Hper mjection) 6f e/ach LCS compound. Under "Reported," enter
the conce'Rtratbxiobtained in ng (per injection) calculated from the
analysis of^sl^e LC5v C/lculate the percent recovery of each LCS
compound to theNi^areSyC whole percent and enter in the column under
January, 1992
Page B-26
-------
Exhibit B
Seraivolatile Organics Analysis of Ambient Air
"% Recovery". At the bottom of the table are the QC^Limits for LCS
percent recoveries. Flag all values outside of thp limits with an "*"
in the column under the "Q" symbol.
3.1.7.5 Summarize the values outside the QC li^mits^t the lower part
of the form.
3.1.8 GC/MS Instrument Performance Check and
[FORM IV - AASV]
iss/Calibral
3.1.8.1 This form is used to report the/results of GC/MS instruml
performance check (also known as "tuning")/and to summarize the date
and time of analysis of samples, standards, and b/artks associated with
each analysis of the instrument performance checX solution.
3.1.8.2 Complete the header infori^atiohx^s ir/section 3.1.2. Enter
the "Lab File ID" for the injectionifrentairtirig me instrument
performance check mixture. Enter the date and 4^6 (military time) of
injection of the instrument performance chebk^mixtttrje.
3.1.8.3 For each ion listed,
abundance in the right coli
number of significant figui
criteria column.
the form, enter thexperafent relative
Report—Sfij^tiye abundances to the
for eachion—-HW-the ion abundance
3.1,8.4 Under "to m/e 198", all\ior
to the nominal base peak listed on\Foi
ions, determine the percentage of tl
mass and report undear^To^specified
relative ion abundance of mas.s 443 and
"to m/e 198" column 4rre~]TCKanffl $&, resp>
(under the "to spec/fied maps''column) as
443 relative tc/ma6s 442.
inces are to be normalized
'-AASV. For some of the
abundance to the specified
For example, if the
.442 ions under the
rely, then enter "20"
ion abundance of mass
3.1.8.5 All^rela^ve ab
zero, enter "tX^ not^a./last
ices must be reported as a number.
or other non-numeric character.
If
3.1.8.6 In the lowervhalf"sbf the form, list all samples and standards
analyzed under—fch^t insrisument^pfirformance check in chronological
order. Jw time of analysis cin military time). Refer to section 3.1.2
for s^cL£5TcTTns~t*4ictibns for identifying standards and blanks. Enter
"EPA/Sample No.", "brt> Sample ID", "Lab File ID", "Date Analyzed", and
"Time Analyzed" for al^ standards, samples, and blanks.
The GC/MS instiumdnt performance check must be analyzed again
the time /of injection of the instrument performance
check^s^lutibo listed /at /he top of the form. In order to meet these
requirements, samples/ standards, or blanks must be injected within 12
hours of the^injectl/on f>f the instrument performance check solution.
January. 1992
Page B-27
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.9 Initial Calibration Data Sheet [FORM V - AASV]
3.1.9.1 Each time the GC/MS system undergoes a
to initialize subsequent quantitation of semivoj
blank analysis, the laboratory must complete ai
'point calibration
'atiltes in sample and
Form V-AASV.
3.1.9.2 Complete all header information as /m ,/ection
3.1.9.3 Enter the "Case No." and "SDG No/"
package, regardless of the original Case/for/which the initial
calibration was performed. Enter "Inst/umerit ID"I/N"GC Column ID", and
"Injection Volume" in microliters.
3.1.9.4 Enter the "EPA Sample No."/and/"Lab Fi/e
five calibration standards.
3.1.9.5 Enter the injection dates and times of'•each
calibration standards analyzed under "Date ihVI - AASV]
3.1.10.1 Each
calibration ta ct
laboratory m\
3.1.10.2 Complete
the "Case No." and
of the or>i
Enter
recent
caliji
AAS;
the GC/MS
3m una*»goes a continuing
ne tfalidityv^f/the initial calibration, the
)lete/and/submit a Form VI-AASV.
for
3.1.10.4
response fact
recent valid inft
11 heg&er information as in section 3.1.2. Enter
No/^xfor the current data package, regardless
ich che initial calibration was performed.
GC CbJ.umn/ID" , and the date(s) of the most
pn. Ir^ene calendar date changes during the
inclusive dates should be given on Form VI-
time of injection of the continuing
"1C mean RRF", enter the mean relative
target compound as determined in the most
libration.
Januarv, 1992
Page B-28
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.10.5 Complete the relative response factor (RRF/9
each target compound in the space provided.
calculation for
3.1.10.6 Calculate the percent difference (%D) Between the continuing
calibration RRF and the mean RRF from the most /ecent^valid initial
calibration for each target and surrogate compyaund^and e^ter the
values obtained under the "XD" column.
3.1.10.7 At the last Form VI-AASV, enter
Sample ID, and date and time of analysis df
associated with the continuing calibration.
iPA Sample numt^er,
2 samples and blc
3.1.11 Internal Standard Area and Reten}
[FORM VII - AASV]
''Time St
3.1.11.1 This form is used to sumnlarize^^he neak/areas and retention
times of the internal standards addedxt^o allvsamples and blanks. The
data are used to determine when changes rt^interiial standard responses
will adversely affect quantification of targetcomjremids. This form
must be completed each time an initial or continuing calibration is
performed for each GC/MS syst
3.1.11.2 Complete the head
ition
section 3.1.2.
the
3.1.11.3 Enter the Lab File
as well as the date and time of
If samples are analyzed immediate!
before another instrument performan<
calibration, a FornyVTI^ASSV shall be
internal standard ,areas_of tfte mid leve\ (
sequence standard/ Use th
standard, and ios L/b File
continuing calibration sta
aur
fol
and time
in
ration standard,
the calibration standard.
ing an initial calibration,
k and a continuing
eted on the basis of the
, 3) initial calibration
analysis of this
lace of those of a
3.1.11.4 Fr^m tfie-^resuit's of the analysis of the 12-hour calibration
standard, ente^Js^the ase^ measured for each internal standard and its
retention time (ih^decima]/minutes) under the appropriate column. For
each internal standard.calbuLate the upper limit of the area as the
area of th«--paYtHtcular sbandardx^lus 40 percent of its area (i.e., 1.4
times tKe area in tn>sJ.2 HOtlRsSTD/box), and the lower limit of the
area SLS the^area>»f the\internaT>/standard minus 40% of its area (i.e.,
0.6 /im»s the area itv thev12 HOUR STD box). Report these values in
the/bojfes labeled "UPP^R UJMIT" and "LOWER LIMIT", respectively.
uppter limit of the retention time as the
1 standard plus 0.33 minutes (20 seconds), and
retention time as the retention time in the
'es (20 seconds) .
January. 1992
Page B-29
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.11.6 For each sample and blank under a given
sequence, enter the EPA Sample Number and the are
internal standard and its retention time. If th<
area is outside the upper or lower limits calcu
area with an asterisk (*) placed in the far rig'tit-^hanci'
box for each internal standard area, directly/un
Similarly, flag the retention time of any i
outside the limits with an asterisk.
3.1.12 Filter/Adsorbent Cartridge Certific/tioh [FORM VIII - AASV]
aur analytical
for each
ternal standard
^above, flag that
ace of the
symbol.
is
3.1.13 Surrogate IJfeco/ery [F<
3.1.13.1 Forpf I
surrogate compo
3.1.13.2 Comple
as described in
recovery
signifj/cant
3.1.
3.1.12.1 This form is used to documer
cartridges prior to use.
3.1.12.2 Complete the header info
AASV according to the instructions
3.1.12.3 Enter "Filter Batch No.", "PUF
No.", where applicable.
3.1.12.4 Enter the results/of the
clean cartridge. For targe^ c
the CRQL of the compound fol
less than the CRQL, enter the
ibation of PUF/XAD-2
,ch/page of Form VIII-
.Z.2.
and "XAD-2 Batch
ed certified
Detected, enter
tected level is
3.1..12.5 If none of the values
than the corresponding CRQL of any
total level of semivjeiatTi^s is not
the cartridge is certified.
icular cartridge are more
thfe target compounds, and if the
earer than 10 jig/cartridge, then
column,
le numbe
(Total
limi
td^epotft the recoveries of the
'each PUF/S3O)-2 adsorbent cartridge.
information and enter EPA Sample Numbers
For each surrogate, report the percent
itage point, and to the number of
limits at the bottom of the form.
,ate recovery outside the QC limits with an
must be placed in the last space in each
the "#" symbol. In the far right-hand
surrogate recoveries outside the QC limits
If no surrogates were outside the
January, 1992
Page B-30
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3.1.14 Analytical Sequence [FORM X - AASV]
3.1.14.1 A Form X-AASV is required for each analytical sequence for
each GC/MS system used to perform semivolatile analysis on PUF/XAD-2
cartridge samples in an SDG.
3.1.14.2 Complete the header information on fact
according to the instructions in section 3.1/2.
of
X-AASV
3.1.14.3 On the numbered lines, enter the/EFA sample numbers a3
with the other information which identifies ,che samples, blanks, at
standards. The first item in the table/muse be the DFTPP since the
12-hour time period starts at the inje/tiori of the/instrument
performance check standard. Arrange ydhe/i terns it/chronological order
for each GC/MS system.
3.1.15 Sample Receipt/Log-In Sheet [FOB
?rm
th>
led to
3.1.15.1 This form is used to document the
sample containers and samples. One original o
required for each sample shinpiiigcontainer. If
single sample shipping container mus
Sample Delivery Group, the origJnai^Egrm AADC-
the deliverables for the Sample D«slivery~]2roup_of th<
number and a copy of Form AADC-1 must be/placed wit
for the other Sample Delivery Group(a) ./ The copies should be
identified as "copy(ies)," and theN^Locati^on of the original should be
noted on the copies.
nd inspection of
-1 is
les in a
e than one
be placed with
lowest Arabic
the deliverables
3.1.15.2 Sign and/date.
shipping contained and rec
and their condition/^i.e., intact
Record the custody/seal numbers
he airbill (ifXpre'sfint). Examine the
d phe_presencV/aBsence of custody seals
ken)\£n item 1 on Form AADC-1.
itern^
3.1.15.3 Opefo thexcontayher,
documentationT
record(s), SMO forms (i.e.
airbills or airbill sbipkerl
there is an—airbill pres«
AADC-1./Record theairbill"
remove the enclosed sample
presence/absence of chain-of-custody
Traffic Reports, Packing Lists), and
.n items 3-5 on Form AADC-1. Specify if
or an airbill sticker in item 5 on Form
stacker number, if present.
Remove the^-samp^ies from the shipping container(s), examine
thesamples and the saropleXtags (if present), and record the condition
of /the' sample (i.e., inttactl dent, leaking) and presence of absence of
nplex^ags in items 6 apd y on Form AADC-1.
3.1. l$>»i Review the s^mpl/e shipping documents and complete the header
informatibn^desctibed/in/Section 3.1.2. Compare the information
recorded on a!4^ the^ocvunents and samples and circle the appropriate
January. 1992
Page B-31
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
Receipt, sign and
record, and
3C-1. Record
if
Jorm
answer in item 8 on Form AADC-1.
3.1.15.6 If there are no problems observed durij
date (include time) Form AADC-1, the chain-of-
Traffic Report, and write the sample numbers
the appropriate sample tags and assigned lab$
applicable. The log-in date should be reco^
AADC-1 and the date and time of sample rec«
should be recorded in items 9 and 10. Re/or^ the specific
designation (e.g., refrigerator number) /in the Sample Transfer bl
located in the bottom left corner of Form ytADC-1. Sign and date the
Sample Transfer block. Cross out unus4d -columns Xndj spaces.
/ /
3.1.15.7 If there are problems observed during^receipt or if an
answer marked with an asterisk (i.^. , etb^ent^') jwas circled, contact
SMO and document the contact as wellNas res^aiution of the problem on a
CLP Communication Log. Following resolfctt^pn> sq.m and date the forms
as specified in the preceding paragraph anaNj^pte/^Hh^ere appropriate,
the resolution of the problem.
3.1.16 Complete SDG File (CSF/ Docume
3.1.16.1 This form is used
Purge documents and count of
Package which is sent to the
Cgntory
AADC-2]
iZgntory yf the SDG File
original Sample Data
3.1.16.2 Organize all EPA-CSF dociijqent^ as described in Exhibit B,
Section 1. Assemble^Che^TiQcuments irk thev order specified on Form
AADC-2, and stamp >each_page v?ith a conSvecu\ive number. (Do not number
the AADC-2 form)/ Inventory Vhe CSF byNreviewing the document numbers
and recording p^ge >nurabers jrangesls.the columns provided in the Form
AADC-2. If thkre/are no dacumejats^ fc^a.^specific document type, enter
an "NA." in th& empty space
3.1.16.3 Cer^fcain rafe^atoiy specific documents related to the CSF may
not fit into a clearly defined category. The laboratory should review
AADC-2 to determine'ii it ts^most appropriate to place them under No.
16, 17, l£-r-*f—3^- Catfegpry iS^should be used if there is no
appropiriate previcoJs^categcjisx. TJiese types of documents should be
descr/bed^6rTl>feed irNphe blahks under each appropriate category.
Januarv, 1992
Page B-32
-------
Exhibit B
Semivolatile Organics Analysis of Ambient Air
3 .2 Data Reporting Forms
3.2.1 Cover Page [COVER PAGE - AASV]
3.2.2 Analysis Data Sheet [FORM I - AASV]
3.2.3 Tentatively Identified Compounds [FORM I
3.2.4 Blank Summary [FORM II - AASV]
3.2.5 Laboratory Control Sample Data Sheet
3.2.6 GC/MS Instrument Performance Check/am
[FORM IV - AASV]
3.2.7 Initial Calibration Data Sheet <(FO]
3.2.8 Continuing Calibration Data Sheet
3.2.9 Internal Standard Area and Retention Times
[FORM VII - AASV]
3.2.10 Filter/Adsorbent Cartr^i
3.2.11 Surrogate Recovery [FORM
3.2.12 Analytical Sequence [FORM X \
3.2.13 Sample Receipt/
3.2.1A Complete SDC/Fi/e
.III - AASV]
iC-1]
ry Sheet [FORM AADC-2]
.Inri'iarv, 19P2
Page B-33
-------
Lab Name:_
Lab Code:_
SDG No.:
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Comments:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
COVER PAGE
Contract No.:
Case No.: /
SAS No.: /
/ 7
EPA Sample No.
/O
\ \
\
/ /
7
7
V /
\
I certify that this/da
technically and/for
contained in mis
has been authorized b"
Signature:
Date:
pliknce with the terms and conditions of the contract, both
;er than the conditions detailed above. Release of the data
ana in the computer-readable data on floppy diskette
ar/ager's Designee, as verified by the following signature:
Name:
Title:
COVER PAGE - AASV
-------
Lab Name:_
Lab Code:_
SDG No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Scmivolatile Organics in Air
SAMPLE RECEIPT/LOG-IN SHEET
Contract
Case No/:
SAS
4 / \^ ^X
ITEM
1. Custody Seal(s)
REMARKS
Present/Absent/Intaci/Broken *
2. Custody Seal No(s). |
1
3. Chain-of-Custody records
' 4. Traffic Reports or
Packing List
; 5. Airbill
i Airbill No(s).
j 6. Sample Tags
! Sample Tag No(s):
7. Sample Condition
i 8. Do informations on custody
Present/Absent*
Present/Absent*
Sticker/Present; Absent *
/
\
Present/Absent*
Listed/Not Listed on COC
Intact/Broken/Leaking*
^ ^
records, traffic reports, and : /
sample tags agree? > )fes/N«r \.
9. Date Received at Lab: / / j
, 10. Time Received at Lab: / / /
Sample Transh^ ^X^ / /
: Arca#: | "\^ "^^ /
By: "\ X
On:
^ -^ ^x
EPA
Sample No.
/
^
-^H
^v— J
\ \
\ \
\
\
\
}
s ^
\^
X
Sampte^i, Assigned
Ta/No/f Lab No.
/ /! „
/ /
/
\^
"X. X
\
-~— _
^^***-
-«-^
7 r
, / /
v /
s \
\ \
\ ;
. V
s /
/ ;
/ /
/ /
/
\ ^^
\
•^-— ^
Sample
Volume
X^
X/
R&M^jEUCsT^oiiditions
of Sampl^finipment^ctc.
'•' Contact SMOand atlaci
Received by:
Signature:
Print Name:
Log—in Date:
Reviewed by:
Signature:
Ln»b(x)k No.:
Date:
Logbcx)k Page No.:_
FORMAADC-1
-------
Lab Name:_
Lab Code:_
SDG No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
COMPLETE SDG FILE (CSF) DOCUMEf
INVENTORY SHEET
Contract
Case No
SASN
/x~
DOCUMENT / /
1. Cover Sheet (Cover Page - AASV) / /
2. Sample Receipt/Log- In Form (FORM AADC- ly /
3. CSF Document Inventory Sheet (FORM AADC-/2) /
4. Analysis Data Sheet (FORM I - AASV) / <\ /
5. Tentatively Identified Compounds (FORM I - A^V-f^S)/
6. Blank Summary (FORM II - AASV) "\ j
7. Laboratory Control Sample Data Sheet (FORM III - AASV^
i 8. GC/MS Tuning with DFTPP (FORM IV -AASV) ^
9. Initial Calibration Data Sheet (FORMA1— AASV)
10. Continuing Calibration Data Sheet (fOKM VI - AXSVy — «^_
11. Internal Standard Area and RT Summary ^SRTtf-VILsr AASV)
i 12. Filter/Cartridge Certification Data SheeKFORM VIII / AjBVf
13. Analytical Sequence (FORM IX -AASV)\ \ / /
14. Percent Surrogate Recovery (FORM X - AA^V) v /
15. EPA Shipping/Receiving Documents \ (
Airbill (No. of shipments:/'^) ~~\ \ \
Chain-of-Custody Re/fords. — ^ \ \ \
Sample Tags / / \ ^ — ^ \ /
Sample Log- In Sheet (Lab & AADC- 1) \^ v
16. Misc. Shipping/Re^eivi^g Records ffist ipCfivIJoa^ record^
Telephone Logs/ ^ / / ^--V
*X ^\ / /
'• ^^ /
^^ ^\
', 17. Internal Lab-Saraplc^Ctansfer ^eBQrds ^X^
IS. Interna^&riginaLSample^reparation^HwJ Ansrlysis Records
Page Nos.
From
/ 7
/ /
/
/
X
\
X
^7
-^y
To
X.
?
^^
Please Che>k
Lab T^eg |
,., „, . ^
*
j i
i
19. Othe/Repdfds (descrWpr listV !
/ / X \ i i '
Completed by (C:
Signature:
Audited by (EPA):
Signature:
Printed Name/Tille:_
Printed Name/Title:
Daie:_
Dale:
FORM AADC-2
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Scmivolatile Organics in Air
ANALYSIS DATA SHEET
Lab Name:
Lab Code:
Lab Sample ID:
SDG No.:
Contract N6.: \. \^
\^\
7
La^Fi^ID: >Sv/
SAS/No.: /^
Date Received: Date Extracted: / / Date Analyzed:
Instrument ID:
7
Cleanup Procedure:
Air Sample Volume ( STP):
CASRN
83-32-9
208-96-8
98-86-2
116-06-3
309-00-2
62-53-3
120-12-7
22781-23-3
92-87-5
56-55-3
50-32-8
205-99-2
192-97-2/
191-24,4
207-0^-9
m3
COMPOUND
j — — »^^_
NA>fE_
Acenaphthene \ \
Acenaphthylene
\\
Acetophenone \
Aldicarb ^,
Aldrin S ^ \
Aniline / / >> \s — \
Anthracene' / / — ^
Bendiocaro ^ / /
BenzidmVx^ ^\/ /
Benz[a]anthraceiDe^ x^
Benzofafayfeu^ ^\ "X^
B^nzojbJfluQranttiene \^y
de-Column I£
);
Dilution FaOTor:
Injectio^kVolui
bftiuL):
Concentration
--f^.
// ~
^ /
\\
L \)
^^-,
\^y
1ng/m3 Q
<—/
i
! i
!
! i
i
BeraofejpyreneX \ ; i
Benzo[g,h,i]perylene\
1B^nzo[k]tluoranthene
I00-5i^v§enzy>alcohol /
319-84-6
58-89-9
92-67-1
\
/
alph^BHtX^ / / !
gamma— BHQ (Lindane)
p- Biphenylamiife/
84-74-2! Bis(n-butyl)phthalate
FORMI-AASV-1
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
ANALYSIS DATA SHEET
Lab Name:_
Lab Code:
Lab Sample ID:
SDG No.:
Date Received:_
Instrument ID:
Date Extracted:
Cleanup Procedure:
Air Sample Volume (STP):_
CASRN
85-68-7
133-06-2
5103-71-9
5103-74-2
COMPOUND NAME—-^.
Butylbenzylphthalate \ T~-
Captan \ \
alpha— Chlordane \
gamma— Chlordane \
Conbei
_ ng
^^-^
^7 /-^
^/ /
v/
59-50-7 U-Chloro-3-mefhytphenpl |\ \
106-47-8 i 4-Chloroanilin/ / — ^ \
lll-91-i
111-44-4
1897-45-6
2921-88-2
218-01-9
1861-32-1
72-54-8
T2-55-9/
50-29/3
333-4^5
Bis(2-chlor9e/tho^)methkne ^ ^
Bis(2-chlpyoe^l)ether / /^~^\
Chloroth/lonik^ / /
ChlorpyrifoV^ \/ /
Chrysene ^"^x^ ^\^
Da9thaT(DCPA^ ^x^ ^X
tfi-JdOD — \ \ \/
^4,4^-DDE \ \
4^4'-DDT \ \
Diazipon } }
53-70-3 ^Bir^enzlJr&lanthrace/e /
62-73-7 Dichk>rvQs (E^BYPJ /
115-32-2
Dicotbl ^\ /
\ \
K V
[ "-7
^^/
[itratfon
^96/m3
-'^.
7
Q
i
60-57-1 IDieldrin
FORM I - AASV-2
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semhrolatile Organics in Air
ANALYSIS DATA SHEET
Lab Name:_
Lab Code:
Lab Sample ID:_
SDG No.:
Date Received:_
Instrument ID:
Date Extracted:
Cleanup Procedure:
Air Sample Volume (STP):_
1
! CASRN
i 84-66-2
; 105-67-9
131-11-3.
534-52-1
51-28-5
COMPOUND NAME _
Diethylphthalate \ \
2,4-Dimethylphenol \ \
Dimethylphthalate \
>
4,6 — Dinitro — 2 — mgitydphenol
2,4— Dinitroph^riol \
121- 14-2 j 2,4-Dinitrotp(hiejlfe \ T--^v
Concentration
--« —
. //
v/
\ \
\ \
. \/
ng/m3
7
•*^/
Q
959-98-81 EndosulfanX /
33213-65-9
72-20-8
7421-93-4
; 533-41-5
117-81-7
206-44-Oy
86-73^7
Endosulfem Il£
Endrin \s^ ^\/
Endrin aldehydeX^
/ / 1
/
/
Endjariretone^ \^ \^
B^2^>ethy4he^)phtjwlateVx\/
Fluoranthene \. \
^iuorene \
!33-(?7-3 fcalpet i
76-44-8x4jeptachl£r /
1024-57-3
118-74-1
77-47-4
HepfetclilorepQxid/
Hexachlorbbenzene /
i
i
\ !
J --
7
/
Hexachlorocyclopwtadiene
i
1 !
I
i
! !
hi-12-1 Hexachloroethane
FORM I - AASV-3
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
ANALYSIS DATA SHEET
Lab Name:_
Lab Code:
Lab Sample ID:_
SDG No.:
Date Received:_
Instrument ID:
Date Extracted:
Cleanup Procedure:
Air Sample Volume (STP):_
CASRN
193-39-5
78-59-1
72-43-5.
91-57-6
95-48-7
106-44-5
2385-85-5
91-20-3
91-59-8
88-74-4
100-01-6
98-95-3
92-93-3
COMPOUND NAME „
Indeno(l,2,3-c,d)pyrene \ ^ — ^
Isophorone \ \
Methoxychlor \ >
2— Methylnaphthalene \
2 - Methylphenol/-- v
4-Methylphen^l x-^x \
Mirex / / \ \^~~^
Naphthale/e / / / \
2-NapI^tnyla'mine / /
2-NitroaruTkj^ "^^ /
3 — Nitroaniline ^\^ ^x^
NijFoBehzene^-v^ ^x^ ^x.
^Nkfodlpriwixl \ \/
Codcej
^ ng
I -— ^
1 ^7 /— .
U /
v/
k \
\ \
x V
^7
^-V
atraiion
"x^^g/m3
J
Q
(
j
i
!
8S-75-S/;27^Nitrophenol \ \
i 100-02/7 /-Nitrophenol \ \
i H7~fcl— n Rfa£n— nr-n/nnhthnlflta /
i
I
j 27304- B-snSjQ'chkfrdajie / /
| 56-38-2 j ParatnloQ. ^\/ /
i 60S-93-5 | Pentachlorobeqzene/
87-86-5; Pentachlorophenol
FORM 1 - AASV-4
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organks in Air
ANALYSIS DATA SHEET
Lab Name:_
Lab Code:
Con
Lab Sample ID:_
SDG No.:
Date Received:_
Instrument ID:
Date Extracted:
Cleanup Procedure:
Air Sample Volume (STP):_
CASRN
52645-53-1
85-01-8
108-95-2
90-43-7
114-26-1
129-00-0
10453-86-8
299-84-3
95-95-4
88-05-2
27323-18-8
25512-42-9
25323-68-6,
26914-33y6
25429-^-2
26601-64^1
28655-71-2
31472-83-0
53742-07-7
COMPOUND NAWE_
cis/trans-Pennethrin \ N\
Phenanthrene \ \
Phenol \
o-Phenylphenol ^ — ^
Propoxur. / N,
Pyrene / / >^ ^ — \
Resmethrin/ / j ^ — ^
Ronnel / ^ / /
2,4,5-Tncfelgropn«Qo(' /
2,4,6-TrichlorotAenol C^
Monpehterebipjienyls^X^ ^\^
Dichlprebiphejiyl^v ^x^ /
Tritihlorobiphenyh^ \
Tetrachlorobiphenyik \
rentachlorobiphenylSj )
^exachlQrobiphenyls/ /
HeptachlorolMghertyls/
Octachlorobighenyls/
Concentration
' — «—
7 _-
// -
V /
^ \
\ \
\l
KV
Nonachlorobiphe^yls |
1ng/m3
7
-j
Q
i
2051-24-3 j Decachlorobiphenyls
FORM I - AASV-5
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
ANALYSIS DATA SHEET
TENTATIVELY IDENTIFIED COMPOU
PA Sample No.
Lab Name:_
Lab Code:
Lab Sample ID:_
SDG No.:
Date Received:_
Instrument ID:
Date Extracted:
Injection Volume (uL):
Air Sample Volume (STP):_
CASRN
COMPOUND NAME
Concentration
FORM I - AASV-TIC
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Orgaoks in Ambient Air
BLANK SUMMARY
Lab Name:_
Lab Code:_
SAS No.:
Lab Sample ID:
Lab File ID:
Date Analyzed:
Time Analyzed:
THIS BLANK APPLIES TO THgFqfLLOW
I1 ' ' . I.... ..-•• i. .Hi IIM. njf mm^^——> i ••"<
SAMPLES:
EPA Sample No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
70
21
[??"
73
74
25
Laboratory ID^^ / /
Sample
<
/^ ^^
/ /^~^X
/ / /
/
^X
^- ~
/"
/ /^
/ /
C /
^ >NX/ /
"X^
\/
7
Analysis
Date
^\
x,/
/
Time
l
i
i
1
i
Comments:
FORM II - AASV
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organic* in Air
LABORATORY CONTROL SAMPLE ,.
DATA SHEET /EPA Sample No.
Lab Name:
Lab Code:
SAS No.:
Lab Sample ID:
Lab File ID:
Contrac
CaseN?
//
ttfo.: V
{: /\ \^
SDGtfo./ \ "\
Date Analyzed: /\>
Time Analyzed: / /
' InstrumentlB^ ^x^
Column ID:
\y
COMPOUND NAME
Bis-(2-chloroethyl)ether
Benzyl alcohol
Methylphenol
Hexachloroethane
Nitrobenzene
2,4— Dimethylphenol f
Bis(2-chloroethoxy)methane \ ^
2-Methylnaphthalene \
Hexachlorocyclopentadiene
3-Nitroaniline
4-Nitrophenol ^- ^
Diethylphthalatp^ "\
Fluorene / / ^\ [/
Bendiocapo / /
Pentachloro^heXiol / f
Diazi6on ^x^ / /
Fluoranthwie^ ^s/^ /
Folpet \^ ^\
/Endrin ^-v^ ^^^
Bujylbejizytphttwiate^X ^\
/ Ejrarin ketone ^\ \
/ / Dicofol \ \
2,2',3,3'X,4',5j5:,6,6'-Decachlorobi\)hehyl
lrhkno(1^3-cd)pyrene / /
Dibeife^jh)aittb(acene/ /
GbnobntratioiTtag)
S^ik^a
/ /
^ \. ,
\^
\
^
^tl^^
V ^**'^^-^
\ / r
\ \ / /
\ ^ /
\ \
\ \
-^ \;
^s. V
""O?
\
y
Kepbrted
/ /
/ /
^
^\
\ %
\y
— -^
— ^J
%
Recovery
*
Q
j
%Recovery QC Limits:
LCS Recovery:
outside limits out of total.
FORM III - AASV
-------
Lab Name:_
Lab Code:_
SAS No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
GQMS INSTRUMENT PERFORMAN
AND MASS CALIBRATION
Contract N<
Case No.:
Lab Sample ID:
Date Injected:
Instrument ID:
Injection Volume (uL):_
z
ted:
umn ID:/;
•FTPP Injected (ng):_
m/e
51
68
69
70
127
197
198
199
275
365
441
442
443
\^ \
ION ABUNDANCE CRITERIA\^
30-80% of mass 198
Less than 2.0% of mass 69 „
Present / ~~ — —
Less than 2.0% of mass 69 \ X"""--- „
25 -75% of mass 198 \\ /
Less than 1.0% of mass 198 \ \/ /
Base peak, 100% relative abundance \ /
5-9% of mass 198 x -\ \ \
10- 30% of masses , — ^ \ \ N
Greater than 0.^%/f mass\98l^-^\ \
Present, but lew than mass 4^3 ^ — ^ — -,
40-110%o/ma^sl98 / / ^^V
15-24% of^jass"^^ / /
^j% Relative Abundance
to4^l98
"X^ \^
\^
\s
•
— 7
/ --/
\
/
to specified mass
>
THIS
TUNEsAPMES
TO THE FOLLOWING:
1
/*
3
^
6
7
8
9
EP£'8SmpTe~NO>\
/
/ / X
//
L
\^ ^\
\. \
"x^
Lab^tmple IE?
\ ^\
^ \
\ \
) )
/ 1
/ /
/ /
/
•J
M^bFilelD
./
Date Analyzed
Time Analyzed
!
1
1
FORM IV - AASV
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatilc Organic* in Air
INITIAL CALIBRATION DATA SHEET
Lab Name:_
Lab Code:_
SAS No.:
GC Column ID:
Injection Volume (uL):_
/v.
STANDARD
EPA Sample No.
LAB FILE ID
MASS INJECTED (ng)
DATE INJECTED
TIME INJECTED
COMPOUND NAME
Acenaphthene
Acenaphthylene
Acetophenone
Aldicarb
Aldrin
Aniline
Anthracene
Bendiocarb
Benzidine
Benzfalanthracene
Benzo[a]pyrene
Benzofb|fluoranthene
Benzo[e]pyrene
Benzofg,h,ilperylene
Benzo[k]fluoranthene
Benzyl alcohol
alpha- BHC
gamma -BHC (Lindane)""
p— Biphenylamine/ ^_
Bis(n-butyl)phtbalater^
Butylbenzylphtjialaie'
Captan / /
alpha - Chla£dane\^
gamma— Chlorchme ^x
4-Chloro-3-methylpheqpl
4— Chloroaniline
Bis(2-chloroethoxy)methane
Bis(2-chloroethy|)ether
CAL1
CAL2
CAL3 ,
/
/
/ /
/ /
/ L
' (2AL4
/
/
^ /
/
/ /
CAL5
1
/
Relative Response Factor fRRF)
CAL1
/"
/ /
/ /
/ /
/ /
k \
X^^ ^
"X
^
X
^\
N
"\ /
\ ^V
^v. /
\/
CAL2
^, ^
/
\ T
\
'
^X
^^ ^
) V
I ^
/ /
/ /
^ /
. \
^x^^ \
^ "X^
\
V \
A \
) )
/ /
/
/
f
Chlorothalonil
CA1>2L
X
— —^ -
\ • _
\ /
\ \ /
\ V /
\ <,
\
^X
-^ "—
X^y
,
^
/
^GAI/4
k \l
^^
X
-— ^^
— -.
/ -^
/
\
N
\/
r
|
CAL5
X^
, 7
"x/
~~!
/
\y
mean
RRF
.
%RSD
I
_[ .. ..
FORMV-AASV-1
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Orgaoics in Air
INITIAL CALIBRATION DATA SHEET
Lab Name:_
Lab Code:_
SAS No.:
GC Column ID:
Injection Volume (uL):_
^COMPOUND NAME
Chlorpyrifos
Chrysene
Dacthal (DCPA)
4,4'-DDD
4,4'-DDE
4,4'-DDT
Diazinon
Dibenzfa.hjanthracene
Dichlorvos (DDVP)
Dicofol
Dieldrin
Diethylphthalate
2,4- Dimethylphenol
Relative Response F>ctpf (RRF)
CAL1
CAL2
\ '
\
! Dimethylphthalate /"
4.6-Dinitro-2-methylphenol / s~~
i - 1 ! ,
2,4— Dinitrophenol ' / /
i2,4— Dinitrotoluene i / /
i Endosulfan I / /
Endosultan II >C ^X.
i Endrin ^X^
i Endrin aldehyde j ^x
~~x,
X \
CAL?
/ /
/ /
/ V
X^
^
^— -—
\ — ~~-~-^
\ ;
\ \ /
\ ^
\ <
\ i
\
A Upx '
) L. ^j
/ /
^/ /
X^
Endrin ketone ^-— 1 -^
Bis(2-ethylhexyhphthalatej "X>
X ^
x^
X^ /
^
7
Fluoranthene / /" ^\ X ^
Fluorene / / X
Folpet / / i
Heptachlor / X^
; Heptachlor epb^UJe ^\
i HexachlorobenzeneX^ X^ >
' Hexachlorocyclopentadie^ttx. "X,/
s.
j
V
1
Hexachloroethane i ^X /
\
\
/
/
/
/CAL4 r
' /
/
/ /
X/ /
\ x^
"X^
X
««« —
^-~~- — .
r- —
/
/
\
\
\/
p
. CAL5
7
/
x^
*>«. /
x/
—-,
/
mean^
RRF
%RSD
i
1 i
1
:
I !
!
1
|
-
i • '
i - -
I
Indcno(l,2.3-c.d)pyrene
X/i
Isophorone _
Methoxychlor
FORM V - AASV-2
-------
Lab Name:_
Lab Code:_
SAS No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatilc Organics in Air
INITIAL CALIBRATION DATA SHEET
Contract ]
Case No/ _T_
GC Column ID:
Injection Volume (uL):_
SDGNb.: ^
Insti/me/t IDs.
Relative Response FajtftorARRF)
mean /: !
RRF !%RSDJ
COMPOUND NAME
Hexachlorocyclopentadiene
Hexachloroethane
! Indeno(l,2,3-c,d)pyrene
'• Isophorone
i Methoxvchlor
2- Methylnaphthalene
2-MethylphenoI
4—Methylphenol
i Naphthalene
2—Naphthylamine
2-Nitroanihne
3-Nitroamline
Nitrobenzene
4—Nitrodiphcnyl
2-Nitrophcnol
4-Nitrophenol _
Bis(n-octyl)phthalate
Oxychlordane
Parathion
Pentachlorobenzene
Pentachlorophenoi
cis/trans—Permethrin
Phenanthrene_
Phenol
o—Phcnylphen
Propoxur
Pyrcne
_Rcsmethrin
1 Ronnel
2.4:5—Trie hlorop hcno[
2,4.6-Trichlorophcnol
FORM V - AASV-3
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Scmivolatite Orgaaics in Air
INITIAL CALIBRATION DATA SHEET
Lab Name:_
Lab Code:_
SAS No.:
GC Column ID:
Injection Volume (uL):_
1 COMPOUND
NAME
CAL
1
Relative
1 CAL 2
Response F/actql (RRF)
i CAL?' 1/CAL4 A
CAL
5
mean^
RRF
i%RSE
PCBs
Monochk, obiphenyls
Dichlorobiphenyls
/
' Trichlorobiphenyls
* Tetrachlorobiphenyls
' Pentachlorobiphenyls
Hexachlorobiphenyls
Heptachlorobiphenyls
Octachlorobiphenyls
Nonachlorobiphenyls
Decachlorobiphenyls
SURROGATES
Nitrobenzene— d,
/ : ~ — ~H
\ ^\-~-— ___
\i\ )
K \ /
\ V
\ 1
^~^\ \
^
•**. — m
-—I
" /— ^
/
/
N
^ 7
— -^_
J
2—Fluorobiphenyl
; p—Terphenyl—
LJ.\ i
; 2.4.6-Tribromophenol
i Benzo(a)pyrene—d,-,
THIS JNmAJL^ALIBka^riO>hAPPLIES TO THE FOLLOWING:
_
EPA Sample N<£ ! __ Lab^atppie
i^ J Date Analyzed __ Time Analysed
FORMV-AASV-4
-------
Lab Name:_
Lab Code:_
SDG No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
CONTINUING CALIBRATION DATA SHEE
Contract No.:
Case No.: /
EPA Sample No.:_
GC Column ID:_
Date injected:
Injection volume (uL):_
COMPOUND NAME
Acenaphthene
Acenaphthylene
Acetophenone
Aldicarb
Aldrin
Aniline
Anthracene
Bendiocarb
Benzidine
Benz[a]anthracene
Benzofalpyrene
Benzofblfluoranthene
1 — i ..
Benzofe]pyrene
Benzofg,h,ilperylene /
Benzo[k]fluoranthene /
Benzyl alcohol <^
alpha -BHC ^
— i
gamma -BHC (Lindane)
p- Biphenylamine/-'" ~
Bis(n- butyl)ph-
^ X ^\/
\ \
\ \
/ /
/ /
\y /
\ /
GAL/3 RRF /
/ / /
<^ ^\ / /
"X^ ^ ^
\
r — ^~
-^ ^--
K 7 /—• - ~
\ / /
\ ^ /
\ \
\ \
^ \ ;
V. V
^N. /
^
p
i
/ %D
/
X
•^ /
"~^»
J
\
\
1
1
1
FORM VI - AASV-1
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
CONTINUING CALIBRATION DATA SHEET/
Lab Name:_
Lab Code:_
SDG No.:
EPA Sample No.:_
GC Column ID:_
Date injected:
Contract No/
Case
SAS No.
Lab Fil
Instrument ID:
Time infected:
Injection volume (uL):_
I
i COMPOUND NAME
'•• Chlorothalonil
Chlorpyrifos
Chrysene
Dacthal (DCPA)
4,4' -ODD
4,4' -DDE
1 4,4' -DDT
Diazinon
Dibenz[a,h]anthracene
Dichlorvos (DDVP)
Dicotol
Dieldrin ,
Diethylphthalate /
2,4-Dimethylphenol /
Dimethylphthalate / *
4.6-Dinitro-2-methylphehoJ
2,4— Dinitrophenol
2,4— Dinitrotoluepe
Endosultan I / ^——^
Endosultan Jl /
Endrin / /
Endrin a,raeh#de
Endrin KetQne^\
Bis{2-ethylhexyHrjhthatete
Fluoranthene ^\
1 Fluorene ^\
Folpet
1C mean RRF
!
r— t
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
CONTINUING CALIBRATION DATA SHEETx
Lab Name:
Lab Code:
SDG No.:
EPA Sample No.:
GC Column ID:
Date injected:
Injection volume (uL):
! COMPOUND NAME
i Heptachlor epoxide
• Hexachlorobenzene
! Hexachlorocyclopentadiene
Hexachloroethane
L Indeno( 1,2,3— c,d)pyrene
i Isophorone
! Methoxychlor
Hexachlorocyclopentadiene
Hexachloroethane
j Indeno(l,2,3-c,d)pyrene
Isophorone
Methoxychlor
; 2-Methylnaphthalene
j2-Methylphenol /
4-Methylphenol /
Mirex ^
Naphthalene ^-
1 2— Naphthylamine
2-Nitroaniline /•-" ~~~
3-Nitroanilin?' /
Nitrobenzen/e /
4— Nitrodirihenyl
2-Nitro0hen&L
4-Nitroprfeqpl ^\
1 Bis(n— octyOpnthajate^Xj
| Oxychlordane ^\
JJParathion ;
: Pentachlorobenzene •
1C mean RRF
1 '-.
V v~
\ N
\
-
^ ^
s \
/ S ^\ }^
7 ; J
/ / s •
x^ / /
\ /
^\ ^\ \
^ "\ "\/
.\ \ ,
\\ 1
\ I
/ 1
/ /
\y /
\ /
"v/
1
Contract No.: /
Case No.: /
SASNo.: / /•
Lab File JD: /
Instrument/ID:
Time>mjected:
Da^/of/C.:
/ / /
^AI/3 RRF/
/ / /
<^ \^ / /
^\ ^ /
^\ ^
^\
-^
L^ ^—
v 7 , — ^
V V /
\ /
\ \
\ \
. \ ;
V /
/
<^
^ \^
\^ ^x^
"x^ \
"x^
x^
/ %D
/
\
\,
\/
~~-^
J
s^
J
•J
FORM VI- AASV-3
-------
Lab Name:_
Lab Code:_
SDG No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatite Organks in Air
CONTINUING CALIBRATION DATA SHE
Contract No.
Case No.:
SASNo.:/ /
EPA Sample No.:_
GC Column ID:_
Date injected:
LabFileOD/
Instnufieht ID:
Tim/iniected:
Injection volume (uL):
COMPOUND NAME
Pentachlorophenol
cis/trans- Permethrin
Phenanthrene
, o-Phenylphenol
Phenol
Propoxur
Pyrene
Resmethrin
Ronnel
2,4,5 - Trichlorophenol
2,4,6-Trichlorophenol
Monochlorobiphenyls
Dichlorobiphenyls /
Trichlorobiphenyls /
Tetrachlorobiphenyls / ^
Pentachlorobiphenyls ^\
Hexachlorobiphenyls
Heptachlorobiphenyls — -^
Octachlorobiphenyls.
Nonachlorohjphenyls
Decachlorooip^enyls
Nitrobenzene/- ds
2-Fluor^bjpheJnl
p-Terphenyt^dj,, ^X^
Phenol -d,; "^x^ ^
2 — Fluorophenol ^x
2,4,6— Tribromophenol
1 Anthrarpnp— ri. .
1C mean RRF
/ — -
< ^
\ \
\
\
/^ ^\
/ / — x \
/ )
/ / / — "
^ / /
\y /
"x^
x^ \j
x ""7
"^-^
r
/ %D
\^
X^ /
7
-*/
i
1
i
iUl-
Benzo(a)pyrene-d,o
FORM VI - AASV-4
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
CONTINUING CALIBRATION DATA SHEETS
LabNz
LabCc
SDG^
EPAS
GCCo
Date ii
Injectii
ime: Contract No.: / /
)de: Case No.: / X.
Io.: SASNo.: / ,x ^x
ample No.: Lab File /ID: / ^\ ^vx
lumn ID: Instrurngst/ID: ^X^ ^\
ijected: Time/injected: ^\ /
an volume (uL): Dafe ofl.C:
THIS CONTINUING CALIBRATION APP/IES TO THE FOLLOWING:
EPA Sample No.
/
/
/ /
X^
^
/^ ^~
/ s — ^
/ /
/ /
£ x^
"\ \^
\^ ^\
^\
Lab Sample ID
\ V
\ N
\
^ — -^
/ \
f / \\s~
/ 1 ^
K / /
^"X, / / •
X ^ /
"X^ X^
"x^ "X^ x.
X X "X/
X \
\ \
/ /
/ /
x/ /
\y
/Dat^ Analyzed/
^X ^X/ /
x^ <^
"X^ "X
x.
— — -^
•— ^ ^^
v / 7^—
\/ /
\ " /
\ \
\ \
x \/
x^^
x^^y
Time Analyzed
\
X
x/
"~7
y
FORM VI- AASV-5
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organks in Ambient Air
INTERNAL STANDARD AREA AND RT SUM
Lab Name:_
Lab Code:_
SAS No.:
Contract
Case Njo.:
SDG
! Dichlorobcnzene-d4 j Naphthalene-d^ 7| Accnaphthcne-din
[Area # !RT #[A/ea/ #|RT /# Area ^ RT #\
RT: Upper Limit: +0.33 minutes of internal standard RT.
Lower Limit: -0.33 minutes of internal standard RT.
All values outside of the QC limits must be fofibwfed by an "*" under the "#" column.
FORM VII-AASV-1
-------
Lab Name:
Lab Code:_
SAS No.:
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semhrolatile Organks in Ambient Air
INTERNAL STANDARD AREA AND RT SUM
Contract
Case No.
SDG
Ctrysene-d19
Phenanthrene- d10
Area
# |RT #
/#
RT/
Perylene—
Area # RT #
12-HOUR STANDARD
Upper Limit
Lower Limit
EPA Sample No.
l!
\ \
\
\
V /
\ I
8_
9
1«[
111
r~
12
13
14
15
16 C
17 i
is;
19
201
\ \
X
\
AREA: Upper Limit: +3&&of ime«jal standard area.,
Lower Limit: -40%orsQternal>t^ndar(rare
RT: Upper Limit: +033 minutes of internal standard RT.
Lower Limit -0.33 minutes of internal standard RT.
All values outside of the QC limits must hel
'by an "*" under the "#" column.
FORM VII - AASV-2
-------
Lab Name:_
Lab Code:
Lab Sample ID:_
SDG No.:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
FILTER/ADSORBENT CARTRIDGE
CERTIFICATION DATA SHEET
Contract No.:
Case No.: /
Lab File
SASNo
Date Extracted:
Instrument ID:
Filter Batch No.:_
Injection Volume:_
CASRN
83-32-9
208-96-8
98-86-2
116-06-3
309-00-2
62-53-3
120-12-7
22781-23-3
92-87-5
56-55-3
50-32-8
205-99-2
192-97-2
! 191-24-2
207-08-9
100-51^"
319-7&-6>
5^-89/9
/92-^7-l
/ 84^34-2
^5^68^
133-06^
5103-71-9
5103-74-2
59-50-7
\ ^V
COMPOUND NAME\
Acenaphthene ^x^
Acenaphthylene
Acetophenone / "~~-~-^^
Aldicarb \ \ — _ ^
Aldrin \ \ / / '
Aniline \ \ / /
Anthracene \ /
Bendiocarlj. ^ \ \
Benzidine/ ^ ^ \ \ \
BenzfaJantKraceneN, [^ — \ \ /
Ben^fal^rene / ^_ ^-^
Bej-izotb'lfluorantHene/' "\^ /
B&jzofetowens/ /
BenrofeA,ilpefyl^e
Benzofklflubfantherte^
Ben^TatBohol "X^ "\
•SIpRa^BUCX ""X/
gamma- BHC (Dmdane)
p— Biphenylamine\
Bisfn-butyOpHthajate
^Bjutylbenzylph/haiyte
Ca>an / /
alpha — Chrord^ne
gamna^Chjo'rdane
4-Chloro-3-methylphenol
106-47-8 j4-Chloroaniline
/ Concentration
\ ug/assembly
Xx^
\^ >
X/
-7
/
J
\
\
\
\
FORM VIII-AASV-]
-------
Lab Name:
Lab Code:
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Air
FILTER/ADSORBENT CARTRIDGE
CERTIFICATION DATA SHEET
Contract No.:_
Case No.: /
Lab Sample ID:
SDG No.:
Date Extracted:
Instrument ID:
Filter Batch No.._
Injection Volume:_
Lab File ID
SAS No.: /
Date
GC Cefluroh ID:
PU:
No.:
Batch No.:?
CASRN
111-91-1
111-44-4
1897-45-6
2921-88-2
218-01-9
1861-32-1
72-54-8
72-55-9
50-29-3
333-41-5
53-70-3
62-73-7
115-32-2
60-57-1
84-66-2
105-67-9
131-ll^f
534-^i-r
51/28/5
124-J4-2
4$9-'$8^8
33213^65-9"
72-20^8-
7421-93-4
533-41-5
COMPOUND NAME \V
Bis(2-chloroethoxy)methane ^\
Bis(2-chloroethyl)ether - ^X
Chlorothalonil , — _
Chlorpyrifos / "" ~~-^_
Chrysene \ \~^"~~~— --,
DacthaHDCPA) \ \ / / ^~~
4,4'-DDD \ \/ / •
4,4' -DDE \ /
4,4'-DDT/^ \ \ \
Diazinoi/ /- — -^ \ \ \
Diben4a,bfanthracfeneK ~-\ \/
Dicl/orv/s (DDVPA ,^-^ "^-7
Di/ofo^ / / \V
Difektrin^^ / /
Diethyl^htjialate ^
2,4^iPimethylplienol\
Dimethylt)hthalate\^ "">
^-Binkro^vmethyi^enol
2,4-Dinitroftienbl •
2,4-DinitrotoKien^
Endosulfan I J )
"Eijdosulfan II/ /
sEndrilK^ / /
En&rin aldehy/ae
EndrinketQjre
/ Concentration
/ ug/assembly
\
"\
\. ^
^^/
^7
*-**—-/ 1
117-81-7 | Bis(2-ethylhexyl)phthalate
FORM VIII - AASV-2
-------
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semtvolatile Organks in Air
FIUTCR/ADSORBENT CARTRIDGE
CERTIFICATION DATA SHEET
Lab Name:_
Lab Code:
Lab Sample ID:
SDG No.:
Date Extracted:
Instrument ID:
Filter Batch No.:_
Injection Volume:_
CASRN
COMPOUND
NAMEtX
/ Concentration
ug/assembly
i 206-44-0 I Fluoranthene
86-73-7 | Fluorene
133-07-3 I Folpet
76-44-8 i Heptachlor
\ V
1024-57-3 | Heptachlor epoxide \ \ /
118-74-1
Hexachlorobenzene
\\/ /
77-47-4
Hexachlorocyclopentadiene\ " /
67-72—1 Hexachloroethane^
\ \
193-39-5
78-59-1 jlsophofon/
\\
72-43-5 i Met|*oxyefnlor
\/
x/
91-57-6 2-xMejfaylnaphth/len/
7
95-48-7
106-44-5 |4-MetBjdphenol/
2385-85-5 Mirex
91-20r^1NaphtBa1cne
88/74/4
2-Nitroaniiine\
3-Nitroanilim
--3! Nitrobenzene
rNitrodiphenyl
100-02-7
117-84-0 | Bis(n^bctyl)phthalate
273Q.4.- 13-8jOxychlordane
56-38-2 IParathion
FORM VIII - AASV-3
-------
Lab Name:_
Lab Code:
Lab Sample ID:_
SDG No.:
Date Extracted:
Instrument ID:
Filter Batch No.:_
Injection Volume:_
ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semhrolatile Organics in Air
FILTER/ADSORBENT CARTRIDGE
CERTIFICATION DATA SHEET
Contract No.:
Case No.:
Lab File
SASNo
Date
GCCohrafolD:
PUFWch No.:
CASRN
COMPOUND
NAME. ^^
/ Concentration
ug/assembly
608-93-5 Pentachlorobenzene
87-86-5 Pentachlorophenol
52645—53—1 cis/trans—
85-01-8
Phenanthrene
108-95-2
Phenol
\ \
90-43-7 o-Phenylphenol
114-26-1 jPropoxur
\
129-00-0 iPyrene
\ <
10453-86-8 j Resmethckf
299-84-3|Ronnel/ '/"~-x \
95-95-4 j 2,4,5ylTri^nlorophe>ior
\_\
-06-2 12,4,6^-T^chloroph^noj
/ /
/PCBs
27323-18-8
MonochibfQbipheB^ls
25512-42-*
>iphehyl§
25323-68^6
/
L_ 26914-33-^ TetrachlbTQbiphenyls
25429/29/2
PentachloropipheVl;
\ \
1-04-9 Hexachlorobipi
"~
-7P^|Heptachlorobi0hei](yls
31472-8S^O
2051-24-3, Dec^ehjorobifftienyls
FORM VIII - AASV-4
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organks in Ambient Air
SURROGATE RECOVERY
Lab Name:
Lab Code:
SAS No.:
^Recovery QC Limits: 25-150%
Values outside of QC limits are flagged with a "*" under the "#" column
FORMIX-AASV-1
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Ambient Air
SURROGATE RECOVERY
Lab Name:_
Lab Code:_
SAS No.:
Contra
EPA Sample No.
Surrogate Percent Recjtfve
Anthra—
cene-d
Benzo(a)-
pyrene— d2
Tribromo— /
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Semivolatile Organics in Ambient Air
ANALYTICAL SEQUENCE
Lab Name:_
Lab Code:_
SAS'No.: ~
Instrument ID:
THE FOLLOWING IS THE ANALYTICAL SEQUENCE
1
2
3'
4
5
6
7
ARRANGED
IN CHRONOLOGI
ICMXyiDER:
i EPA Sample No.
•
i
Lab Sample ID /
/
Analysis Time
/ / ?
/ / / /
<^ ^
"\ / /
Analysis Date
9!
\\
\ \ //
FORM X - AASV
-------
January, 1992
-------
Exhibit C
Semivolatile Organics Analysis of Ambient Air
EXHIBIT C
SEMIVOLATILES IN AMBIENT AIR
TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMITS
I. PAHs, PESTICIDES, AND OTHER SEMIVOLATILES
Target Compound
Ac enaphthene
Acenaphthylene
Ace tophenone
Aldicarb
Aldrin
Aniline
Anthracene
Bendiocarb
Benzidine
Benzo(a)anthracene
Benzo(a)Pyrene
Benzo(b)fluoranthene
Benzo ( e) pyr.ene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
Benzyl alcohol
alpha-BHC
gamma-BHC (Lindane)
p-Biphenylamine
Bis(n-butyl)phthalate
Butylbenzylphthalate
Captan
alpha-Chlordane
gamma -Chlordane
4-Chloro-3-methylphenol
4-Chloroaniline
Bis(2-chloroet!
Bis(2-chloroe
Chlorothalo
Chlorpyrifi
Chrysene
Dacthal
4,4'-DDD
4,4'-DDE
4,4'-DDT
83-32-9
208-96-8
98-86-2
116-06-3
309-00-2
62-53-3
120-12-7
22781^21^3
/ On/column
ct ion. ne
111-4
97-45-6
1-88-2
8-01-9
1-32-1
2-54-8
72-55-9
50-29-3
ne/m3
37
37
37
146
146
73
37
83
73
37
37
37
37
37
37
37
146
146
183
37
37
183
146
146
183
73
183
37
183
183
37
183
146
146
146
January, 1992
Page C-l
-------
Exhibit C
Semivolatile Organics Analysis of Ambient Air
TABLE 3
SEMIVOLATILES IN AMBIENT AIR
TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMIT!
(continued)
I.
PAHs, PESTICIDES, AND OTHER SEMIVOLATILES (continued)
/ / CRQL
Target Compound
Diazinon
Dibenzo(a,h)anthracene
Dichlorvos (DDVP)
Dicofol
Dieldrin
Diethyl Phthalate
2,4-Dimethyl phenol
Dime thylphthalate
4,6-Dinitro-2-methylphenol
2,4-Dinitrophenol
2,4-Dinitrotoluene
Endosulfan I
Endosulfan II
Endrin
Endrin Aldehyde
Endrin ketone
B i s(2 -e thyIhexy1)phthal/te ^
Fluoranthene
Fluorene
Folpet
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
HexachlorocyclopewLacTLeiK
Hexachloroethajp
Indeno(l,2,3-/
Isophorone
Methoxychlc
2-Methyln^pht
2-Methyl^henol
4-Methylphteuol
Mirex
Naphthalene
2 -Naphthylamine
CAS RN
333-41-5
53-70-3
62-73-7
115-32-2
60-57-1
84
51-2
121-14-
959-98-8
33213-65-9
Page C-2
January, 1992
-------
Exhibit C
Semivolatile Organics Analysis of Ambient Air
SEMIVOLATILES IN AMBIENT AIR
TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMITS
(continued)
I. PAHs, PESTICIDES, AND OTHER SEMIVOLATILES (conti
Target Compound
2-Nitroaniline
3-Nitroaniline
Nitrobenzene
4-Nitrodiphenyl
2-Nitrophenol
4-Nitrophenol
Bis(n-octyl)phthalate
Oxychlordane
Parathion
Pentachlorobenzene
Pentachlorophenol
cis/trans-Permethrin
Phenanthrene
Phenol
o-Phenylphenol
Propoxur
Pyrene
Resmethrin
Ronnel
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
CAS RN
88-74-4
100-01-6
98-95-3
92-93-3
88-75-5
100-02-7
117-84-0
27304-13-8
t->oltunn
Injection, ne
ne/m3
January, 1992
Page C-3
-------
Exhibit C
Semivolatile Organics Analysis of Ambient Air
SEMIVOIATILES IN AMBIENT AIR
TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMITS
(continued)
II. FCBs (Congeners)
Target Compound
Monochlorobiphenyls
Dichlorobiphenyls
Trichlorobiphenyls
Tetrachlorobiphenyls
Pentachlorobiphenyls
Hexachlorobiphenyls
Heptachlorobiphenyls
Octachlorobiphenyls
Nonachlorobiphenyls
Decachlorobiphenyl
CAS RN
27323-18-8
25512-42-9
25323-68-6
26914-33-0
25429-29-2
26601-64-9
28655-71-2
31472
5374
205W
January, 1992^
Page C-4
-------
ANALYTICAi:
DETERMINATION OF
COLLECTED ON PUF,
GAS CHROMATOGRAPHY AND
BY
;TRY (GC/MS)
January, 1992
-------
EXHIBIT D
ANALYTICAL METHOD FOR THE
DETERMINATION OF SEMIVOLATILE ORGANICS
COLLECTED ON PUF/XAD-2 AND ANALYZED
GAS CHROMATOGRAPHY AND MASS SPECTROMETRY eR FIElA SAMPLING
SECTION 5 GO/FIEf OR GC/EC
January, 1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
SECTION 6 GC/MS ANALYSIS
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.8
6.9
.10
.11
.12
.13
.14
.15
6.16
SUMMARY OF METHOD
INTERFERENCES
APPARATUS AND MATERIALS
REAGENTS
STANDARDS
INSTRUMENT OPERATING CO*
ANALYTICAL SEQUENCE
INSTRUMENT PERFORMANCE CHECK
INITIAL CALIBRATION
CONTINUING CALIBRATION
BLANK ANALYSIS
LABORATORY CONTRC
SAMPLE ANALYSIS
PERFORMANCE EVALUATl
QUALITATIVE ANALYSIS
QUANTITATIVE ANALYSIS
SECTION 7 BIBLIOGRAPHY . . .
57
January, 1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
EXHIBIT D
ANALYTICAL METHOD FOR THE
DETERMINATION OF SEMIVOLATILE ORGAN!
COLLECTED ON PUF/XAD-2 AND ANALYZE
GAS CHROMATOGRAPHY AND MASS SPECTROME1
1 INTRODUCTION
1.1 SCOPE AND APPLICATION
1.1.1 Polynuclear aromatic hydrocarbons (fPAHk), pest
polychlorinated biphenyls (PCBs), and ottier/semivola/til^ compounds (SVOCs)
have received increased attention in re/entr years im a/r pollution studies
because some of these compounds are highly carcinOgeivicior mutageni'c. In
particular, benzo[a]pyrene (B[a]P), 4,45N[}Dp, $>«'-pDT, ,and PCBs have all
been identified as being highly carcinogenic
1.1.2 The analytical method that follows is designed to"~a*ialyze samples
containing the compounds listed eo^the Target Compouno^ist/in Exhibit C.
1.1.3 The analysis technique r
Methods 610 and 625, Methods for
and Industrial Wastewater; Methods\80
Evaluation of Solid Waste (SW-846) ;
Statement of Work for Low Concentrati
EPA Method 680, Determination of Pestic?
Soil/Sediment by Gas ChixJt5atS^vand
response/of/each compoui
standa
each
store,
mpou
cartr,
trati
£^samplfiag)/are added to each PUF/XAD-
dditWnal surrogate compounds
eceived from the field just
od blank (LMB), laboratory
nee evaluation (PE) samples, all of the
piked onto the cartridges just prior to
dges are not sent to the field. Internal
and sample extract before GC/MS
.ement is based on an integrated ion
Analytes are identified as
concenfrEAtion is calculated by relating the MS
to\the MS response of the corresponding internal
^es the internal standard assignments for
und.
stm (DS) to control data acquisition and to
la/te mass spectral data is essential.
January, 1992
Page D-l
-------
Exhibit D
Seraivolatile Organics Analysis of Ambient Air
meas
1.1.6 Applicability of the Method to PCBs
1.1.6.1 This method is applicable to samples
single congeners. PCBs are identified and
(i.e., by level of chlorination) by GC/MS usi
1.1.6.2 The existence of 209 possible PCB
of the Chemical Abstracts Service RegistryJ
potential method analyte impractical.
foi
CO
ling PCBs as
isomer groups
software.
iecav.
1.1.6.3 A concentration is measured
total PCB concentration for each samp
isomer group concentrations. Nine
calibration standards and one inter
to calibrate MS response to PCBs.
measured as isomer groups, the non
chlorination is used to describe method
1.1.7 Detection Limits
Detection limits vary
matrix, sample preparation
type of data acquisition, s
analyses of calibration solutions u^ing
of approximately six months, the>
assist the analyst:
isting
PCB isomer group, and
^tract isrohtained by summing
ec/ed PCB /ongfeners are used as
1 .standard/ chrysene - d12, is used
PCB/ aife identified and
ificXAS JttJ for each level of
and with sample
conditloTr-wf^the GC/MS system,
ised on numerous
>ne/instrument over a period
Lng/comments are provided to
1.1.7.1 Pesticiiae*""anlriytes other\thahendosulfans I and II can be
identified and/accurately\ measured yhen\the injected aliquot
contains 2 ngyofy^acn^na^^te^.^ The endo^ulfans require about 4 ng
each.
1.1.7.2 ^petadtion lit
with increasing numb«
for decachiorobibb^yl
of a raonochlots^biphenj
and accurately me^asurec
1 ng and fuU>scan
ts/for ifrd^vicKaal PCB congeners increase
chlorine atoms, with the detection limit
ieing about 5 to 10 times higher than that
A monochlorobiphenyl can be identified
ten the injected extract aliquot contains
acquisition is used.
fmra
tecbjx)n limits/for total PCBs will depend on the
r of indivbsLualNfCB congeners present.
1.1.8
toxicity of carcinogenicity of each reagent used in this
methoJKhas nbtbeen precisely defined; however, each chemical compound
should b^xreate^d^as &. potential health hazard. From this viewpoint,
exposure to these chemicals must be reduced to the lowest possible
level by whateve^txmeans available. The laboratory is responsible for
January.1992
Page D-2
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
maintaining a current awareness file of Occupational
Administration (OSHA) regulations regarding the sal
chemicals specified in this method. A reference fil«
safety data sheets (MSDSs) should also be made aval:
personnel involved in the chemical analysis. A/adit?
laboratory safety are available and have been
analyst.
fety and Health
indling of the
of material
ible to all
lal references to
r the
1.1.8.2 Care must be exercised when workin|Kw/ith these
This method does not purport to address a/l^f the safety protv
associated with its use. It is the responsibility of whoever
this method to consult and establish appropriate safety and health
practices, and determine the applicability of regvilatory limitations
prior to use. The user should be thoroughly fam/liar with the
chemical and physical properties of /targeted sujftstances.
1.1.8.3 Treat all analytes as carcinogens .\/fiea/ compounds should be
weighed in a glove box. Spent samples ahdunusad standards are toxic
wastes and should be disposed according to regulations. Regularly
check counter tops and equipment with "black fifch£" fois^fluorescence
as an indicator of seraivolatirle^contamination.
1.1.8.4 Precautions must be
extreme fire hazard and the p*
producing an explosive mixture
evaporate to dryness. It is thev
personnel on the proper use and
safety practices for handling ethers
diethyl
because of its
may form
d th^ £y6lutiorTT)e allowed to
's duty to instruct all its
this solvent. Standard
be implemented.
1.2 SUMMARY OF METHOD
1.2.1 Prior to fiel/6 u/e. the
2/PUF) are cleaned/In .solvents
spiked i^ith a miniraun/of threer s
adsorbent cartridge ate stor«
foil prior to insrallati
it cartridge (PUF/XAD-
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
standards are added to the concentrate. (If applicabl
extract is screened for levels of semivolatiles utili
flame ionization detector (FID) or an electron capt
1.2.4 For final identification and quantificatio
injected onto a GC with <•; -apillary column and t
separate the compounds, v. _ch are then detected
(MS) in the full scan data acquisition mode.
NOTE: This method is based upon full scan
concentrations are based upon the use of 1
volumes are used, the concentrations must
concentrated
a GC with a
itector (ECD).)
he extract is
ed to
ta/acquisition. All
:L Injections. If different
>e >appropriyate'iy adjusted.
1.2.5 Target compounds are identified fn rfie samples fly analyzing
standards under the same analytical condition* us«a as the samples and
comparing resultant mass spectra and GC rte^entibn times. A relative
response factor is established for each targVt compound during the initial
and continuing calibrations by comparing the MSTsesponVa for the primary
ion produced by the compound to the MS response for^^e primary ion
produced by an internal standard./—E^ch identified target compound in a
sample is quantified by comparing there^pwtses^for the target compound
and the internal standard, whiley tdlttrng-jjjtro accounE~~~ct*e-7relative response
factor from the most recent calibration, the^Lnyeia^jmd/final sample
volume, and any sample dilutions.
1.2.6 Non-target compounds are identi^iec
spectra from the non-target compounds
National Institute of SfcdndarStSvand T£
Library. Non-target compoimds ar^ quantifi
for the non-target
nearest internal sty
1.3 INTERFERENCES
MS
sponse
comparing the resultant mass
spectra contained in the
(NIST) Mass Spectral
•^ comparing the MS response
•>nse produced by the
1 is assumed.
ETATIONS
1.3.1 ContaminantSs.in sbty&ntsf, reagents, glassware and other sample
processing hardware m&jLcauseAnethod interferences such as discrete
artifacts and/or elevatetNbasertxtes in the total ion current profiles
(TICPs). LaberaCBry^methodTbJ.anks^are analyzed with each analytical
sequence tt/demonstrate^Shat the^se materials are free of interferences
under the/ana^ticaT^^ondrfcipns usett/for samples. Matrix interferences
may be caused by contamrnanta. that are coextracted from the sample. The
extent/of/atrix interfere\ces\ will vary considerably from source to
source
1.3.2
cleaned. ^As sooJKas possj
solvent used/XJhen^vashy
water followed
at 450°C for a few
s, glassware should be meticulously
after use, rinse glassware with the last
it/h detergent in hot water and rinse with tap
water. Drain dry and heat in a muffle furnace
olumetric glassware should not be heated in a
Page D-4
January.
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
muffle furnace). After cooling, store glassware invert
aluminum foil. Before using, rinse each piece with an
solvent.
NOTE: Some thermally stable materials such as PCBs
by this treatment. Solvent rinses with acetone anj
hexane may be substituted for the muffle furnace.
pr covered with
jot be eliminated
:-quality
1.3.3 For both pesticides and PCBs, interferenc
presence of much greater quantities of other Sample components
overload the capillary column; additional sainple/extract preparation
procedures must then be used to eliminate iiiteiXferences. Capillary column
GC retention times and the compound-speci£tc cmaracterfis-tics of mass
spectra eliminate many interferences that/fo/merly were /of concern with
pesticide/PCB determinations by electron/capture de/ect/ion. The approach
and identification criteria used in th^ method for PGBs eliminate
interference by most chlorinated compoumlspthelfvythail PCBs. With the
isomer group approach, coeluting PCBs that cotitain the same number of
chlorines are identified and measured together^xjhereikjre, coeluting PCBs
are a problem only if they contain a different numbso: of chJLorine atoms.
1.4 DEFINITIONS
NOTE: Definitions used in this \ioctment a
standard operating procedures (SOPsO should
Methods D1356, D1605-60, E260, and E\55.
are defined within this document at tft^ p
of terms can be found in Exhibit G.
irr^any user-prepared
>e /consistent with ASTM
1 ^abbreviations and symbols
.nt/of use. A detailed glossary
1.4.1 CAL: Calibration standards are definedVn Table D/SV-1 in which 5
levels of calibration/ar^dTfloed!| CAL 1, CA\ 2JCAL 3. CAL 4, and CAL 5.
CAL 1 is the lowest -con^entratum '^ndC&L5 is\the highest concentration.
CAL 3, which is the/mi/ level s^and^atd^, isNle.s,ignated as the solution to
be used for contii
1.4.2 Continuing
used to evaluate
check of the initial
The continuin;
curve.
andard: A solution of method analytes
rometer response over a period of time. A
is performed once each 12-hour period.
CAL 3 of the initial calibration
1.4.3
1.4.5 Laborator
peak area or height of analyte. x.
A compound added to a sample extract in
Irate concentration measurements of other
nents. The internal standard must be a
component.
nk (LMB): The concentrate from the extraction
January. 1992
Page D-5
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
of a clean, certified filter/adsorbent cartridge solutionythat is treated
as a sample. The filter/adsorbent cartridge is carri/d tzhrough the same
analytical procedure as a field sample. The surrogates/are spiked onto
the cartridge bed prior to extraction. The purpose/of cfee LMB is to
monitor for possible laboratory contamination.
1.4.6 Mass spectral interference: Defined as
analyte quantification ion due to presence of
"noise" at Che same mass.
nability\to
levels of
1.4.7 Method detection limit (MDL): A statistically determined value
indicating the minimum concentration of an analyte thatjtan be identified
and measured in a sample matrix with 99 /eroent confiide/ce that the
analyte concentration is greater than z/ro/ This valu/ varies with the
precision of the replicate measurement^useo^^or jme /calculation. (See
40CFR 136 APP.B)
1.4.8 PAH: Polynuclear aromatic hydrocarbon.
1.4.9 PCB: Polychlorinated bi
1.4.10 Performance evaluation
concentrations of method analyte
determine the accuracy and precisi
performed by a competent analyst.
concentrations are unknown to the
Agency.
A samp
has bsten
/zee
analyst!
taining known
to statistically
fe expected when a method is
and
samples are supplied by the
1.4.11 PUF:
XAD-2.
PolyureOnane^fonm \sed as anNadsorbent and as a support for
1.4.12 Re tent ion ydim/window:/ Ra6e«vion "t±ntp is determined for each
analyte of interest ils the tLjne *rom inJs^tLon to elution of a specific
chemical from a ^hroma^pgraonic/column. The window is determined by five
injections of a ihi£ialcsajabriition standard over a 24-hour period as plus
or minus three times^fehe standard deviation of the absolute retention time
for that analyte. For this doc^saent, the window is ±0.06 RRT units of the
continuing op-mlTt" te^gl cali1>r>atiohvs>tandard RRT for each target and
surrogate Compound.
/^"\ \ ^
1.4.13 /Selected Ion Guldent\Profile (SICP): A plot of ion abundances of
the ioris at an analyte produced by the mass spectrometer. SICP is used
inter^nai>geably with EICP, Vxt\-acted ion current profile.
1.4.1>xStoc>sstandard solj/tioti: A solution used to prepare calibration
standardsX. Nornf?wU.y. thisr solution will be at a concentration which is
easily dilute^^to aHe^ve/ which can be injected into the GC.
1.4.15 Surrogate
xmnd: A compound not expected to be found in the
January.
Page D-o
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
sample that is added to each sample prior to field deplayoient and before
extraction, and is measured with the same procedures used/to measure
sample components. The purpose of a surrogate compound %s to monitor
method performance with each sample.
1.4.16 VTSR: Validated Time of Sample Receipt
logged-in on the Chain-of-Custody Log-In Sheet b>
1.4.17 Working standard solution: A solutior
calibration standard. Normally, this soluti^
GC without additional dilution.
1.4.18 XAD-2: A resin used as an adsorb
sample is
January.
Page D-/
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
2 SAMPLE STORAGE AND HOLDING TIMES
2.1 SAMPLE IDENTIFICATION
2.1.1 In the field, the samples are packed in dry/ic
glass sample container containing the filter and
properly chilled, and shipped to the designated
2.1.2 The samples are logged in the laborato
data tracking system according to sample loc
cartridge number identification, and total
to standard temperature and pressure (STP),
logged-in on the Chain of Custody Log-In
validated time of sample receipt (VTSR)
ure that the
idge are
volume sampled, corrected
samples are
moratory is the
2.1.3 If the time between sample receip
24 hours, then the samples must be kept
of samples to fluorescent light. All samples mi
five (5) days of VTSR.
2.2 SAMPLE/SAMPLE EXTRACT STORAGE
2.2.1 The samples must be contarnedXin air-~l
protected from light, and refrigerkted\at 4'
receipt until extraction. Unused sahroles
regenerated in a manner that complies\ritF
ion is greater than
Minimize exposure
tracted within
containers,
£2eC)Trrfm the time of
'be disposed of or
applicable regulations.
2.2.2 -Sample extracts ma^rotected>fronM.ight and stored at 4°C
(±2°C) until 30 days aft er__de livery of a complete data package to the
Agency.
2.2.3 Samples and,
demonstrated to b€
51e extracts JBUSt bes-st^red in an atmosphere
of al]/ poytentialveontfaminants.
lets/ and standards must be stored separately.
2.2.4 Samples, si
2.3 CONTRACT REQUIRED HOLDING Til
2.3.1 The .Extraction shaj.1 be">
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
3 CARTRIDGE PREPARATION AND CERTIFICATION
3.1 SUMMARY OF METHOD
This section discusses pertinent information res
and cleaning of the filter, adsorbents, and filter/ads
assembly. The separate batches of filters and ad/
with the appropriate solvent. At least one PUF/^
assembly and one filter from each batch, or 10
whichever is greater, must be extracted and certi?
considered for field use. Prior to field sampling,
spiked with surrogate compounds.
3.2 APPARATUS AND MATERIALS
3.2.1 Acid-washed Pallflex filter: 4
Works, Inc., Cat. No. GMW QMA-4, 145
OH, 45002, 800-543-7412, or Supelco Inc., Cat
Bellefonte, PA, 16823-0048, or equivalent.
the preparation
cartridge
racted
Iter, General Metal
Village of Cleves,
, Supelco Park,
3.2.2 Polyurethane foam (PUF):
6.5 cm by 5 cm. These can be ms
stock, polyether type (density
upholstering, General Metal Works ">v
Ave., Village of Cleves, OH, 45002 ,v
No. 1-63, Supelco Park, Bellefonte,
two separate plugs are also commercial!
Works. •
3.2.3 XAD-2 resin:
Bellefonte, PA, 16823
3.2.4 Aluminum fo
with hexane.
3.2.5 Soxhlet ext:
and adsorbent cartrid"
3.2.6 Minivi
screw caps
plugs, S^Scm/by 2.5 cm and
3 inch tmck sheet
ure
_-16/, 145 South Miami
or Supelco Inc., Cat.
or equivalent. The
from General Metal
^79, Supelco Park,
tght at 500°C after rinsing
>le of extracting GMW Model PS-1 filter
5" length), 1000-mL flask, and condenser.
glass, with conical reservoir and
i^icone septa, and a vial holder.
lon®-coated stainless steel.
3.2.10 Kuderrta^Dani^k^K/D) /Apparatus: 500-mL evaporation flask (Kontes
K-570001-500, or esmivatentV, 10-mL graduated concentrator tubes (Kontes
K-570050-1025, or equis^alej/t) with ground-glass stoppers, and 3-ball
Januarv, 1992
Page D-9
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
macro-Snyder Column (Kontes K-5700010500, K-50300-0121 ./an/K-569001-219,
or equivalent).
3.2.11 Adsorption columns for column chromatography:
stands.
3.2.12 White cotton gloves: For handling cartridge's and
;m x 10 cm with
standards
3.2.13 Glove box: For working with extremely taxi
reagents, with explosion-proof hood for venting/fumes from
reagents, etc.
solvents,
3.2.14 Vacuum oven: Vacuum drying oven /system capat/le /of maintaining a
vacuum at 240 torr (flushed with nitrogen) e>vernigh£.
3.2.15 Concentrator tubes and a nitrogerNsyaporacio^ apparatus: with
variable flow rate.
3.2.16 Laboratory refrigerator.
3.2.17 Boiling chips: Solventyextractec
equivalent.
3.2.18 Water bath: Heated, with c«
temperature control.
mcentric
jnesh silicon carbide, or
7 capable of ±5°C
3.2.19 Vortex evaporator (optional).
/•""^
3.2.20 Teflon® sleeve/ for_the ground-glas\ jo\nts on the Soxhlet
extraction apparatusy
3.3 REAGENTS
3.3.1 Hexane: ghroma^pgraphdc ,g*rade, glas?' distilled.
3.3.2 Diethyl ether:\cJiromaTOgraphic grade, glass distilled.
3.3.3 Methyl£«e~~cttiej^ide: "Ckromatt>graphic grade, glass-distilled.
3.3.4 Sod'ium/s'ulfate^-s. Anftydrous ffcGS), granular (purified by washing
with metViylane chloride followed by heating at 400°C for 4 hours in a
shallow/ tr^y).
n: High puritfy RJrade .
3.4 PROCEDURES^FOR>REPARATIOp OF' FILTER, ADSORBENT, AND CARTRIDGE
3.4.1 Glass Fib^Filtfet P/eparation
3.4.1.1 The quartz^lber filters are baked at 600°C for five hours
January, 1992 —— • Page D.10
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
•sC learNc_ontainer
5-2/PUF
before use. To ensure acceptable filters, they are/extracted with
methylene chloride in a Soxhlet apparatus, similaryro /he cleaning of
the XAD-2 resin. The extract may be analyzed for/the/purpose of
determining cleanliness prior to certification.
3.4.1.2 The extracted filters are set aside
prior to combined extraction (certification)
glass cartridge assembly.
3.4.2 XAD-2 Adsorbent Preparation
3.4.2.1 For initial cleanup of the XAD/2 ifesin, a batch of XAD-2
(approximately 50-60 grams) is placed/in / Soxhleit apparatus and
extracted with methylene chloride fo^r 16/hours a>t approximately 4
cycles per hour.
3.4.2.2 At the end of the initial S&xhlet^xtraction, the spent
methylene chloride is discarded and repT&c^d wich fresh reagent. The
XAD-2 resin is once again extracted for 16 ne^irs atxaj>proximately 4
cycles per hour.
3.4.2.3 The XAD-2 resin is/removed
in a vacuum oven connected
dried at room temperature for\ap^roximate
solvent odor is detected).
leSpxhlet apparatus, placed
nTtro^eR~-gas stream and
hour/ (until no
NOTE: Alternatively, a 600 g batdt of XAD-2 resin is extracted with
methylene chloride for 16 hours. Atter Extraction, the resin is
transferred to a cleaffdry^ng columnX Th\n the resin is dried with
high-purity nitroaen us_ing Taflon® tubxtig from the nitrogen cylinder
with a charcoal tube/in tfis line^In an alternative method of drying,
the XAD-2 resin As placed in a Pyrex^coluhm (10 cm x 60 cm), allowing
sufficient spao4 for fluidi/ziru^?—»xhlet extraction procedure from each
;e of determining initial
fs prioi
Co c«
3.4.3
Adsorbent Prepa\ati
. 4.3>i The PUF adsorbent lis a polyether-type polyurethane foam
,0225 g/cm3)/
3.4.3.2
illustrated
while the top p]
is
assembly is composed of two inserts, as
rSV-2. The bottom PUF is 6.5-cm by 2.5-cm.
i.5-cm by 5.0-cm. The PUF inserts are cut from
January, 1992
Page D-ll
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
sheet stock and should fit with slight compression/in efhe glass
cartridge, supported by the wire screen. The two/PUF/plugs (i.e.,
1-inch and 2-inch deep) are also commercially available as pre-cut
separate pieces.
3.4.3.3 For initial cleanup, the PUF plugs a/e cfiacefra a vaWium/oven connected to a
water aspirator and a source of clean dryxnitrogen or air. Nitrogen
or air is purged through the oven to dry theNPJJF atxroom temperature
for approximately 2 to 4 hours. At the end of tfee^ drylsag period,
there should be no solvent od«£__detected.
3.4.3.5 The extract from tfte S
batch may be analyzed for thexpu
cleanliness prior to certification
extractTorT-pi?«c£dure from each
""""'"•*•"*••»— /
pse of^etjwaaining/initial
3.4.4 PUF/XAD-2 Adsorbent Cartridge Pfcepairat-ion
3/4.4.1 A nickel or/g^aTrTtess steel s^ree« (mesh size 200/200) is
fitted to the bottom! of a hex«ne-rinsed\gla\s sampling cartridge to
retain the PUF/XA^S-2/^dsor^entjs^as illustrated in Figures D/SV-1 and
/acuulfrvdriea\PUF (2.5-cm thick by 6.5-cm
>f cke-^screefr-i
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
3.5 PROCEDURE FOR CERTIFICATION OF PUF/XAD-2 CARTRIDGE ASSEMBLIES
3.5.1 Assemble the Soxhlet apparatus. Charge the Sophie/ apparatus with
500 mL of the extraction solvent (10 percent v/v diejzhyl/ether/hexane) and
reflux for 2 hours. Let the apparatus cool, disasssrnible^it, and discard
the used extraction solvent. Transfer the filter /ndJ'UF/XAD-2 glass
cartridge to the Soxhlet apparatus (the use of an/ex^rabtion Izhojnble is
optional).
NOTE: The filter and adsorbent assembly are
reach detection limits and to minimize cost..
together in
3.5.2 Add 500 mL of diethyl ether/hexane
apparatus. Reflux the sample for 18 houi
per hour. Allow to cool, then disassemble
10/percent
a rate/of/t
:he appa/atv/s
to the Soxhlet
least 3 cycles
3.5.3 Assemble a K-D concentrator by atbaching^^10/mL concentrator tube
to a 500-mL evaporative flask. Other concertferation^devices or techniques
may be used in place of the K-D, if equivalencyM^ demonstrated for all
the target analyte compounds listed in Exhibit C.
3.5.4 Transfer the extract by tfouring
containing about 10 cm.of anhydsou,
the extract in the K-D concentrator.
column with 20 to 30 mL of 10% die
quantitative transfer.
ract througfi--4 drying column
lular sodiunT-st*l£ate, and collect
Rinse~~ttie Etlenmey/r flask and
kther/nex/ane to~~Complete the
3.5.5 Add one or two clean boiling chips arih attach a three-ball Snyder
column to the evaporativer"fTa~S'ks. Pre-wet\the\Snyder column by adding
about 1 mL of the extraction solvent to the, top\of the column. Place the
K-D apparatus on a ho/t wa€erbath\(50°C) so tshay the concentrator tube is
partially immersed im tjie hot wjater, anb\the eiytire lower rounded surface
of the flask is bached/with hot/ vanw^_ Adjttfrt the vertical position of
the apparatus and/the/water te4pe/atures*ksre'quired to complete the
concentration in/oneSimir. At the proper rate of distillation, the balls
of the column willxactivfej^y/chatter but the chambers will not flood with
condensed solvent, when the apparent volume of liquid reaches
approximately 5 mL, remov«stheSsKvminutes. Remove the Snyder column and
rinse the f^ask and its^ipwer J^Hsnt mto the concentrator tube with 5 mL
of hexane/ Ax5^mL^s>tinge\is recomlBemded for this operation.
3.5.6 Jfwo/different types\of
obtair/a .final volume of 1. y ml
blowoVpwn techniques outline^ ii
respecsts-iye ly>
oncentration techniques are permitted to
micro-Snyder column and nitrogen
sections 4.4.2.4 and 4.4.2.5,
3.5.7 Analyz
section 6.6.
b/ GC/MS according to the conditions in
'point standard is used for certification.
The
January,
Page D-13
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
analytes in the standard should have concentrations at/or
the analyte CRQLs per injection (similar to CAL 1).
slightly above
3.5.8 The level of each target analyte for the ext^act'seach pair of
filter and adsorbent assembly analyzed must be leas than orxequal to the
analyte's CRQL, and the total level of target compou/dsNnust ns£ exceed
10 UK.
3.5.9 Document results on Form VIII-AASV, FiZtefc/Adsorbent Cartridge
Certification Form. Reporting requirements /are/listed in Exhibit B.
3.6 DEPLOYMENT OF CARTRIDGES FOR FIELD SAMPI
3.6.1 Prior to field deployment, a minimum/of thr«
(i.e., chemically inert compounds not e^xpecb&d toA>cc,
environmental sample) are added to the c?
cartridge, using a microsyringe. The surrogate con
each cartridge assembly.
rrogate compounds
r in an
the top PUF
ounds must be added to
3.6.2 The recoveries of the sur
unusual matrix effects and gros/ samp]
recovery is evaluated for accepsanc
concentration falls within the a
jate compounds are
:essing erro
determining
monitor for
Surrogate
.er the measured
ince
3.6.3 The following surrogate stam
determining matrix effects, breakthro
GC/MS. Refer to section 6.5.4 for
mixture.
Surrogate Coi
prep*
een successfully used in
analytical problems by
Kpn of surrogate spiking
Spikec
Anthracene - d10
Benzo(a)pyreny-
2,4,6-Tribro
2-Fluoropheno
Phenol-ds
Nitrobenzene-d5
2-FluoroM
p - Te rpheny 1-
it (tfg/cartridge)
100
100
100
100
100
100
100
too
ounds must be added to each adsorbent
as pre-sampling surrogates. The other
e added to the cartridges just prior to
ns are based upon a l-/zL injection of the
Page D-14
January,1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
4 SAMPLE PREPARATION FOR GC/MS ANALYSIS
4.1 SUMMARY OF METHOD
The filters and adsorbent cartridges are spiked
surrogate compounds and extracted with a Soxhlet
appropriate solvent. The extract is concentrate
evaporator, followed by optional GC/ECD or GC/F
GC/MS analysis, as illustrated in Figure D/SV-3^
4.2 APPARATUS AND MATERIALS
4.2.1 .Soxhlet extractors: Capable of extracting GMW
and adsorbent cartridges (2.3 in. x 5 in./lej(gth), 1(/00-
condenser.
DOSt-sampling
the
Lsh (K-D)
PS-1 filter
nL flask, and
4.2.2 Pyrex glass tube furnace system: ^Sor acbi^atfng silica gel at
180°C under purified nitrogen gas purge for aa^hour ,
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
4.2.13 Laboratory refrigerator.
4.2.14 Boiling chips: Solvent-extracted 10/40 mesh
equivalent.
4.2.15 Water bath: Heated, with concentric rin
temperature control.
con carbide, or
4.2.16 Vortex evaporator (optional).
4.2.17 Teflon® sleeves for the ground-glass
extraction apparatus.
of ±5°C
jo/lnts on the Soxhlet
ni2«d to avi
is
as
ied in
jntai
NOTE: Reuse of glassware should be min
cross-contamination. All glassware th
that is reused, must be scrupulously clea1
use. Rinse glassware with the last solvent
purity acetone and hexane. Wash with hot water
Rinse with copious amounts of tap water and severa
water. Drain dry and heat in a mu££le furnace at 400
Volumetric glassware must not b
should be rinsed with high-puri
is dry and cool, rinse it with hex
with solvent-rinsed aluminum foil rr
furnac^
4.3 REAGENTS
4.3.1 'Methylene chlori
4.3.2 Sodium sulfate/ Anhydrous \(ACS)
with methylene chlcr/lde/followe^
shallow tray).
4.4 PROCED
4.4.1
wi
he risk of
spatially glassware
as possible after
t and then with high-
.g detergent.
of distilled
hours .
rather, it
er the glassware
prtior
or
ted or capped
.de, glass-distilled.
(purified by washing
00°C for 4 hours in a.
4.3.3 Diethyl ejmerSxChromaffcogifaphic grade', glass-distilled.
4.3.4 Hexane: Chroma<£graphi
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
NOTE: The filter and adsorbent are analyzed togetherein order to
reach Contract Required Quantitation Limits (CRQLs) / to/avoid
questionable interpretation of the data, and to minimise cost.
4.4.1.2 Prior to extraction, the following five/add^J^ional surrogate
compounds are spiked onto each cartridge received from che field.
Spiked Amount
Surrogate Compound
Anthracene -d10
Benzo(a)pyrene-d12
2,4,6-Tribromophenol
2 -Fluorophenol
Phenol-d5
For blank and sample cartridges not^sentXmt tc/the field, these
surrogate compounds are spiked along with thWthree pre-sampling
surrogates (nitrobenzene-d5, 2-fluorobipnfe
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
concentrator tube is partially immersed in the hot/watJer, and the
entire lower rounded surface of the flask is bathed yith hot vapor.
Adjust the vertical position of the apparatus at
temperature as required to complete the concent
the proper rate of distillation, the balls of
chatter but the chambers will not flood with
the apparent volume of liquid reaches 5 mL,/ren
from the water bath and allow it to drain
minutes. Remove the Snyder column and
joint into the concentrator tube with 5 zfeL off
is recommended for this operation. Th^extract is^now ready for
further concentration to 1.0 mL by eijrher/the mic^o^Jinyder column or
nitrogen blowdown techniques.
4.4.3 Micro-Snyder Column Technique
4.4.3.1 Add another one or two clean boring ch«s /ron/ the gas source to the blowdown apparatus must
eel. copper, or Teflon tubing.
Page D-18
January, 1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
4.4.4.1 Place the concentrator tube with an open mLCxo-Snyder
attachment in a warm water bath (30° to 35°C) and evaporate the
solvent volume to just below I mL by blowing a gentle/stream of clean,
dry nitrogen (filtered through a column of activated/carbon) above the
extract.
4.4.4.2 The internal wall of the concentrator tube
down several times with hexane during the operation.
be\rinsed
4.4.4.3 During evaporation, the tube soWenb level must be kept bel$3w
the water level of the bath. The extrac/c mvfst never be allowed tc
become dry.
4.4.4.4 Bring the final volume brought lio 1.0 ml£ wi/th hexane.
Transfer the extract to a Teflon-sealed/screw-c/p dmber vial, label
the vial and store at 4°C (±2°C). Ahe extract/is/now ready for
optional GC/FID or GC/ECD screening/^io^llowfec/by/GC/MS analysis.
4.5 DILUTIONS
4.5.1 When a sample extract is analyzed that has an ahu^yte/ target
compound concentration greater tfnan tKe~Tipp«j^limit of the^initial
calibration range or saturated Xpnss~§«jni__a compoun
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
within the initial calibration range.
4.5.6 Do not submit data for more than two analysesJ i-d., the original
sample extract and one dilution, or, if the semivolarilexscreening
procedure was employed, from the most concentrated/dil^itionXanalyzed and
one further dilution.
Page D-20
January, 1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
5 GC/FID OR GC/ECD OPTIONAL SCREENING METHODOLOGY
5.1 SUMMARY OF METHOD
As an option, the sample extract may be screene
analysis to approximate the range of concentration/of
dilution prior to quantitation with the GO/MS. S,
utilizing a gas chromatograph coupled to specif
pesticides and other chlorinated compounds, el
(ECD) is used, and for the other semivolatile
detector (FID) is employed.
5.2 APPARATUS
5.2.1 Gas chromatograph: The gas chro
adequately regulate temperature in ord
temperature program and have a flow cont
column flow rate throughout temperature
must be suitable for splitless injection and ha:
including syringes, analytical columns, and gases.
to GC/MS
compounds for
>mplished
5.2.2 GC column: 30 m x 0.25 mm I.D.
thickness (DB-5, J&W Scientific\Fo'
prog
stem must
oducible
a constant
The system
uired accessories
jj.i.ca columnyi.O
_CA, or
filter
5.2.3 Electron capture detector: x^he\nakeu]4 g^s musFlDe P-5, P-10
(argon/methane) or nitrogen according^toNthe instrument specification.
The GC/ECD system must be in a room inNwhich /che atmosphere has been
demonstrated to be free of all contaminants which may interfere with the
analysis. The instrumene^muTt->be vented \o tne outside of the facility or
to a trapping system wjrtich_E£events the rer§ase\of contaminants into the
instrument room.
5.2.4 Flame ioniza/tiorf detectc
5.2.5 Data system: T^data system must be interfaced to the GC/FID or
GC/ECD. The dataajcstemSuso^t allow the continuous acquisition of data
throughout the duratibn^pf the/chromatographic program and must permit, at
the minimum, the output o^timeNzs intensity (peak height or peak area)
data. Also, tfe« da-fca^systemNftust Bistable to rescale chromatographic data
in order to//repojrt^chrom*t^>granisssiieet^ag the requirements listed within
this methc
5.3 REAG
le c
choose^Xp use
in the SDGNJarra
chromatograph
choose to use
rourjinel applications is helium. Laboratories may
carrier gas, but must clearly identify its use
ayL divider pages preceding raw
bmi4sions to the Agency. Laboratories that
dvised to exercise caution in its use. Use of
January. 1992
Page D-21
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
a hydrogen leak detector is highly recommended when hydrogen is used as
the carrier gas. All GC carrier gas lines must be con/trutted from
stainless steel or copper tubing. Non-polytetrafluor/ethylene (PTFE)
thread sealants or flow controllers with rubber comp,onenT5^ are not to be
used.
5.4 STANDARD PREPARATION
5.4.1 The CAL 3 working standard solutions
to section 6.5.11 may be used for screening
5.4.2 If the level of chlorinated solvent
the standards prepared for GC/MS analysis/in
methods, .-;tock standard solutions made
such as hexane may be prepared, then ac
solvent to contain CAL 3 levels outlined
5.5 INSTRUMENT OPERATING CONDITIONS
Suggested GC operating condit^
GC Column:
hexane prepared accoi
irppses.
solutions) in
the GC screening
orinated solvents
in an appropriate
1.
Carrier Gas:
Flow Rate:
Column Program:
Initial Time:
Ramp Rate:
Final Temperature:
5.6 PROCEDURE
5.6.1 Before anal/si*
within optimum op/rat3
procedure, and it
properly calibrated,
DB-5 fus\d
siloxane
Helium, 28
1 cm/minute.
Initial Temper
1 min
^to 200°C
300°C.
can be yerfi6rmed7Nnake/sure that the system is
conditions. This is an optimal screening
laboratory to ensure that the GC is
that /table retention times are obtained.
5.6.2 Inject ifc«-TraiibratioiK$tan
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
the necessary dilutions, if any, to reduce the major pee
and full scale deflection when performing GC/MS analysis.
to between half
5.6.6 Make any necessary dilutions and proceed with/GC^MS analysis
(Section 6).
5.6.7 It is recommended that extracts be diluted7 so/tfi^t all^eaks are on
scale. Overlapping peaks are not always evident/when peaksxare off scale.
Computer reproduction of chromatograms, maniptd^^e^ to ensure ail pes
are on scale over a 100-fold range, are accepytab^e if linearity is
demonstrated. Peak height measurements are .recommended over peak arel
integration when overlapping peaks cause eyrory in area integration.
Januarv, 1992
Page D-2J
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6 GC/MS ANALYSIS
6.1 SUMMARY OF METHOD
This method outlines a GC/MS procedure for th
semivolatiles following sample preparation (Sect}
screening (Section 5).
6.2 INTERFERENCES
6.2.1 Method interferences may be caused
reagents, glassware, and other sample proc
discrete artifacts and/or elevated basel^i
All of these materials must be routineli
interferences under the conditions of
method blanks (LMB).
contaminants in solvents,
iss/ng harcwarfe that result in
in the ydet^ctor profiles.
nonstraced to be free from
by/running a laboratory
6.2.2 Glassware must be scrupulously cleaned. ^S^ean>il glassware as
soon as possible after use by rinsing with the 1 ast^^olvenoused in it.
This should be followed by deter
with tap water and reagent wate
rinsed with acetone and spectro&rapl
rinsing, glassware should be seal
prevent any accumulation of dust o
washing with hot w^er/and rinsing
It sKotti^—tlienbe drained dry, solvent
hexane~:A£ter drying and
environment to
Glassware should
be stored inverted or capped with alumira
NOTE: The glassware, except for volumetric
placing in a muffle furpsJc"e~at--4500C for
ho'
ninants.
may be further cleaned by
nrs to remove trace organics,
6.2.3 The use of high pvfrity
minimize interference nroblems.
in all-glass systems may be rej/uir
6.2.4 Matrix in^erfe^sences
coextracted from tfee sambie/
reagents\. ahd solvents helps to
lirif ib&tion \/T solvents by distillation
caused by contaminants that are
6.2.5 The extent of inte'Tsfereric^s that may be encountered has not been
fully assessed—KithQugh GC^cpndifelons described allow for unique
resolution/of comj)oundsx&overeaxk¥ th?s method, other compounds may
interfere/ TKeanaly^j^cai^ystem mtwt be routinely demonstrated to be
free of/internal contamrejantSv such as contaminated solvents, glassware, or
other oeae/nts which may IteadVo method interferences. A laboratory
reagetit biank may be run for each batch of reagents used to determine if
reagents arc^e contaminant-fr?e .
6.2.6 The^T&e are^opncerns /fchalf during sample transport and analysis, heat,
ozone, N02, ahd ultr>5^ioLet /UV) light may cause sample degradation.
These problems should oe adoressed as part of the user-prepared SOP
manual. Where possible, i/ncandescent or UV-shielded fluorescent lighting
in the laboratory shoul^S/be used during analysis.
Januarv. IV91
Page D-24
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
/ith a
^plitless
constant column
6.3 APPARATUS AND MATERIALS
6.3.1 Gas chromatograph: An analytical system compl
temperature-programmable gas chromatograph suitable
injection equipped with a flow controller that main
flow rate throughout temperature program operation
accessories, including syringes, analytical columj
carrier gas lines must be constructed from stai
tubing. Non-polytetrafluoroethylene (PTFE) th
controllers with rubber components should not/be
6.3.2 Mass spectrometer: Capable of scanning /from 35 to 510 amu every 1
second or less, utilizing 70 volts (nominal') edectron/^nfergy in the
electron impact (El) ionization mode and/producing a/mass spectrum which
meets all the instrument performance cri/teri:a when %Q ng of
decafluorotriphenylphosphine (DFTPP) is(injebted through the. GC inlet. To
ensure sufficient precision of mass spectral da^^a/ ttie MS scan rate must
allow acquisition of at least five scans whibs^a sample compound elutes
from the GC. The GC/MS system must be in a roonf'xith a"fcmpsphere
demonstrated to be free of all potential contaminanbsswhichvwill interfere
with the analysis. The instrumen*—msist be vented outsitte the facility or
to a trapping system which prevents there~b&e*e_pf contamirtants into the
instrument room.
NOTE: DFTPP criteria must be met b\
Any samples analyzed when DFTPP crite
reanalysis at no cost to the Agency.
any/sample extracts are analyzed.
lot been met will require
6.3.3 GC/MS interface:
interface that gives a^cep
parameters of interes
(Exhibit E), may be .use
interfaces constructed/of
recommended. Glass c/n be
dichlorodimethyl^ilan
ny fa* chromatograpPK to mass spectrometer
le calibratioTVNpoirvts for each of the
ev|es^_all acceVtaHle performance criteria
hromatoi?aph to/mass spectrometer
ed materials are
tiyated BYvjsil/anizing with
6.3.4 Data system: Ttvcompute-tsystem must be interfaced to the mass
spectrometer that allows ctje con^nuous acquisition and storage on
machine-reada>te~MSTiia^of allxmass spectra obtained throughout the
duration of/the chroma tog-caphicpr^gram. The computer must have software
that alloys se^rchingxs^he G'S/MS dat&^file for ions of a specific mass and
plotting/suon ion abundancesN/ersus time or scan number. This type of
plot is/defined as Selecteo. loii Current Profile (SICP) . Software must be
avail able/that allows integnat'itig the abundance in any SICP between
numbejr limits. Also, for the non-target compounds,
softwabssmustN^e available /hay allows comparing sample spectra against
ecent release of the NIST/EPA/MSDC mass
spectral 1 ibraiiy shaH.be/usera as the reference library. The data system
must be capable oSvflaggrng/all data files that have been edited manually
by laboratory personr
January. 1992
Page
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.3.5 Magnetic tape storage device: The magnetic tape/stotage device
must be capable of recording data and suitable for lory;-term, off-line
storage.
6.3.6 Chromatographic Column: A 30 m x 0.25 mm I/D. Ipr th^ mm I.D.)
bonded-phase silicone-coated fused silica capillary oolulBn (J&Wv^Scientific
DB-5, Alltech Associates SE-54, or equivalent) imast/toe useoX^A
thickness of 1.0 pm is recommended because of ics^Jfarger capacrt
thickness of 0.25 fj,m may also be used. A megabor« column (0.53
may also be used as long as all QC criteria are jnet.
6.4 REAGENTS
6.4.1 Hydrogen and helium:
percent).
Gas cylind
purity, (99.9999
6.4.2 Combustion air: Ultra high purity.
6.4.3 Zero air: May be obtained from a cylinder o*^zero^§rade compressed
air scrubbed with Drierite or sili^agel and 5A molecular siJive or
.activated charcoal, or by catalytic cTearm^-Qf__ambient airx All zero air
must pass through a liquid argon\coi^—tr^£ for fina"i--€-l6ajiup.
6.5 STANDARDS
6.5.1 The Contractor must provide all\standards to be used with this
contract. These standards may be used only efter they have been certified
according to the procedupcr-~Iri>£jdiibit E oVbyNthe manufacturer. The
Contractor must be able/to verify^that the \tanXards are certified.
Manufacturer's certificate's""ofN^na\Lysis mustN^e detained by the Contractor
and presented upon request. Eaqh call&r^tion sjtandard solution shall
contain all the appropriate sur/ogatesand^saternal standards. Neat
standards with compou/fd purity/of/at lea^s^ 97/ percent must be used.
6.5.2 Commercial"tyvsprep^ed'st/ck standards may be used at any
concentration if they^-a^e certified by the manufacturer or by an
independent source, or tr^ceablexto EPA-supplied standards. Fresh stock
standards musju-fee—pe«j>ared OTK^ ewisy tweIve months, or sooner, if
standards have degradedNar conceTi^ratea. Stock standards should be
checked for sigfis oT^degraas^tion or^xioncentration just prior to preparing
secondary diJ^ution and w&rking standards from them. Table D/SV-1 outlines
the concentrations of the wprlcing calibration standards.
CAUTI0N: '"•Each time a vial cbntkining small volumes of solution is warmed
to roomxtempeTsature and opened^ a small volume of solvent in the vial
headspace^e^apora^s, significantly affecting concentration.
6.5.3 InstrumeivbNperfoWanoe check solution
Prepare a solut^«t/ of decafluorotriphenylphosphine (DFTPP), such
January, 1992
Page D-2b
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
*
*
*
that a 2-/iL injection will contain 50 ng of DFTPP.
also be included in the calibration standards at tfctis
6.5.4 Surrogate Compounds Spiking Solution
DFTPP should
evel.
Prepare separate solutions to contain approximate 1^\H)00 Mg/roL of
each surrogate compound. From these solutions, .prepare tnfexspiking
solution to obtain the following amounts wham 1/mL is spiked ra^o the
cartridges. Fill a 1-mL syringe with the sWybgate spiking\solutlvcolume
Table
surrogate compound.
6.5.6
-di^h-lorobenzene-d4,
, chrysene-d12,
mg of each compound in
accessary to use 5 to 10
on and a few minutes of
the constituents. The
standard at a concentration of
of this solution should be added to each
will result in 40 ng of each internal
extract injected into .the GC/MS. See
andards used for each target and
NOTE: Each
le Spiking Solution
compounds used for the laboratory control
spiking mixtures containing the acid-
he base-neutral LCS compounds at a
ig/mL. Spike a clean cartridge with the
of each LCS compound.
(acid-neutral and base-neutral) may be spiked
January, 1992
Page D-2/
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
separately onto the cartridge or may be mixed into /one/solution just
prior to injection into the cartridge. /
/ /
6.5.7 PAHs Stock Standard Solutions
eighing
6.5.7.1 Place 0.1 gram of native PAHs on a
disk and weigh on a balance.
6.5.7.2 Quantitatively transfer each to 4 15-mL volumetric fla^k.
Rinse the weighing disk with several small portions of methylene
chloride. Ensure all material has been/tramsferred. Dilute to mark
with methylene chloride. The concentration of th^^ock standard
solution of PAHs in the flask is 10
6.5.7.3 Transfer the stock standaxxi solutions/infa Teflon-sealed
screw-cap bottles. Store at 4°C (+2xure pesticide analyte,
these two pesticides,
d as that prepared for
pound in hexane and dilute
osulfans) volumetric flask.
mL, except the Endosulfans,
rger volumes of stock solution
6.5.9 PCBs
Standard solutions into Teflon-sealed
(±2°C) and protect from light. Stock
frequently for signs of
l.on, especially just prior to preparing working
.s may be prepared by diluting the stock
g standards are then prepared from the
.s .
lutions
6.5.9.1
concentration
Prepare
caliS
£k solution of each of the nine PCB
;ion congeners at a concentration of 1
in
Page D-28
January,
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
hexane. Place each solution in a clean glass vial wTfch a Teflon-lined
screw cap. Fill to the top so no headspace is evident/ Store at 4°C
if solutions are not to be used right away. SoluViong are stable
indefinitely if solvent evaporation is prevented.
6.5.9.2 The 9 individual PCB congeners listed/in
used as the calibration compounds for PCB
at each level of chlorination is used as th
standard for all other isomers at that
decachlorobiphenyl (C110) which is used i
groups. The basis for selection of thes
been reported and referenced in Section/7
4.
rableXQ/SV-4 are
isomer
cotfcentrattsri calibration
chlorinatio~n^ except
C19 and C110
ibration congeners hits
itation 9) and Table D/SV-
.etbfer
6.5.9.3 Take aliquots of the stock /solutions of t
concentration calibration conge ners(and
proportions that will provide a prim.
the composition ratios illustrated in Tab^e D/S
solution in a clean glass vial with a Teflor
at 4°C. Mark the meniscus on the vial wall to
during storage; solutions are-^£able indefinitely
evaporation is prevented.
te nine PCB
in the
on/standard solution of
Place each
c^rew cap and store
olution volume
ent
6.5.9.4 Five calibration solutions are
internal standards, surrogates\ anX tarj
Table D/SV-1. Because MS respond
level of chlorination, PCB congeneV cot
solutions increase with level of chtorir
highest concentratiQR"sorution (CAL 5^
that allow injections of 1 /u\aliquots
column overloading. /""X
6.5.10 Stock Standard/Solutions oi
icr
Ijuitejdcpntiiining the
§t (compounds as specified in
decreases with increasing
itrations in calibration
jition. Components of the
^present at a concentration
aut MS saturation or GC
tivolatiles
6.5.10.1 Pla^e
a tared alumirtt
gram/ofyeach native semivolatile target analyte on
sk and weigh on a balance.
6.5.10.2 Quantitative^ transfer to a 10-mL volumetric flask. Rinse
the weigh^g—tfrsk^with se^^eral^sjjiall portions of methylene chloride.
Ensure >tnat all mate'sial hav^sbeew transferred. Dilute to mark with
me thy lrene/6nlorio^&- Tfiie concenb«ation of the stock standard solution
of s/miyolatiles in^he riask is 10
6./5.10'. 3 Transfer the sto
bottles. Stone
stkadard 3<^lutions shouid
degradation^c evaporatio
calibration standards
ik standard solutions into Teflon-sealed
4°C (±2°C) and protect from light. Stock
'e checked frequently for signs of
especially just prior to preparing
6.5.10.4 Seconc
standards may be prepared by diluting the stock
January, 1992
Page D-29
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
standard solutions. Working standards are then pre^are^d from the
secondary standard solutions .
6.5.11 Working Calibration Standards
Prepare calibration standards in hexane at a /mrtmum
concentration levels as outlined in Table D/2V-V. EactNc^l itration
standard shall contain the appropriate targetCompounds , intrnal
standards, and surrogate compounds as outlone-d in Tables
Great care must be taken to maintain the /integrity of all standard
solutions. Store all standard solutions' at/4" C (±2°C) in screw-cap
amber bottles with Teflon liners. Fresfti s/tandards/^hpuld be prepared
every twelve months at a minimum. Th/ continuing^ calibration standard
(see Table D/SV-1, CAL 3) should be yprejtered weekly and stored at 4°C
(±2°C).
6 .5 .12 Storage of Standard Solutions
6.5.12.1 Store the stock and secondary standar"&ssolu
(±2°C) in Teflon-lined screw-cggamber bottles. Sbscre
standard solutions at 4°C (°C)irr^&£iQivlined scre
bottles.
is at 4°C
e working
ap amber
sample extracts,
replaced every twelve
ty control check samples
6.5.12.2 Protect all standard,
and standards must be stored sep
6.5.12. 3 Stock standard solutions
months, or sooner, if-^omTwicison withN
indicates a probler
6.6 INSTRUMENT OPERATIN
6.6.1 Gas chroma to gra'ph: The/foMowingx^re >6he recommended gas
chromatographic analy&^cal conditions, as oQtlined also in Table D/SV-2,
to optimize conditions fct^cjompyund separation and sensitivity.
Carrier Gas:
Linear Vel
Inj ector^Temperatur
Injector:
Temperature Program":'
Iniclal/Hold Time:
Ramp Bate:
F/nal^Temperature:
/•tica^^Time:
Injecbipn Voiyme*:
/ splitless.
litial Temperature: 50°C
4JQ ± 0.1 min.
NOTE: A vobme
shown in this do
/appyroximate ly 50 minutes
l-AL
las been found to work with the concentrations
If a different volume is used, the laboratory
Page D-30
January, 1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
must make appropriate adjustments to the calibratiorT^&cncentrations.
Smaller volumes may be used only with automated sys4:en
6.6.2 Mass spectrometer: The following are the rec
spectrometer conditions for full range data acquisy
Transfer Line Temperature: 250-300°C
Source Temperature:
Electron Energy:
lonization Mode:
Mass Range:
Scan Time:
6.7 ANALYTICAL SEQUENCE
According to May
Specifications.
70 volts (nom/na)
El
35 to 500
At least
second pe
data acquisition
not to exceed 1
me period shall be as
Perforance Evaluajtio
The GC/MS analytical sequence for each
follows:
6.7.1
6.7.2
6.7.3
6.7.4
6.7.5
6.7.6
6.7.7
6.8 INSTRUMENT PERF^RMAN€E CHEC
6.8.1 Summary
Instrument Performanj
Initial or continui
Laboratory method bla:
Laboratory Control Sample
Field Blank
(if available)
to e^abli^h^that a given GC/MS meet tuning and
abundance Criteria prior to initiating any on-
s illusWated in Figure D/SV-4. This is
througfNtheNanalysis of decafluorotriphenylphosphine
6.8.
6.8.27
analyzed
Also, whenev
rformance check solution of DFTPP must be
Id o/ice per 12-hour time period of operation.
atory takes corrective action which may change
January, 1992
Page D-.5I
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
or affect the mass spectral criteria (e.g., ion source/cleaning or
repair, column replacement, etc.), the instrument/per/formance check
must be verified irrespective of the 12-hour labj/ra^ory requirement.
Lys;
Its
6.8.2.2 The 12-hour time period for GC/MS an.
injection of the DFTPP which the laboratory
of a compliance tune. The time period ends/afte'r 12 ho>«:s ha
elapsed. In order to meet instrument performance check
samples, blanks, and standards must be in/ec^ed within 12 hou:
DFTPP injection.
6.8.3 Procedure
at the
documentation
6.8.3.1 Inject 50 ng of DFTPP into/the/GC/MS
conditions must be identical to th^se
that a different temperature programNu^y
6.8.3.2 The DFTPP may be analyzed separately or
calibration standard.
fstdm. All instrument
section 6.6 except
:>art of the
6.8.4 Technical Acceptance Cri/eria
6.8.4.1 Prior to the analysis 0$. any
standards, the laboratory must\escablist
the mass spectral ion abundance\riceria
performance check solution containing DI
;> lea^bl anils', or calibration
at tne"EC/MS system meets
&or the instrument
PP.
6.'8.4. 2 The GC/MS syg'teST'Taus t be che^ckedxfor instrument performance
at the frequency described rh section &^8.A. The GC/MS system must be
tuned to meet the/ma«ufacburer' s specif iWtibns , using a suitable
calibrant. The/mas/ calibration afitk^resoiv'tion of the GC/MS system
are verified by/ ch^e analyses of—ttje installment performance check
solution.
6.8.4.3 The abundarfee^yrit?eria listed in Table D/SV-5 must be met for
a 50 ng injectiorN^f DFTP^. The mass spectrum of DFTPP must be
acquired by averagingxthreeXscans (the peak apex scan and the scans
inunediately—p-reseding and^folrbHing the apex) . Background subtraction
is required, ^nd mus^be accomplished using a single scan prior to the
eluti0n
/All ion abundance MUST be normalized to m/z 198, the nominal
ifeak, even though \he\ion abundances of m/z 442 may be up to 110
that of m/z 198.
6.8.4^^ The^x^riteriayaboye are based on adherence to the acquisition
specifications rdenti/fieia in Table D/SV-5 and were developed for the
specific target conTp'ouna list associated with this document. The
criteria are bas~«4 on/performance characteristics of instruments
January, 1992
Page D-32
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
currently utilized in routine support of Program activities. These
specifications, in conjunction with relative response factor criteria
for target analytes are designed to control and moftit/r instrument
performance associated with the requirements of finis/document. As
they are performance-based criteria for these soeciric analytical
requirements, they may not be optimal for addi/ion^l target compounds.
6.8.5 Corrective Action
6.8.5.1 If the DFTPP acceptance criteria,
retuned. It may be necessary to clean tl
or take other actions to achieve the
6.8.5.2 The DFTPP acceptance critery
standards, field samples, or require
standards, field samples, or requii
criteria have not been met will requii
cost to the Agency.
6.8.6 Documentation
Reporting requirements
Performance Check data resu
Instrument Performance Check
6.9 INITIAL CALIBRATION
6.9.1- Summary
6.9.1.1 Prior to
after tuning crity
each GC/MS syste,
concentrations
of GC/MS resp
6.9.1.2 All
in the initial ca
continuing calibratio
6.9.2 Fre
not met, the MS nttist be
>n source, or quadrupoWs,
criteria.
>
fore any
lyzed. Any
alVzed when tuning
s at no additional
trument
-AASV, GC/MS
Januarv.1992
and required blanks, and
check) have been met,
libraȣed at a minimum of five
itivity and the linearity
and the surrogates.
''are quantified using the RRFs from CAL 3
'or the RRFs from the most recent valid
within the same 12-hour period.
be initially calibrated upon award of the
ratory takes corrective action which may
calibration criteria (e.g., ion source
eplacement, etc.), or if the continuing
ria (see section 6.10.5) have not been
Page D-33
-------
Exhibit D
Setnivolatile Organics Analysis of Ambient Air
6.9.3 Procedure
6.9.3.1 Set up the GC/MS system under the conditzlon^ outlined in
section 6.6.
6.9.3.2 All working standard solutions must Be afllo^edto
ambient temperature (approximately 1 hour) h€fo;re analyst
6.9.3.3 Tune the GC/MS system to meet the' te
criteria in section 6.8.4 for DFTPP.
bhnical acceptance
6.9.3.4 Prepare five calibration standard's contaihir^g the target
compounds, internal standards, and surrogate compounds at the
concentrations outlined in Table D/SAf-l^and acc^rdjmg to the procedure
in section 6.5.
6.9.3.5 Calibrate the GC/MS by injecting^l^O ^I^f each standard. If
a compound saturates when the CAL 5 standaroHs injected, and the
GC/MS system is calibrated to achieve a detectio^xsens^fcivity of no
less than the CRQL for each oe«pQund, the laboratoryxmus/t document it
in the SDG Narrative, and attach a qu2n"tt&a-tion report and
chromatogram (see Exhibit B)\ Tn~-t*tis^_instanceT~"ttre--4aboratory must
calculate the results based on. a Xour-poi^t initial Calibration for
the specific compound that saturates. Secondary ion quantitation is
only allowed when there are sampre interfe/rences with the primary
quantitation ion. If secondary ion. quanta tation is used, calculate a
relative response factory using the a\ea xesponse from the most intense
secondary ion which/tsrreex,of interferences, and document the reasons
for the use of the/secondarv\on in the\SDG\ftfarrative.
spectrum of each
ecorded spejctra
6.9.3.6 Record
subtraction and/ spectrum
acceptability
libraries. J(f atT^accepta'bl
component is nb-tacqui
performance. If pterformar
extract data for the partic
compound(>}-~ancr-tiie_ natur
mpound. Background
.eeded. Judge the
Baring them to spectra in
spectrum of a calibration standard
ake necessary actions to correct GC/MS
e cannot be corrected, report sample
compound(s), but document the affected
problem.
6.9.3/1 P6r PCBs>sCompire the ^qVantitation ion to the confirmation
ion. / A/proper calibrations using the CAL 3 standard should document
the/rap.0 in the ranges^ fo\nd in Table D/SV-7.
6.9.4/ CaDs^lations
NOTE: "^in theXfollowin^ calculations, the area response is that of the
primary qtiaotitatipn /on/unless otherwise stated.
6.9.4.1 Relativ>x^.esp/6/nse Factors (RRF) : Table D/SV-8 outlines
January,1992
Page D-34
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
characteristic ions for the surrogate compounds and internal
standards. Table D/SV-9 outlines primary and secondary quantitation
ions for the target compounds. Calculate RRFs f or/earfn analyte target
compound and surrogate to the appropriate internal s/andard using the
following equation:
RRF =
A C
. D/SV-I
where: A^ = area of the primary quantisation ion for the compound
to be measured;
Ais = area of the primary quapftit^tion ion for the internal
standard;
C1S = concentration or amount
-------
Exhibit D
Seraivolatile Organics Analysis of Ambient Air
6.9.4.4 Mean of the Relative Retention Times (RRT/: yCalculate the
mean of the relative retention times (RRT) for eac(n analyte target
compound and surrogate over the initial calibration/range using the
following equation: / \_
RRT.
n
D/SV-5
where:
RRT
= mean relative retention
or surrogate for each it
and
= relative retention tiipfe
surrogate for each
for the target cotepounc
calibration standard
rg«t compound or
at/on standard.
6.9.4.5 Mean Area Response (Y) foaf Internal Standard: Calculate the
area response (Y) mean for primary qb^ntita^on /ion each internal
standard compound over the initial calife^tion £ange using the
following equation:
n ** ^^ ^^
Eq. D/SV-6
where: Y
mean area res^pon&e;
area response
internal standai
6.9.4.6 Percent Area Response Change
each calibration leyeiToTx^ach of
following equatior
where:
quandtation ion for the
calibration level.
.C) : Calculate the %ARC at
ernal standards using the
Eq. D/SV-7
response cnange;
of the internal standard at a
jcentratt'ion level; and
mean^^rea response of the internal standard in the
antire caj^ibratiojn range.
6.9.4/7 M€arTofM±e Re^ention^Cafnies (RT) Fo_r Internal Standard:
Calculate the mean o€ th\ retention times (RT) for each internal
sta/datfa over the inicialValibration range using the following
ecjuat/on:
Eq. D/SV-8
where: RT
RT =
retention time; and
stention time for the internal standard for each
inrt4/&l calibration standard.
January, 1992
Page D-36
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.9.4.8 Internal Standard Retention Time Shift (RTS,
RTS between the_RT of each internal standard at
level and the RT for that internal standard over
calibration range using the following equation:
RTS = ~RT~i - RTX
where: RT£ = mean of the retention time
in the initial calibration;
RTX - retention time of the intgrr
concentration level.
Calculate the
Sncentration
Eq. D/SV-9
standard at a
6.9.5 Technical Acceptance Criteria
6.9.5.1 All initial calibration stahda/ds must/be/analyzed at the
concentration levels and frequency mescribed Ln tWis section on a
GC/MS system meeting the DFTPP installment pessrorjmance check criteria.
6.9.5.2 The performance criteria for initii
must show:
Baseline separation/of beta^l
Baseline separation
calibration of the CAL
amma-BHCTN
Signal/noise ratio of >5
to illustrate MS sensitivi
^£ ^99 of PCB congener C110-PCB
Lack of degnatlatT&Ts^of endrin\ eXamine an extracted ion
current profile (EICP^ for m/z\7 rn the retention time window
between 4/4 'T^DEsfcd dndgsulfan aulfate; confirm that the
abun nofe ot m/z 67jarthelxtentrian time of endrin aldehyde
is gi jrcer/than lO^ercyetU^of th^yabundance of m/z 67 produced
by enjnriiyf and
6.9.5.3 The ItR^s a£^e^h calibration concentration for each target
compound and surrogate thg£ has a required minimum response factor
value must be greaterx^hanJM^equal to the compound's minimum
response factor see Table D/SV-6.
equal to the
, the value
When the valu<
Ltion]
of RRl
GC/MS perl
6.9.5.5 The RR'
Lhe initWl calibration range for each target
has a required maximum %RSD must be less
ed maximum value. For all the other target
D must be less than or equal to 25
%RSD exceeds 25 percent, analyze
'opriate CALs to obtain an acceptable %RSD
icentration range, or take action to improve
ch of the target compounds and surrogates at
January, 1992
Page D-37
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
each calibration level must be within ±0.06 relative retention time
units of the mean relative retention time for the /compound.
6.9.5.6 The internal standard %ARC at each cal
within ±40 percent of the mean area response
calibration range for each internal standard..,
6.9.5.7 The retention time shift for each
at each -alibration level must be within
mean retention time (RT) over the initia c
internal standard.
level must be
initial
range
6.9.5.8 The compounds listed in Exhibit/C must ideej/f the minimum RRF
and maximum %RSD criteria for the ii/iti^l calibration, with allowance
made for up to four target ai.d surR^gateXompoundy. However, the RRFs
for those four compounds must be greats^r thaw 0.010, and the %RSD of
those four compounds must be less than orxejqualN^i 40.0 percent for
the initial calibration to be acceptable.
6.9.6 Corrective Action
6.9.6.1 If the technical a6cep^3n«e_£riteria
are not met, inspect the system for proo]
clean the ion source, change tree column,
actions to achieve the acceptance
ial calibration
be necessary to
take otner corrective
6.9.6.2 All initial calibration tecHmic%l acceptance criteria MUST be
met before any sampLe"s"'or>>eauired blanksxare analyzed in a 12-hour
time period for an/:Lni£ial calibration \naIVtical sequence. Any
samples or requir/ed b(lanks\analyzed whenNinicial calibration criteria
h'tve not been mar w/11 require reanaS^ysis »t ro add' ional cost co the
Agency.
6.9.7 Documentation
Reporting reqC
calibration data
tabulated
,™
cement^ are listed in Exhibit B. Initial
reported on Form V-AASV, Initial
standard area and retention times
shall
6 . 10 CONTIN#INeen/met, the initial calibration of each GC/MS
checked by analyzing a continuing calibration
'ens/ire that the instrument continues to meet the
and linearity requirements of the method, as
D/SV-4. The continuing calibration standard
Page D-38
January. 1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
surrogates,
calibration
ipd after
(CAL 3) shall contain the appropriate target corapou
and internal standards.
6.10.2 Frequency
The GC/MS system shall be calibrated with
standard (CAL 3) at the beginning of every
the injection of DFTPP, to check for the va
calibration.
6.10.3 Procedure
6.10.3.1 Set up the GC/MS system under the condifioys outlined in
section 6.6 and as specified by the manufacturer/ and. tune the GC/MS
system to meet the technical acceptance/criteria iji section 6.8.4 for
DFTPP.
6.10.3.2 All working standard solutionsNnust ba^allowed to warm to
ambient temperature (approximately 1 hour) oe^ore analysis.
6.10.3.3 Start the analysis/-af^the continuing calrkrati&n by
injecting 1.0 ftL of the CAL/3 standa?lh~&«iiition which contains the
appropriate target analytesV su^r«ga£ecompoun3sT~a«d/ internal
standards using the procedure\li9£ed the~7ini/tia_l calibration section.
6.10.4 Calculations
\v
6.10.4.1 Relative Response Factor (>RRF)s: Calculate a relative
response factor (RRpjT^Eor~"B^ch target\comfcpund and surrogate using the
equation in sectic
6.10.4.2 Percent D/fferenc\ (ID)T'^Cg.lcuJ^aite the percent difference
between the meam relative t/espons^.facfeb^y (RRF) from the most recent
initial calib/ati/on and ttte c^ntinurngc/libration RRF for each
analyte targ/t coftmpund /ndy4urrogate using the following equation:
x 100
Eq. D/SV-10
where
6.10.5
difference between relative response factors;
e relative response factor from the most recent
calibration; and
response factor from the continuing
ion standard.
riteria
6.10.5.1 The\contfnuing calibration standard must be analyzed for the
compounds listeoMji Exhibit C at the frequency described in section
January, 1992
Page
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.10.2 on a GC/MS system meeting the DFTPP instrument
check and the initial calibration technical accepzfanc
6.10.5.2 The RRF for each target analyte and
required minimum relative response factor valv
or equal to the compound's minimum acceptably
factor.
irro§
must
fat}
performance
criteria.
Ite that has a
greater than
response
ration, the %D bet
the
impound ot the CAL 3 standard
. calibration must be
%D are/no^: met for any
:tion nu.
taken and
6.10.5.3 For an acceptable continuing
measured RRF for each target/surrogate
and the mean value calculated during
within ±25.0 percent. If the criteria
target or surrogate compound, remedial
recalibration may be necessary.
6.10.6 Corrective Action
6.10.6.1 If the continuing calibration techalcal acceptance criteria
are not met, recalibrate the GC/MS instrument a&cordihjt to section
6.9. It may be necessary toy-clean the ion source/^change the column
or take other corrective ac/ionsto"~3c:h-ieve___the acceptance criteria.
6.10.6.2 Continuing calibrabionXtechrucM acceptance criteria MUST be
met before any samples or requ!Lrea\blanks are analyzed in a 12-hour
continuing calibration analytical sequencer. Any samples or required
blanks analyzed when continuing calibration criteria have not been met
will require reanalysis at no additi^ma](cost to the Agency.
6.10.6.3 Remedial/actions, \hich include but are not limited to the
following, must be talcen rf criteria are\nov met:
ating conditions;
fervent according to manufacturers
ion (approximately 0.33 ra) of the
nstruct:
Break off a
rf^~
oTuran
(in (performance of all initial calibration
required);
ter or lesser resolution:
jcale;
new continuing calibration; and
new7initial calibration curve.
January, 199z
Page D-40
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.10.7 Documentation
Reporting requirements are listed in Exhibit B. /Continuing
calibration data results are reported on Form VI/AA9V, Continuing
Calibration Data Form. Internal standard area /and retention time
shall be tabulated on Form VII-AASV.
6.11 BLANK ANALYSIS
6.11.1 Summary
6.11.1.1 To monitor for possible labotfato/y and field contamination,
laboratory method blank (LMB) and fieVd blanks are^ttracted with each
SDG and analyzed at least once in a TL2-hour analytical sequence. All
steps in the analytical procedure are p4rformed: on/the LMB using all
reagents, standards, surrogate comRound^xequipmeynt, apparatus,
glassware, and solvents that would b^vujsedi^r a/sample analysis.
6.11.1.2 An LMB is an unused, certified fi>t§r/ca^ridge assembly
which is carried through the same extraction pr&cedurexas a field
sample. The LMB extract musfi-^cfintain the same amount of. surrogate
compounds and internal standards tnat~Tts--a4ded to eacrr sample. All
field samples must- be extra\tearaRd^analyzedwirCh~-ait,associated LMB.
potential sample
process of a field
must be associated with
fhe blank cartridge is opened
through the same
ient air.
>
ards that are added to each
samples must be analyzed
6.11.1.3 A field blank is
contamination during the handli
sample. The cartridge used as a
the actual sampling process; there
with the other c
handling process as thfise us
6.11.1.4 The s^meyamount ojf
sample is addend tc/each bl/nk..
with associated planks.
t
6.11.2 Frequency
6.11.2.1 An LMB aloh^shalls^be prepared along with each batch of <20
samples atKT^STrail^be carlsied through the entire extraction,
concentration-andatialysis^proce/lures. The laboratory method blank
mustyoe affaTyze(F>afterNthe calibration standard(s) before any samples
are/anaiyzed. Whenever \n unusually concentrated sample is
en
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
5ry/reagent blank
is extracted, and
this
produce an
-arget
6.11.2.3 The laboratory may also analyze a labora
which is the same as an LMB except that no cartri
no surrogate compounds or internal standards are
demonstrates that reagents do not contain impur
ion current above the level of background nois
compound quantitation ions.
6.11.3 Procedure
6.11.3.1 Spike the blank cartridges with
compounds using the same spiking technique/4s the field samples (see
Figure D/SV-5). For the field blank, /he/three
surrogates are spiked onto the cartridge/prior t
along with the cartridges to be usedr for sampling
the LMB, all eight surrogate compounds a«^ spiked
just prior to extraction.
same amount of surr
field deployment,
bient air. For
nto the cartridges
6.11.3.2 Extract the blanks following the p^pce dulses in Section 4.
6.11.3.3 Add the internal standards to the blank extracts at the same
concentration as the field
6.11.3.4 Analyze the blank
procedures as the field sample^
6.11.4 .Calculations
The equations iu^s^c
6.11.5 Technical
6.11.5.1 All Manjfs must
section 6.11.2/on/a GC/MS
performance smecRxand in}
technical
analysis
to the blanks.
e frequency described in
:he DFTPP instrument
or continuing calibration
6.11.5.2 The percemsxreco'v
must be wLtki«—the acceptance
for each of the surrogates in the blank
.dows listed in section 6.13.5.3.
6.11.5.5 TKfexblaa
concentration g
resp>ose change (%ARC) for each of the
blank must be within ±40 percent compared
in the most recent CAL 3 analysis.
for each of the internal standards must
'ween the blank and the most recent CAL 3
ust: not contain any target analyte at a
than its CRQL and must not contain additional
Page D-42
January,1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
compounds with elution characteristics and mass spe
would interfere with identification and measuremen
analyte at its CRQL. The total level of analyt
filter/cartridge must not exceed 10 ^g. If the
along with a batch of samples is contaminated,
the entire batch of samples must be flagged
6.11.6 Corrective Action
il features that
a method
blank
Lhat was extracted
values for
6.11.6.1 If a. Contractor' s blanks do no
acceptance criteria, the Contractor mus
system to be out of control. It is t
ensure that method interferences caus
reagents, glassware, and other sampl
that lead to discrete artifacts and
chroma to grams be eliminated. If contain
source of the contamination must be
corrective measures MUST be taken and do
analysis proceeds.
itractorj
cent
irage
levate
itio
sider the analytical
's responsibility to
in solvents,
pocessing hardware
elines in gas
a problem, the
and appropriate
before further sample
nente
6.11.6.2 All samples proces»»d^wiJCh a method blankx£haj^ is out of
control (i.e., contaminated/ must be~TH»gR£d with a
6.11.7 Documentation
.Reporting requirements are l\steM fn Exhibit B. Blank results are
reported on Form I-AASV and assocratea samples are entered in Form II-
AASV, except the surrogate recoveries, which are reported on
Form IX-AASV. Intej?rtaT~?tandard area\and\retention time shall be
tabulated on Form/7II-.AASV.
6.12 LABORATORY CONTROL SAMPLES
6.12.1 Summary
The LCS isX^n inbe^nal/laboratory quality control sample designed
to assess (on an»QG-by-S$G basis) the capability of the Contractor to
mettibd listed in this Exhibit.. Table D/SV-11
kd thexcorresponding QC recovery limits.
perform the analytic
lists the^-tCS "CtwiRounds
6.12.2
6.12.
d and reported once per 12-hour analytical
with the samples in the SDG.
6.12.3.1
mixture(s) ,
F/&AD-2 cartridge spiked with the LCS spiking
according to section 6.5.6, to contain each LCS
January. 1992
Page D-43
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
compound at a concentration of 50 ^g.
6.12.3.2 Spike the LCS cartridge with the surrogate7 compounds at the
same concentration as the field samples.
6.12.3.3 Extract the LCS extract following
Section 4.
6.12.3.4 Add the internal standards to
concentration as the field sample extrac
6.12.3.5 Analyze the LCS extract folj
procedures as the field sample extra^
s of the LCS using
Eq. D/SV-11
. 13 >^lso apply to the
6.12.4 Calculations
6.12.4.1 Calculate individual compound
the following equation:
Concentration,
LCS ^Recovery = /-.
6.12.4.2 Field sample calculsti
LCS for the internal standards
6.12.5 Technical Acceptance Criteria
6.12.5.1 The LCS m
tuning, initial or/con£inuin'
acceptance criteria /ft the
6.12.5.2 The tfer
must be withi
6 .12.5.3 The
within the QC rec
6.12.5.4
valid
than
MS system meeting the
nd blank technical
d in section 6.12.2.
the surrogates in the LCS
ted in section 6.13.5.3.
2coVery for each of the LCS compounds must be
{its listed in Table D/SV-11.
between the LCS and the most recent
e internal standards must be less
ne shift between the LCS and the most recent
ich of the internal standards must be within
6.12.6.1 If^-fche teVhni/Cal acceptance criteria for the internal
standards are no'fcxmet/ check calculations and instrument performance.
Page D-44
Jamuiry. 1992
-------
Exhibit D
Semivolatile Org^nics Analysis of Ambient Air
It may be necessary to recalibrate the instrument oc^^fcake other
corrective action procedures to meet the technical/acceptance
criteria.
6.12.6.2 The laboratory may not submit data fr/m anxSDG until all the
LCS technical acceptance criteria are met. LCS contamination from
laboratory sources or any LCS analyzed not meeting ail theX^echnical
acceptance criteria will require analysis of ad/ditionalM^S ca^s^ridges
at no additional cost to the Agency.
6.12.6.3 LCS acceptance criteria MUST
samples, performance evaluation (PE) s
analyzed. Any samples or required bl
technical acceptance criteria have
of additional LCS cartridges at no
6.12.7 Documentation
Reporting requirements are listed in
Control Sample analysis data are reported on
standard area and RT shall be—tabulated on Form
surrogate recoveries are reportedi
6.13 SAMPLE ANALYSIS
t before any field
or required blanks are
en the LCS
require analysis
to the Agency.
6 . 13 . 1 Summary
The sample extract from Section^
standard
quantitated by the
6.13.2 Frequency
6.13.2.1 Befo/e
GC/MS tuning
technical a
analyzed by GC/MS and
d.
6.13.2.2 If
valid initial
analyzed
Laboratory
.SV. Internal
and
ther
calibr
'MS
6.13.
temperatu
extracts mus
the instrument must meet the
ontinuing calibration
remaining in the 12-hour time period with a
^continuing calibration, samples may be
meets the instrument performance
system under the conditions outlined in
cts must be allowed to warm to ambient
y 1 hour) before analysis. All sample
under the same instrumental conditions as
January, 1992
Page
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
the calibration standards.
6.13.3.3 Add the internal standard spiking solu/ior/to the 1.0 mL
extract to contain 40 ng/juL. For sample diluti/ns,>^dd an appropriate
amount of the internal standard spiking solution to maiiatain the
concentration of the internal standards at 4Q/ngALxin the^xiiluted
extract.
6.13.3.4 Inject 1.0
data acquisition.
of sample extract/ im?o the GC/MS, and siked injfo t/ne tot^hLsairfple extract;
recent continuing calibration or
of
vol
of
,
extract injected in microliters
l extract in microliters (;iL) ; and
the extract. If there was no
L. If the sample was diluted, the
eater th^m 1 .
''Total PCB concentration in each sample extract is obtained by
isomer group concentrations.
l£ the volum^
become^
of/ air sampled is known to the laboratory, the
**I.VJ>t
A,SVUV{RRF
Eq. D/SV-13
Page D-46
January.1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
where: V0 - volume of air sampled (m3), STP.
6.13.4.3 The equation in section 6.13.6.1 is also/us^d for
calculating the concentrations of the non-target/compounds. Total
area counts (or peak heights) from the total ioii chrsmatograms are to
be used for both the non-target compound to be/mea^ureo^-^A) and the
internal standard (Ais). Associate the nearest i^nterTsal st^qdard free
of interferences with the non-target compour
relative response factor (RRF) of one (1) is~x&o be assumea.\The vaj.ue
from this quantitation shall be qualified,/
(estimated, due to lack of a compound-sp«
"N" (presumptive evidence of presence)Vindicating the quantitative
and qualitative uncertainties associated yfith thisrnbn-target
component. An estimated concentration sjaould be/calculated for all
tentatively identified compounds as /veil as those identified as
unknowns. This estimated concentration must be calculated for all
tentatively identified compounds as wfe^l as^tnosg identified as
unknowns.
6.13.4.4 Surrogate Percent Recovery (ZR):
percent recovery using the f<;
where: Q
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
RTS =
- RTV
Eq. D/SV-16
where: RTS
RT,
retention time of the IS in the/sample: and
retention time of the IS in th/ mo^t rebejit CAL 3
analysis.
6.13.5 Technical Acceptance Criteria
6.13.5.1 All target compound concentrations'must not exceed the upfter
limit of the initial calibration range Andmo compound ion (excluding
the compound peaks in the solvent fron^) pfay satu^at^ the detector.
6.13.5.2 Internal standard response's arid reteiyfiorf' times in all
samples must be evaluated during oiCimnie&iateLy after data
acquisition. If the retention time fbr any^irite/nal standard changes
by more than 20 seconds from the latest continuing calibration
standard or CAL 3 if samples are analyzed irN^he sa^ae 12-hour sequence
as the initial calibration, the chromatographic>svsterassnust be
inspected for malfunctions, a*d^c_orrections made as^-^equared. The
SICP of the internal standairas must~Be~-ffl»nitored and evaluated for
each field and QC sample. The ^ritaxia^are descfrbdtL in detail in the
instructions for FORM VI1-AAS\L ^ternaT^ta^Kiar_dA.re/a Summary. If
the SICP area for any internal ^standard/hanges by more than a factor
of ±40 percent, the mass spectrometrlc /sys/tem must be inspected for
malfunction and corrections made ais appropriate. If the analysis of -*
subsequent sample or standard indicates 4hat the system is functionirc
properly, then correeCions^may not beNreqoired.
6.13.5.3 The per,
specified as fo
Surro
coveris
Anthracene - d10
Benz o (a) pyrene -
Nitrobenzene-ds
2 - Fluorob>ptrenyi-
p - Terph^ny1-
2,4,6Vrri)?fomop
2 - Flidorophenol
Phe/oiyd
ist be within the limits
Recovery Limits
25-150%
25-150%
25-150%
25-150%
25-150%
25-150%
10-150%
25-150%
When target cdmpojunds are below CRQLs but the spectrum meets
crit/eria, report the concentration with a "J." For
if ^fcfee CRQL i/s 3/ng and concentration of 1 ng is calculated,
report
Page D-48
January. 1952
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.13.6 Corrective Action
6.13.6.1 If the sample technical acceptance crit
surrogates and internal standards are not met,
surrogate and internal standard solutions, and
It may be necessary to recalibrate the instr
corrective action procedures to meet the sur
standard technical acceptance criteria.
for the
calculations,
performance.
other
6.13.6.2 If the Contractor needs to anal^ze^more than one (1)
dilution to have all the target compounds w/thin the initial
calibration range and to have all compound/ions not saturating the
detector (excluding the peaks in the solvent fron/)/^contact SMO. SMO
will contact the Region for instructions
6.13.6.3 Sample analysis technica£saccepQmplished oy the analysis of a standard or
sample that meets jttie SI£P criteria. AXter\corrections are made, the
reanalysis of sample^analyze q^hile the^ys^em was malfunctioning is
required.
the/
6.13.6.6 If ifft
standards aref ins
problem with thefir
control of the lab^aratory
analysis with SICPs
the initlajr'ana'tvsj.s and
reanalysis/ the ?K^jireas for all internal
contract limits (±40 percent), then the
on
Exhibi
correctiv
sis is considered to have been within the
Therefore, submit only data from the
contract limits. This is considered
.st Stexjreported as such on all data
of the sample does not solve the problem,
tside the contract limits for both
CP data and sample data from both
en the initial analysis and the reanalysis
.sing the sample suffixes specified in
e SDG Narrative all inspection and
January, 1992
Page D-<+9
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.13.7 Documentation
Reporting requirements are listed in Exhibit
results are reported on Form I-AASV, Analysis D
recoveries are reported on Form IX-AASV, and
compounds (TICs) are reported on Form I-AASV-
area and RT shall be tabulated on Form VII-
6.14 PERFORMANCE EVALUATION (PE) SAMPLES
6.14.1 Summary
6.14.1.1 Performance evaluation (PE);
in monitoring laboratory performanc
informed as to which compounds are
concentrations.
Sample analysis
sheet. Surrogate
identified
>rnal standard
ssist the Agency
will not be
PE samples or the
6.14.1.2 The PE sample containing knoten concentrations of analytes is
analyzed by the laboratory to demonstrate^t^iat it^can obtain
acceptable identifications and measurements wi^h prb&edures used to
analyze environmental samples containing the samexor sitailar analytes.
Analyte and their concentra4io7is"~are~ainknown by theawfalyst.
6.14.2 Frequency
.The Laboratory shall extrac
the PE sample once per SDG, if a\
6.14.3 Procedure
6.14.3.1 The 1
cartridges from/th
instructions concerning
samples.
6.14.4
6.1
and report the results of
ples on PUF/XAD-2
come with special
ocedure required for the PE
6.14.3.2 Ext^ct >nd /onoentrate the PE sample using the procedure
described in Sec^pn 4. Add the surrogate and internal standards
solution to the PE s^mple^s^lution. Analyze the PE sample as
described--J.n Dacjion 67S
6.
DFTPP
technical a
quations necessary for calculations.
riteria
._ (ust be analyzed on a GC/MS system meeting the
calibration, and continuing calibration
iteria at the required frequency.
January. 1992
Page DoO
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.14.5.2 The PE sample must be extracted and concentrated according
to Section 4. /
6.14.5.3 The PE sample must be prepared and airialyked with a method
blank that met the blank technical acceptance/criteria^,
/ /
6.14.5.4 The percent recovery for each of
within the acceptance windows listed in se
6.14.5.5 The area response change between /the PE sample and the'supst
recent continuing calibration check standard analysis for each of the
internal standards must be within +4C/pe/cent.
6.14.5.6 The retention time shift/between the
recent CAL 3 analysis for each of^the r^tern^
within ±20.0 seconds.
PE/sample and the most
standards must be
6.14.5.7 In addition to complying with tne\PE single technical
acceptance criteria, the laboratory will be responsible for correctly
identifying and quantifying-Jjjecompounds includebKin Che PE sample.
The Agency will notify the/
6.14.6 Corrective Action
6.14.6.1 If the PE sample
internal standard and surrogates
standard solutions and instrument
recalibrate the instrument or take
to meet the techn/cal acceptance criti
6.14.6.2 Speci/Eic/lly. thfe
criteria associated with
unacceptable-^performance.
tance criteria for the
et, check calculations,
5rffl(rmance. It may be necessary to
corrective action procedures
ria.
/t meet the following
units listea in Exhibit C;
>\ >V /
Replicatfevprecisfrm within ±30 percent RSD: and
etUrt -^exyaracyb^ lessx^han or equal to 30 percent for
sin P£ sample.
SJzechnical acceptance criteria MUST be met
sorted if the PE sample is provided with the
must demonstrate acceptable performance for
id" quantification. If the Contractor fails
/technical acceptance criteria or achieves a
les-a than 75^ percent, the Agency may take, but is not limited
Lowirtg^actiions: reduction of the number of samples.
suspension of^sample shipment, a site visit, a full data audit, and/or
require the labb^toj/y to analyze a remedial PE sample. and/or a
Page D-51
January,1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
contract sanction, such as a Cure Notice.
6.14.7 Documentation
/
/
Reporting requirements are listed in Exhib/t BC Performance
evaluation (PE) sample results are reported on Form 1-v^ASV. Surrogate
recoveries are reported on Form IX-AASV.
6.15 QUALITATIVE ANALYSIS
6.15.1 Target Compounds
6.15.1.1 The compounds listed in th
Exhibit C, shall be identified by a:
interpretation of mass spectra by
spectrum to the mass spectrum of
Two criteria must be satisfied to
Correspondence of
mass spectra.
sam
d List (TCL),
nt in the
e sample mass
;e suspected compound.
ntifications:
Elution of the sample compound at^fche sameGC relative
retention time as the standard compound., anc
ound and standard compound
6.15.1.2 PCBs are identified\and\ measured/with""~a-6pecial software
(available from Hewlett-Packard\anckFimnigan), using information found
in Table D/SV-7 and the criteria\preVentz4d in Table D/SV-4. The
intensity ratio of the two major fi^ns m the molecular cluster for
each homolog is thex^nSjttts^identifications.criteria used. A ±20 percent
range in this ratto around\:he theore\ica\ or expected value is
considered accep/tablre\vThe labeled sur^pg^tes are examined for
correct retenti/on /ime ana tneaB^snce oX/interference as shown by the
ratio of seleorted/ion abundancjas^from^^the molecular ion cluster.
6.15.1.3 TJie ictentificaltion and quantification extends from the
calibration i>c^lizrng^the/relative response factors (RRFs) for each
PCB homolog groilpswith respect to the chrysene-d12 internal standard.
The primary ion is u«fid toX^alculate a response factor with respect to
the primary—roR->of the^internaJLstandard. This response factor is
used to quantify ea«h membegenerNconcentrajCions are corrected for the different
in&trujjfental sensibivitXes of each Clx (homolog) group. This method
of/quantitation does\iot\ however, take into account the range of
?ens/tivities that may\ ocaur within a single homolog series, e.g.,
fCB isomers. Therefore, use the mean RRF
during initial/calibration or the RRF calculated in the
contl
January, 1992
Page D-52
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
NOTE: For PCB analyses with automated data
fit algorithm will produce erroneous concentrati
interp,
'etation, a linear
dfita.
qualitative
the
Lsomet groups.
ropriate
tb^two
6.15.1.4 Examine results obtained on the specj:
report (for individual components identified
quantitation report (for pesticide analytes)/an<
Individual spectra should be examined and q,
spectra acquired during calibration. Rep
significant figures.
6.15.1.5 For establishing correspondence /6f the GC relative retention
time, the same compound RRT must be w/thin ±0.06/^k^ units of the RRT
of the standard compound. For refer/encp, the standard must be run on
the same shift as the sample. If ooeliition of /interfering compounds
prohibits accurate assignment of tme saragle compound RRT from the
extracted ion current profile for tfrssorimasoy ipn. the RRT must be
assigned by using the total ion chromatb^ram .
6.15.1.6 For comparison of standard and s amp texCompoMnd mass spectra,
mass spectra obtained on the-JJontr actor's GC/MS abe^required. These
standard spectra may be usa4 foric
Contractor's GC/MS meets t
criteria. These standard spectra may
used to obtain reference relativeNrete
cation purposes , only if the
tunTrrg—t*chnical acceptance
obtained f/om the analysis
on time??"
6.15.1.7 The guidelines for quail
mass spectra are as follows:
Lve/verification by comparison of
All ions resent
intensi
s amp 1 e /s pe et rum.
standard mass spectra at a relative
LO percent must be present in the
The tfela>6ive intensifies ofx^he/inajor ions must agree within
±20A>erc>nt between/the standard and sample spectra.
(Examp-ie: tsar/an/Ion with an abundance of 50 percent in the
standaro^apectra/the corresponding sample ion abundance must
be between jQs^and 7-Q^percent.)
Ions_greateNEs.than 2^Deraent in the sample spectrum but not
resent^in theSstandarbVspectrum must be considered and
'accounted fox by\the analyst making the comparison. The
verification\roc^ss should FAVOR FALSE POSITIVE. All
compounds meeting \the identification criteria must be reported
with their s
If ^txcompound/cannot be verified by all of the above criteria,
schriical judgement of the mass spectral
interpretation/specialist, the identification is correct, then
the Conbtactoir shall report that identification and proceed
with quantification.
January, 1992
Page D-53
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
6.15.2 Non-target Compounds
respon
6.15.2.1 All non-target compounds with a
percent of the nearest internal standard shall
identified via a forward search of the NIST
Only after visual comparison of sample spectr
library searches will the mass spectral inte
assign a tentative identification. Compute,
must not use normalization routines if tho
misrepresent the library or unknown spec
other.
than 10
search
6.15.2.2 The following are guideline!
tentat
identification:
Relative intensities of mai6r ions in cfoepreference spectrum
(ions greater than 25 percent of the jnos$r abundant ion) should
be present in the sample spfectrum>
The relative intensities of the ma^jor ion-a should agree within
±20 percent. (Example: For an ion wtth anabundance of 50
percent in the standard spectra, the corr^Rsnonc^Lng sample ion
abundance should be/betweSrr-3£Uand 70 percent
Molecular ions present "in the
present in the sample\spe\trumy
Eerence spectrum should be
Ions present in the sample spectrum but not in the reference
spectrum should be revieweoL for/possible background
contaminatip*r"oT~5iresence of\coe1ivuting compounds.
Ions pre/ent/lntfae Reference sfcect)rum but not in the sample
spectrvun should be]renfiewe^i^for pq/sible subtraction from the
sample/sptfctrum because_^f babkground contamination or
coelucing compounds./DataN^vstem library reduction programs
can /sometimes cr/eat/ these discrepancies.
If, in £he techn^al judgement of the mass interpretation
spectral sp^e^alistsno valid tentative identification can be
compound snbvld be reported as unknown. The mass
:ialisbsshou^d give additional classification of
pound/^Wr possible (e.g., unknown phthalate,
'unknown hydTsocarbon, unknown acid type, unknown chlorinated
compound). rf^ a ]pr°bable molecular weight can be
\Lude it.
January,1992
rage
-------
Exhibit D
SemivoLatile Organics Analysis of Ambient Air
6.16 QUANTITATIVE ANALYSIS
6.16.1 Target Compound Quantitation
6.16.1.1 Target components identified shall be cmantiSied by the
internal standard method. The internal standard/usted, forxatAor
6.16.1.4 Sample quantitation is performed by the data processing
system for all desir€3loTts of all targe\ compounds. Target compounds
are quantified ac
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
measured
hould be
The nearest internal standard free of interferences/vshall be used.
6.16.2.2 The formula for calculating concentrations/is the same as in
section 6.13.4.1. Total area counts (or peak height's) from the total
ion chromatograms are to be used for both the
and the standard. A relative response factor/(RRF)
be assumed. The value from this quantitatiori shr«
estimated (i.e., flagged "J"). This estimated/concent
calculated for all tentatively identified eompounds
identified as unknowns. /v^
6.16.2.3 An estimated concentration stfoul6 be calculated for all
tentatively identified compounds as well/as those/^fcdentified as
unknowns. This estimated concentration/must be/reported for ten
highest tentatively identified compounds as we/1 a4 those identified
as unknowns.
January, 199^
Page Dob
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
BIBLIOGRAPHY
I
7.1 Glaser, J.A., D.L. Forest, G.D. McKee, S.A. Quave,/and/W.L. Budde, "Trace
Analyses for Wastewaters", Environ. Sci. Techno!. 15. V426,
7.2 Ballschmiter, K. and M. Zell, Fresenius Z. Anal/ Cbfem.
1980.
7.3 "Carcinogens - Working with Carcinogens", Dep^r4ystrometricN^Det4
Biphenyls as Isomer Group/". Anal. Ctiem. 57. 2*
Alford-Stevens, W.L. Budde.
^mination of Polychlorinated
V1985.
ppic^Abundance Ratios in
ss Specr.rometrv". J.. Assoc ,
7.9 Rote. J.W. and W.J/. Morris, "Use of
Identification of PoLychLorinated^ip^enyis by
Off ic. Anal. Chem. 5/(lK 188,
7.10 Methods For OrgaTs^c Cnem/cal^Analysis of Municipal and Industrial
Wastewater. U.S. Environmfe*vtal Ps^tection Agency, Environmental Monitoring
Support Laboratory, Cincinnati^ OH>^PA-600/4-82-057, July. 1983.
7.11 Method
Soil/Sedime
Protection
Cincinnati
7.12 M
Env-ironmen
Washington.
on ot'TSestfcides and PCBs in Water and
phy/Mass Spectroraetry. U.S. Environmental
Monitoring and Support Laboratory,
87\
for Evaluating Solid Waste, U.S.
ffice of Solid Waste and Emergency Response,
A6, Third /dition. November, 1990.
Page D-57
January.1992
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-la /^
CONCENTRATION OF CALIBRATION SOLUTIONS /
/ /
Concentration^ n<£/on column
Target Compound
Solution* CAL 1
plutions A and B/may be used as separate calibration mixtures
or to ipjeortion.
ng calibration.
CAL 3 is used
Acenaphthene
Acenaphthylene
Acetophenone
Aldicarb
Aldrin
Aniline
Anthracene
Bendiocarb-
Benzidine
Benz(a)anthracene
Benzo(a)Pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
Benzyl alcohol
alpha-BHC
gamma-BHC (Lindane)
p-Biphenylaraine
Bis(n-butyl)phthalate
Butylbenzylphthalate
Captan
alpha-Chlordane
gamma -Chlordane
4-Chloro- 3-methylphenol,
4-Chloroaniline
Bis(2 -chloroethoxy)mi
Bis(2-chloroethyl)e
Chlorothalonil
Chlorpyrifos
Chrysene
Dacthal (DCPA)
4,4'-ODD
4,4'-DDE
4,4'-DDT
January, 1992
Page D-58
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-la (continued)
CONCENTRATION OF CALIBRATION SOLUTIO/S
Target Compound
Solution* CAL
Diazinon
Dibenz(a,h)anthracene
Dichlorvos (DDVP)
Dicofol
Dieldrin
Diethyl Phthalate
2,4-Dimethyl phenol
DimethyIphthalate
4.6-Dinitro-2-raethylphenol
2,4-Dinitrophenol
2,4-Dinitrotoluene
Endosulfan I
Endosulfan II
Endrin
Endrin Aldehyde
Endrin ketone
Bis(2-ethylhexyl)phthalate
Fluoranthene
Fluorene
Folpet
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Hexachlorocyclopentadie^e
Hexachloroethane
Indeno(1,2,3 -c,d)pyr
Isophorone
Methoxychlor
2-Methylnaphthalene
2-Methyl phenol
4-Methyl phenol
Mirex-
Naphthalene
2-Naphthyl
2-Nitroani
t Recoramen
or mixed jus
ft CAL 3 is used for>i
id t> may be used as separate calibration mixtures
Action.
ling calibration.
January, 1992
Page D-59
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-la (continued)
CONCENTRATION OF CALIBRATION SOLUTIONS /
Concentration. Rg/on column
Target Compound
Solution* CAL 1
CAL 5
3-Nitroaniline
Nitrobenzene
4-Nitrodiphenyl
2-Nitrophenol
4-Nitrophenol
Bis(n-octyl)phthalate
Oxychlordane
Parathion
Pentachlorobenzene
Pentachlorophenol
c is/trans -Permethrin
Phenanthrene
Phenol
o-PhenyIphenol
Propoxur
Pyrene
Resraethrin
Ronnel
2,A,5 -Trichlorophenol
2,4,6-Trichlorophenol
PCB Calibration Congeners***
may be used as separate calibration mixtures
ion.
calibration.
quantitate PCBs using the special software.
January, 1992
Page D-60
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-lb
APPROXIMATE CONCENTRATION OF INTERNAL STANDARDS AND
IN CALIBRATION SOLUTIONS
Concentrat
:ATE COMPOUNDS
Compound Name
Internal Standards
1,4-Dichlorobenzene-c
Naphthalene-d8
Acenaphthene-d10
Phenanthrene - d10
Chrysene-d:2
Perylene-d12
Surrogate Compounds
Anthracene - d10
Benzo ( a ) py rene - d12
2,4,6-Tribromophenol
2-Fluorophenol
Phenol-ds
Nitrobenzene-d5
2 -Fluorobiphenyl
p-Terphenyl-du
CAL I CAL 2 /CA£ 3
40
40
40
40
40
40
Pre-sampling
Pre-sampling
Pre-sampling
40
40
40
40
40
40
200
200
200
200
200
200
200
200
January, 1992
Page D-61
-------
Exhibit D
Seraivolatile Organics Analysis of Ambient Air
TABLE D/SV-2
GC/MS OPERATING CONDITIONS
Activity
Gas Chromatographv
Column
Carrier Gas
Injection Volume
Injector Temperature
Temperature Program
Initial Column Temp.
Initial Hold Time
Program
Final Temperature
Final Hold Time
Mass Spectrometer
Conditions
Transfer Line Temper
Source Temperature:
Electron Energy:
lonization Mode:
Mass Range:
Scan Time:
J&W Scientific, DB-5 crosslinkX^' 5%
phenylmethyl /ilicone (30 m x 0.32 mm, 1.0
film l/nic)cness) o/^eauivalent
en 28-29 cm3/sec at
itless
50'
4rfe~liijL_min.
[min
0'
15\nin\ oy uotil all compounds of interest
have^
toXXnufacturer' s Specifications.
inal)
iu. full range data acquisition
(SCAN) mode
At least 5 scans per peak, not to exceed 1
second per scan.
January, 1992
Page D-62
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-3 / /
INTERNAL STANDARDS FOR SEMIVOLATILE GC/MS ANALYSIS
Naphthalene -
Acetophenone
p-Biphenylamine
Bis ( 2 - chloroethoxy) me thane
A-ChLoro-3-methylphenol
4-Chloroaniline
2, 4 -Dimethyl phenol
Dichlorvos (DDVP)
Isophorone
2 -Methylnaphthalene
Naphthalene
Nitrobenzene
Nitrobenzene -ds
2-Nitrophenol
Nitrophenols (mixed)
AcenaphChene-dio
Acenaphthene
Acenaphthylene
Diethyl Phthalate
Dimethylphthalate
2,4-Dinitrophenol
2,4-Dinitrotoluene
2 -Fluorobiphenyl
Fluorene
Hexachlorocyclopentadj/tene,
2-Naphthylamine
2-Nitroaniline
3-Nitroaniline
o-Phenylphenol
Propoxur
2,4,5-Trichloronfreno
2 .4 , 6 - Tr ibromopneno.
2 .4 , 6 -
. 4-Pichlorob4nzefre-d;.
Aldicarb
Aniline
Benzyl
Bis(2-
2-FluoCro-
Aldrin
alpha-BHC
gamma-BHC (Linda
yl)phtKalate
zylphthalate
ro- 2 - methylphenol
Enddlteifan I
rinthene
Folpet
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Oxychlordane
4-Nitrodiphenyl
Parathion
Pentachlorobenzene
Pentachlorophenol
Phenanthrene
Polybrominated biphenyls
Ronne1
January, 1992
Page D-63
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-3 (continued)
INTERNAL STANDARDS FOR SEMIVOLATILE GC/MS ANALYSIS
Chrvsene-d1
Benzidine
Benzo(a)anthracene
Bis(2 -ethylhexyl)phthalate
alpha-Chlordane
gamma-Chlordane
Chrysene
4,4'-DDD
4,4'-DDE
4,4'-DDT
13C12-4,4' -DDT
Dicofol
Dieldrin
Endosulfan II
Endrin
Endrin Aldehyde
Me thoxychlor
cis/trans-Permethrin
Pyrene
Resmethrin
p-Terphenyl-dn
Monochlorbbiphenyls
Dichlorobiphenyls
Trichlorobiphenyls
Tetrachlorobiphenyls
Pentachlorobiphenyls
Heptachlorobiphenyls
Hexachlorobiphenyls
Oc tachlorobiphenyls
Nonachlorobiphenvls
Decachlorobiphenyl
Pervlene-d--
Benzo(a)p)
Benzo (a) i
Benzo
Benzc
Ben2
January, 1992
Page D-64
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
PCB Isomer Group
TABLE D/SV-4
PCB CONGENERS USED AS CALIBRATION ST
Congener Number3
Concentration Calibration Standard
Monochlorobiphenyl
Dichlorobiphenyl
Trichlorobiphenyl
Tetrachlorobiphenyl
Pentachlorobiphenyl
Hexachlorobiphenyl
Heptachlorobipehnyl
Octachlorobiphenyl
Nonachlorobiphenylb
Decachlorobiphenyl
'' Numbered according to the system of Ballschmiter^Tn4-Z£j].(see secfioiT3r?T-Ciiation 2).
b Decachlorobiphenyl is used as the calibration congenerfor botiTnoiJ>a-aadjJecachkyx)biphenyl isomer groups.
,5
,4,6
' ,3,4.5'
2'4,4',5,6'
2,2'3,4',5,6,6'
2,2'3.3',4,5',6,6'
1,4,4',5,5',6,6'
January, 1992
Page D-65
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-5
DFTPP KEY IONS & ION ABUNDANCE CRITERIA
Mass
51
68
69
70
127
197
198
199
275
365
441
442
443
Ion Abundance Criteria
30-80% of mass/L98/
Less than 2%/ofxmass
Present
Less than £%
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-6
RELATIVE RESPONSE FACTOR CRITERIA FOR INITIAL
CALIBRATION OF SEMIVOLATILE TARGET CO
CONTINUING
DUNZ5S
Semivolatile
Compounds
2-Methylnaphthalene
2-Methylphenol
2-Nitrophenol
2,4-D ime thyIpheno1
2,4-Dinitrotoluene
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
4-Chloro-3-methylphenol
4-MethyIpheno1
Acenaphthylene
Acenaphthene
Anthracene
Benz(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
bis(-2-Chloroethoxy)methane
bis(-2-Chloroethyl)ether
Chrysene
Dibenzo(a,h)anthracene
Fluoranthene
Fluorene
Hexachlorobenzene
Hexachloroethane
Indeno(l,2.3-cd)pyren
Isophorone
Naphthalene
Nitrobenzene
Pentachlorophefiol
Phenanthren<
Phenol-ds
Pyrene
Terphenylf-d
Minimum
RRF
Januarv, 1992
Page D-67
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-6 ^
RELATIVE RESPONSE FACTOR CRITERIA FOR INITIAL ANDX CONTINUING
CALIBRATION OF SEMIVOLATILE TARGET COMPOUND^'
(continued) /
Semivolatile
Compounds
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benz(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,2,3-cd)pyrene
Dibenz(a,h)anthracene
Benzo(g,h,i)perylene
Minimum
RRF
0.700
1.300
0.800
0.900
0.700
0.70
0.6
0.60
800
0.700
0.700
0.700
January, 1992
Page D-68
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-7
QUANTITATION, CONFIRMATION, AND INTERFERENCE CHECK/IOP
INTERNAL STANDARDS, AND SURROGATE COMPeKJNt
FOR PCBs,
Analyte/
Internal Std
PCB Isomer Group
Clz
C13
ci«
C15
ci6
C17
C18
C19
Clio
Quant.
Ion
188
222
256
292
326
360
394
430
464
498
Confirm
Ion
190
224
258
290
324
362
396
428
466
500
Expected
Ratio3
Internal Standard (IS)
Chrysene-d12 240
* Ratio of quantitation ion to confirmation ion
January. 1992
Page D-69
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-8
CHARACTERISTIC IONS FOR SURROGATES AND INTERNAI/ S
•ARDS
Classification
Surrogates
Phenol-d5
2-Fluorophenol
2.4,6-Tribromophenol
Nitrobenzene-d5
2 -Fluorobipheny1
p-Terphenyl-d14
Anthracene-d10
Benzo(a)pyrene-d12
Internal Standards
1,4-Dichlorobenzene-d4
Naphthalene-d8
Acenaphthene - d10
Phenanthrene-d10
Chrysene - d.12
Perylene-d12
Primary Ion
Secondary
115
68
162, 160
94, 80
120, 236
260. 265
J.-inuarv. 1992
Page D-70
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-9
QUANTITATION IONS FOR TARGET COMPOUNDS
TARGET COMPOUND
Acenaphthene
Acenaphthylene
Acetophenone
Aldicarb
Aldrin
Aniline
Anthracene
Bendiocarb
Benzidine
Benz(a)anthracene
Benzo(a)Pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
Benzyl alcohol
alpha-BHC
gamma-BHC (Lindane)
p-Biphenylamine
Bis(n-butyl)phthalate
Butylbenzylphthalate
Captan
aIpha-Chlordane
gamma -Chlordane
4-Chloro-3-methylphen<
4-Chloroaniline
Bis (2 -chloroethoxy)ijfetha
Bis(2-chloroethyl)eth
Chlorothalonil
Chlorpyrifos
Chrysene
Dacthal (DCPA
4.4'-ODD
4.4'-DDE
4,4'-DDT
Diazinon
Dibenz(
Dichlorvos'
Dicofol
Dieldrin
Diethyl Phthalate
2,4-Dimethyl phenol
PRIMARY
119. 117
77,
86, 89. 58
263, 220
66, 65
179, 176
166, 223, 58, 51
229, 226
253, 125
253, 125
253, 125
138, 277
253, 125
107, 79
181, 109
181, 109
168, 170
150,104
9.1. 206
77. 149
375, 377
375. 377
144. 142
129
95. 123
63. 95
264, 268, 109, 124. 133
97, 199, 125. 258
226, 229
45. 44, 142, 221
237, 165
248. 176
237, 165
179, 199, 93. 97
139, 279
79, 185, 187, 202
141, 250, 75, 140
82, 81
177, 150
121, 122
111,
January, 1992
Page D-71
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-9 (continued)
QUANTITATION IONS FOR TARGET COMPOl
TARGET COMPOUND
DimethyIphthalate
4,6-Dinitro-2-methylphenol
2,4-Dinitrophenol
2,4-Dinitrotoluene
Endosulfan I
Endosulfan II
Endrin
Endrin Aldehyde
Endrin Ketone
Bis(2 -e thylhexyl)phthalate
Fluoranthene
Fluorene
Folpet
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Hexachlorocyclopentadiene
Hexachloroethane
Indeno(1,2,3-cd)pyrene
Isophorone
Methoxychlor
2-Methylnaphthalene
2-Methylphenol
4-Methylphenol
Mirex
Naphthalene
2-Naphthylamine
2-Nitroaniline
3-Nitroaniline
Nitrobenzene
4-Nitrodiphenyl
2-Nitrophenol
4-Nitrophenol
Bis(n-octyl)j
Oxychlordan^
Parathion
Pentachlo/rob$
Pentachl
cis/trans^germet
Phenanthrene
o-PhenyIphenol
Propoxur
PRIMARY
1/49
115
291
250
266
183
178
170
110
57, 87, 117. 149. 121
109, 97, 155, 137. 139
252. 248
264, 268
179, 176
169, 168, 141, 115
111, 41. 43, 81
January. 1992
Page D-72
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-9 (continued) / /
QUANTITATION IONS FOR TARGET COMPOUNDS
TARGET COMPOUND
Pyrene
Resmethrin
Ronnel
2 , 4 , 5-Trichlorophenol
2 .4 . 6-Trichlorophenol
PCB Calibration Congeners
C12
C13
ci«
Cls
C16
C17
C18
C19
Clio
PRIMARY
119, 93, 79, 57,
198, 200
198. 200
189, 190
224, 223, 225
258. 260, 257
4, 296, 291
'8, 324, 330
58, 364, 361
398, 392, 400
426, 434, 431
, 466, 468, 460)
500, 496, 502, 494, 504
Congener Number
January. 1992
Page D-73
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
m/z
KNOWN RELATIVE
Relative
Intensity
TABLE D/SV-10 ~^^
ABUNDANCES OF IONS IN PCB MOLECULAR IQ/ CLUSTERS
/ /
Monochlorobiphenyls
188 100
189 13.5
190 33.4
192 4.41
Dichlorobiphenyls
222 100
223 13.5
224 66.0
225 8.82
226 11.2
227 1.44
Trichlorobiphenyls
256 100
257
258
259
260
261
262
263
13
98.
13
32
4
3.
0.
.5
.6
.2
.7
.31
.73
.47
Tetrachlorobiphenyls
290
291
292
293
294
295
296
297
298
76.2
10.3
100
13.4
49 .4
6.57
11.0
1.43
0.95-
m/z
Relative
Intensity
Hexachlorobipheny
Heptachlorobi
392 43
Relative
Intensity
hlorobiphenyls
426
42\7
428
42/9
4/30
/31
/432
33.4
4.51
87.3
11.8
100
13.4
65.6
tonachlorobiphenyls
460
461
462
463
4)B4
/65
466
467
468
469
470
471
472
473
474
26.0
3.51
76.4
76.4
100
13.4
76.4
10.2
37.6
5.00
12.4
1.63
2.72
0.35
0.39
Decachlorobiphenyl
494
495
496
497
498
499
500
501
502
503
504
505
506
507
508
509
20.8
2.81
68.0
9.17
100
13.4
87.3
11.7
50.0
6.67
19.7
2.61
5.40
0.71
1.02
0.13
January, 1992
Page D-74
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
TABLE D/SV-11
LABORATORY CONTROL SAMPLE COMPUNDS/
Target Compound ^Recovery PC Aimit
Bendiocarb
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzyl alcohol
Butylbenzylphthalate
Bis(2-chloroethoxy)methane
Bis(2-chloroethyl)ether
Decachlorobiphenyl
Diazinon
Dibenz(a,h)anthracene
Dicofol
Diethyl Phthalate
2,4-Dimethyl phenol
Endrin
Endrin ketone
Fluoranthene
Fluorene
Folpet
Hexachlorocyclopentadiene
Hexachloroethane
Indeno(l.2.3-c,
2-Methylnaphth^len.
2-Methyl phepfol
3-Nitroanilj
Nitrobenze
4-Nitrop
Nonachl
Pentachlo^aoheno
NOTE: Per&snt Reb«cvery Limits are hot established at this time. The appropriate
values shall f>^ det&ryjiined f/om/multi-laboratory studies conducted under SAS
analyses.
January. 1992
Page D-75
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
Figure D/SV-1. Sampling Head Configuration for Semivolatiles
Protective
Cap
January, 1992
Page D-76
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
Figure D/SV-2. Configuration of the PUF/XAD-
65mm x 125mm
GLASS
CYLINDER
9 9 o e
o e o
smzmmm
50mm PUF
Plug
Suppo
Scree
V/ W V/ X/ \/ W A
r"10mmXAD-2
SorbentBed
25mm PUF
Plug
January, 1992
Page D-77
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
Figure D/SV-3. Analytical Scheme for the Analysis
Air Flow
ivolatiles
3 Pre -sampling
surrogates spiked
prior to field
deployment
^
Soxhlet Bxtr\ctionwit
10 percent dieXhyI\ether/h6xane
A..Y. Z
K-D EjwfiQrator witnsMacro Column
Nitrogen qilowdowiy
cro-Snyder Column
Internal Standards
GC/MS
Analysis
January, 1992
Page D-78
-------
Exhibit D
Semivolatile Organics Analysis of Ambient Air
Figure D/SV-4. GC/MS Calibration and Analysis Schemati/ Diagram
GC/MS Tuning with DFTPP Instrument Performance Check
(at start of the analytical sequence/ every I^xh°
Initial Calibration
(upon contract award; after
major equipment changes;
failed continuing calibration)
• RRFs • Y_for ISs • RRT
• %RSD • RT for ISs • RRTs
• %ARC • RTS for ISs
Continuing Calibration
(every r^-hour period)
• Surroga
%ARC
• RTS i
• Target Anal
le Analysis
for ISs
• LQS Compound Recoveries
Samples
• Surrogate Recoveries
C for ISs • RTS for ISs
Prformance Evaluation (PE) Samples
/ /(once per SDG, if available)
Recoveries • %ARC for ISs
• RTS for ISs
• Surrogate Recoveries
January, 1992
Page D-79
-------
i
0)
0)
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QUALITY ASSORANCE/QUAOTYXJONTRO:
January, 1992
-------
EXHIBIT E
QUALITY ASSURANCE/QUALITY CONTROL REQUIREMEB
TABLE OF CONTENTS
SECTION 1 INTRODUCTION / / E'1
SECTION 2 QUALITY ASSURANCE PLANS /./...././ E-4
SECTION 3 STANDARD OPERATING PROCEDURES ./. .X. . • / •/ E-7
SECTION 4 CHAIN-OF-CUSTODY ^^XJ ' ' ^ E"14
SECTION 5 DOCUMENT CONTROL ^X.. —Xc E-17
SECTION 6 ANALYTICAL STANDARDS REQJflREMEWCS^.. .... >X/ E-21
SECTION 7 METHOD SPECIFIC QA/QC RE^IKSMESTS-----^, . . /T7^7 E-26
SECTION 8 REGIONAL DATA REVIEW . . . \ .V ./. / E-31
SECTION 9 LABORATORY EVALUATION SAMPLES \. ./ E-32
SECTION 10 GC/MS TAPE AUDI'S . . .X . . . . \ . \ E-34
SECTION 11 ON-SITE LABORATORY EVADJA'IIONS^. . \. / E-35
SECTION 12 QUALITY ASSURANCE DATA/TRBllD~ATSALYSIs7 E-38
SECTION 13 DATA MANAGEMENTX ./../. E-40
SECTION 14 REFERENCES
January, L992
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 1
INTRODUCTION
1.1 Quality assurance (QA) and quality control (QC) are 4Titegr-aJ parts of
EPA's Contract Laboratory Program (CLP). The CLP QA/prograiiKconsts^s of
management review and oversight at the planning, implenrentatiortxand
completion stages of environmental data generationSscjzivities,
data provided are of the quality required. The CLPjQC program includeX.thoi
activities required as part of data generation yo e/isure that the data are^/faf
known and documented quality.
1.2 During the planning of an environmental
activities focus on defining data quality
designing a QC system to measure and docun
generated. During the implementation of ttw
activities ensure that the QC system is functiot
deficiencies uncovered by the QC system are identil
environmental data are generated, QA activities focus
of data obtained to determine its sv^i£ab_ility to support
remedial decisions.
program, QA
iteria, and
of data that will be
ion effort, QA
tively, and that the
orrected. After
ing the quality
'ment or
1.3 The purpose of this Exhibit is X° <3^scril
and the processes by which the CLP meets
This contract requires a variety of QA
requirements are the minimum QA/QC operation
analytical requirements associated with the\det<
method analytes. These opej^fitfTotts. are desigHed
comparison by providing ttie EPA with\ comparab
These requirements do nol: re/feasevtha laborato
checks on method and in/trument peVformanc
:he_D^verall/QA/QC operations
'QC/objectTlCves defined above.
it/es. These contract
essary to satisfy the
rmination of the different
facilitate laboratory
from all Contractors.
from maintaining its own QC
1.4 Appropriate usey6f
conditions encountered
procedures and critei
contract have been valic
(ata genetatsf'd undexthe/great range of analytical
air analysesrequires reliance on the QC
*d into the methods. The methods in this
bnples typical of those received by the
laboratories participating'rs^the oLP. However, the validation of these
methods does not^guarantee thatX^iey parform equally well for all samples
collected undepractual fiebi conditions./ Inaccuracies can result from causes
such as s amp Ling vfirTtr^&ts, equipment^maifunctions , and human error .
Therefore, Jme JqC components^f each method is indispensable.
1.5 The Aa t
analytic/1 r
acquired from QCprdcedures are used to estimate and evaluate
ults and to determine the necessity for or the effect of
The means/used for evaluating the analytical results
include quanbi^ative\and qualiftaGive indicators of quality such as precision,
accuracy, detection liitri^, a^d orher quantitative and qualitative indicators.
In addition, QC dataNgivean overview of the activities required in an
January, 1992
Page E-l
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
integrated program to generate environmental data of known,
quality required to meet defined objectives.
ind/documented
1.6 Necessary components of a complete QA/QC program isCclud^internal QC
criteria that demonstrate acceptable levels of performanca^as oejermined by
QA review. External review of data and procedures is/acpomptishedTS^f the
monitoring activities of the National Program Offic
Sample Management Office, NEIC, and EMSL/LV. Each
accomplishes a different purpose. These reviews
sections of this Exhibit. Performance evaluatioil s
QA reference for the program. A laboratory on-sit
gional
rnal review
.escribed in spec'il^.c
iples provide an external
evaluation system is also
part of the external QA monitoring. A feedback Ipop provifde^ the results of
the various review functions to the contract Aabpratorie/ through direct
communications with the Administrative Project pfficers/(Apt)s) and Technical
Project Officers (TPOs).
1.7 This Exhibit is not a guide to constructing^-QA project plans, QC systems,
or a QA organization. It is, however, an explanatio^v^of the^QC and QA
requirements of the CLP. It outlines some minimum standards ffcr QA/QC
programs. It also includes specific/itemsthat are require^sin TSL QA Plan and
by the QA/QC documentation detailed/in this~"cTm€*ac_t_. Delivery of this
documentation provides the Agency with ^&eac].ete data~^acfc*gB which will
stand alone, and limits the need for\pncect witt&th/a^Qontra/tor or with an
analyst, at a later date, if some aspec\ oBythe/analysis is questioned.
1.8 To ensure that the product delivered
requirements of the contract and to improve'
the Agency requires the fol]
1.8.1 Development a
of the key elements
described in Secti
1.8.2 Preparati
Procedures (SOPs)
1.8.3 Adherence to the
specified in
ontractor meets the
laboratory data comparison,
tor.
1.8.6 Partic^iRatio
adherence to
gram, and documentation
,gh\6 written QA Plan, as
Ice to written Standard Operating
Section 5 of this Exhibit.
1 methods and associated QC requirements
tical Thjjfodards and documentation of the
he purity and accuracy of solutions obtained
llysis of laboratory performance evaluation
,ce to corrective action procedures.
n o/i-sfte laboratory evaluations, including
ct/on procedures.
January, 1992
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
1.8.7 Submission of all raw data and pertinent documentation for Regional
review.
1.8.8 Submission, upon request, of GC/MS tapes and
documentation for tape audits.
1.8.9 Submission for Agency review of all origi^
generated during sample analyses.
January, 1992
Page E-3
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
)rogramxshall
SECTION 2
QUALITY ASSURANCE PLANS
2.1 The Contractor shall establish a QA program with/th?
providing sound analytical chemical measurements.
incorporate the QC procedures, any necessary correcfri^ action,
documentation required during data collection as weljfras the quality
assessment measures performed by management to eysurfi acceptable data
production.
2.2 As evidence of such a program, the Contractor shall/prepare a written
Quality Assurance Plan (QAP) which describes/th^; procedures/that are
implemented to achieve the following:
2.2.1 Maintain data integrity, validity, anbxusability.
2.2.2 Ensure that analytical measurement systems at
acceptable state of stability an
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
Reporting relationships.
Personnel;
Staff resumes;
Education and experience requirer
Contract; and
Training progress.
Facilities and Equipment;
Instrumentation and backi.
Maintenance activities/and'
Document Control;
Laboratory notebook policy;
Sample and data
documentation
Logbook maintenance and archfS
and storage procedures;
aration procedures.
Case file organization^,
procedures; and
/* ^
Procedures for
and dtstwtbution
ation, and review
roval, review, revision,
Analyti
procedures;
ifon procedures ;
January, 1992
Page E-5
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
Data review procedures;
Data reporting and authorization
Data management procedures.
Quality Control Program; and
Solvent, reagent, and adsorbe^
Reference material analysis
Internal QC checks; and
Corrective action and petei
procedures.
Quality Assurance Program Assessmer
Data audits;
Systems audits ;S
Performance audits
Corrective action proVeduYes/ and
- QA
January, 1992
Page E-6
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 3
STANDARD OPERATING PROCEDURES
3.1 In order to obtain reliable results, adherence t
methodology is imperative. In any operation that is
basis, reproducibility is best accomplished through
Operating Procedures (SOPs). As defined by the
document that provides directions for the step-
operation, analysis, or action which is commonly''accepted as
performing certain routine or repetitive tasks
3.2 SOPs prepared by the Contractor must be
comprehensive, up-to-date, and sufficiently/de
results by qualified analysts. All SOPs, a,
reflect activities as they are currently perf'
addition, all SOPs must:
3.2.1 Be consistent with current EPA regulations, gu
contract's requirements;
clear,
;• duplication of
'the Agency, must
laboratory. In
and the CLP
3.2.2 Be consistent with instrx.
manuals;
jrer's specific instruction
3.2.3 Be available to the EPA duringNan ISiyf-Sifte Laboratory Evaluation. A
complete set of SOPs shall be bound togVther/and available for inspection
at such evaluations. Duri»g-Qn-Site evaluations, laboratory personnel may
be asked to demonstrate/the application of\j:he\SOPs;
3.2.4 Provide f or
complete to record
3.2.5 Describe
reported by the
inconsistent results
3.2.6 Describe the correct
analytical r/*sults
3.2.7 Be/re
facilit
fice of alP
^ that is sufficiently
isks" required by the protocol;
3.2.9
ing the validity of data
tplaining the cause of missing or
ires and feedback mechanism used when
requirements;
updated as necessary when contract,
ral modifications are made;
ference in usability or evidentiary
work stations as appropriate; and
January, 1992
Page E-7
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
3.2.10 Be subject to a document control procedure whic
of outdated or inappropriate SOPs.
3.3 SOP SPECIFICATIONS AND FORMAT
recludes the use
3.3.1 An SOP is defined as a written narrative
of laboratory operating procedures including ex
documentation. The SOPs must accurately descri
used in the laboratory, and copies of the wricte
to ensure that analytical data produced unde/ t'
for use in EPA enforcement case preparation/an
cription
ratoi
ipliss of la
:he actual
SOPs shall be
s contract are accep
litigation. The
Contractor's SOPs shall provide mechanisms/and! documerft^
of the following specifications and shaly be/used by/EP^
laboratory evidence audits.
accountabil
followi
ion to meet each
sa the basis for
3.3.2 The format for SOPs may vary depehon tKe kind of activity
for which they are prepared. However, at a'mjjiimum^the following
sections must be included.
3.3.2.1 Title page.
3.3.2.2 Scope and applicat'
3.3.2.3 Definitions.
3.3,2.4 Procedures.
3.3.2.5 QC accepta
3.3.2.6 Corrective
secondary revie
3.3.2.7 Docugfen
3.3.2.8 Misc
3.3.2.9 References^
3.4 REQUIRED
3.4.1
'informa'
Sample forms.
>fote6 and precautions.
ing procedures for
ted.
samp
proce
Contractor
p and use adequate written SOPs to ensure
Evidentiary SOPs shall include specific
ocesses as they are performed by the
January, 1992
Page E-8
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
3.4.1.1 Sample receipt and logging
3.4.1.1.1 The Contractor shall have written
and logging in the samples. The procedures
documentation of the following information^
Presence or absence of EPA chain-
Presence or absence of airbill
Presence or absence of EPA T
lists;
Presence or absence of cv
sample containers and tt
Custody seal numbers,
Presence or absence of sample
• . Sample tag ID numtiejrs;
Conditi-on of the
• Condition of the
for receiving
include,
Verification of agree
on receiving documents
Resolu/ion of pr
onagreement of information
.mple containers;
pancies with SMO: and
to describe sample
3.4.1.2
lave a designated sample
[e for receipt of samples and have written
duties and responsibilities.
shall have written SOPs for
sification of EPA samples throughout the
Dntractor assigns unique laboratory
SOPs shall include a description of the
/ign the unique laboratory identifier and
the EPA sample number.
January, 1992
Page E-9
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
3.4.1.2.3 If the Contractor uses prefixes tor
addition to sample identification numbers/ tt
shall include their definitions.
suffixes in
written SOPs
3.4.1.3 Sample security
. The Contractor shall have writt
the security of samples after log-i'
security of the sample storage a
shall specifically include descript:
for EPA samples in the laborato/ry ,/and ste
sample contamination. The SO!
authorized personnel who havi
Ps for maintenance of
d shall dem&Rstrat
Moratory areas . :Ehe SC
fens of all storage art
s taken to prevent
a list of
e storage areas.
incJ
:ess to seci
3.4.1.4 Internal chain-of-custody/of
>les And/data.
The Contractor shall have wisLtten S^Ps for the chain-of-
custody consisting of sample identrf^-catibn,. chain-of-custody
procedures, sample receiving procedurefevandsample tracking
procedures. For more^information concerning th^ chain-of-
custody procedures fee Sec
of this
3.4.1.5 Internal tracking o
The Contractor shall
performed on any particular
include the following:
OPs for tracking the work
tracking SOP shall
ion used to record sample
ransfers, sample
ation used to record
ther QA/QC activities; and
document formats and laboratory
ed in the sample receipt, sample storage,
sample analyses.
>
information control
3.4.2
^ntractor shall develop and use adequate written SOPs to ensure
data generated foy th/e CLP are of known, documented, and
AnalVtic/1 SOPs shall include specific procedures for
the followin^^procfe^ses /s tfrey are performed by the Contractor:
January, 1992
Page E-10
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
3.4.2.1 The Contractor shall have written SOPs for
contamination, during sample preparation, cleaning
storage, and analysis.
3.4.2.2 The Contractor shall have SOPs to ensu
standards used in sample analysis QA/QC.
3.4.3 Quality Management SOPs
venting sample
assware,
£eability of
3.4.3.1 The Contractor shall have writte
managerial review of laboratory operatic
preparation, laboratory data review/lab,
The procedures shall include but not b,
following information:
data package
jry self inspection system.
acumenting the
3.4.3.1.1 Data flow and chain
3.4.3.1.2 Procedures for measuring
3.4.3.1.3 Evaluation of parameters for
errors.
3.4.3.1.4 Procedures tf
complete and compliant w
3.4.3.
ass em'
'data review;
and accuracy.
systematic
liverables are
Mbit B.
.3.4.3.1.5 Demonstration of
(demonstrated by supervisory
internal PE samples, etc.).
3.4.3.1.6 Fre
quarterly, sp
3.4.3.1.7
actions,
resultin
inspection procedure
on personal notebooks,
audits (e.g., random,
areas).
ot^problebsjdentification, corrective
of: analy^caV processing. Sequence
£udit (i.eTr QA feedback).
3.4.3.1.8 daymen t!ati6n of audit reports, (internal and
external), response, cbvjrective action, etc.
shail hav& written SOPs for organization and
jcumehps relabij^g to each EPA Case, including .
vreview. Documents shall be filed on a Case-
lures must ensure that all documents
logbook pages\ simple tracking records. chromatographic
computer printouts, raw data summaries, correspondence, and
anyiothels^written documents having reference to the Case are compiled
in cmteslocabi^m for supmis'sion to EPA. The system must include a
documentNiumberiqe ana inventory procedure. For more information
January, 1992
Page E-ll
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
concerning document control and case file preparati
of this Exhibit.
3.4.3.3 The Contractor shall have written SOPs
management and handling, and reporting of data
include but not be limited to documenting the/fo
3.4.3.3.1
errors.
Procedures for controlling a
ee Section 5
iample analysis,
shall
>rmation:
3.4.3.3.2 Procedures for reviewing/changes to data and
deliverables and ensuring traceabil
3.4.3.3.3 Life cycle management/prc/cedures/for,
and implementing changes to exiting
hardware, software, and documentation
testing, modifying
systems including
new systems.
3.4.3.3.4 Database security, backup
including recovery from system failures.
3.4.3.3.5 System maintenance"
4lling
archival procedures
and
3.5
3.4.3.3.6 Individual(s)
maintenance, data integrity^ arifc
3.4.3.3.7 Specifications for
3.4.3.4 The Contractor—sfe^ll have
HANDLING OF CONFIDENTIAI
for.
Astern
raining procedures.
SOPs for laboratory safety.
3.5.1 A Contractor/conducting ^orkj.mder^6iiis contract may receive EPA-
designated confidential information frol&^the .Agency. Confidential
information must/foe handled sepairately froBr-other documentation developed
under this contra^. TbXacoompJiish this, the following procedures for the
handling of confidential into rinat ion have been established.
3.5.2 All confid«iit;Lal docusentsshall be under the supervision of a
designated JXJcument CorTs^ol Ofr^er
3.5.3 A
confide
file s,
from
samp
informal
Log. The inJxmnat?
only after it h
documents shall be
fion received with a request of
d as "confidential." A separate locked
re this information and shall be segregated
latioh. Data generated from confidential
idential. Upon receipt of confidential
.esfe documents into a Confidential Inventory
enrmade available to authorized personnel but
out to that person by the DCO. The
to the locked file at the conclusion of each
January, 1992
Page E-12
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
working day. Confidential information may not be repr
approval by the EPA Contracting Officer. The DCO will
into the document control system. In addition, this
be disposed of except upon approval by the EPA Contr
DCO shall remove and retain the cover page of any
disposed of for one year and shall keep a record q,
Confidential Inventory Log.
iced except upon
?r all copies
tmation may not
Officer. The
information
in the
3.6 SOPS DELIVERY REQUIREMENTS
Within forty-five (45) days of contract
SOPs .relevant to this contract shall be ser
Also, during the term of performance of tt
have been amended or new SOPs which have,
TPO, EMSL/LV (quality assurance SOPs) 35
ec^ipt, a complete set tfl
the TPO, SMO and EMSL/LV.
ies of SOPs which
be sent to the
lary SOPs).
(all
January, 1992
Page E-13
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 4
CHAIN-OF-CUSTODY
A sample is physical evidence collected from a
environment. An essential part of hazardous waste i
that the evidence gathered be controlled. To acco
sample identification, chain-of-custody, sample
procedures have been established.
4.1 SAMPLE IDENTIFICATION
4.1.1 To ensure traceability of sample
Contractor, the Contractor shall have
identification of samples throughout the
4.1.2 Each sample and sample preparation
the EPA number or a unique laboratory identifier.
identifier is used, it shall be cycass-referenced
4.2 CHAIN-OF-CUSTODY PROCEDURES
to
Because of the 'nature of the data being dolYectesT, die custody of EPA
samples must be traceable from the time \he/sainples are collected until
they are introduced as evidence in legfcl proceedings. The Contractor
shall have procedures ensuring that EPA^saropde custody is maintained and
documented. A sample is^ofiHer^ustody if\the\following applies:
4.2.1 It is in yy
4.2.2 It is in/yowfr view after^heing lr«-^iour possession, or
4.2.3 It wa§r in>Qur pos/ses£ion and you locked it up, or
sion of the
for maintaining
be labeled with
ue laboratory
iumber.
4.2.4 It is 'in if
accessible to author
_/-
4.3 SAMPLE RECEIVING PROC
secure area (secure areas shall be
pnnel only).
signate a sample custodian responsible for
4.3.3 The co>kditio
be inspected upo
representative.
gnate a representative to receive samples
'stodian is not available.
yy
)f tjie shipping containers and sample bottles shall
by the sample custodian or his/her
January, 1992
Page E-14
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
A.3.4 The condition of the custody seals (intact/not i
inspected upon receipt by the sample custodian or his
4.3.5 The sample custodian or his/her representative
presence or absence of the following documents accoj
shipment.
4.3.5.1 Airbills or airbill stickers.
4.3.5.2 Custody seals.
4.3.5.3 EPA custody records.
4.3.5.4 EPA traffic reports or SAS
4.3.5.5 Sample tags.
t) shall be
epresentative.
11 check for the
.g the sample
4.3.6 The sample custodian or his/her repre
all forms (e.g., custody records, traffic
airbills) accompanying the samples at the time of
4.3.7 The Contractor shall con
problems such as absent documen
seals, and unsatisfactory sample
shall sign and date
lists, and
:eipt.
cies and
n, broken custody
sample bottle).
4.3.8 The Contractor shall record
problems on Telephone Contact Logs.
4.3.9 The following in
AADC-1 by the sample
received and inspect
4.3.9.1 Condi
4.3.9.2 Pr
shipping and
on of discrepancies and
on appropriate Form
entative as samples are
on
er.
of custody seals on
4.3.9.3 Custody seaV^numbe^s^. when present.
4.3.9.4/Conditionvo<. the staple Bottles.
4.3 .>$. 5/ Presence oivabsXnce of airbills or airbill stickers.
4/J.9/6 Airbill or airbill sticker numbers.
te of EPA custody records.
or/absnce of EPA traffic reports or SAS packing
January, 1992
Page E-15
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
4.3.9.9 Presence or absence of sample tags.
4.3.9.10 Sample tag identification numbers cros;
EPA sample numbers.
4.3.9.11 Verification of agreement or non-
recorded on shipping documents and sample c
4.3.9.12 Problems or discrepancies.
4.4 SAMPLE TRACKING PROCEDURES
The Contractor shall maintain records
handling from receipt to final analysis.
documentation of the movement of samples ai$d
designated laboratory storage areas.
erenced to the
ases of sample
include
les into and out of
January, 1992
Page E-16
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 5
DOCUMENT CONTROL
ks, chain-o^Excustc
ocuments relatirlgsto
fcntrol procedures havfc
are assembled and
from the EPA
/rds
eon reque
The goal of the laboratory document control prograrf is to^^sure that all
documents for a specified Sample Delivery Group (SDGy/wi/l&c accounted for
when the project is completed. Accountable documents used by
laboratories shall include but not be limited to loj
records, sample work sheets, bench sheets, and
sample or sample analyses. The following documei
been established to assure that all laboratory
stored for delivery to the EPA or are availab]
prior to the delivery schedule.
5.1 PREPRINTED LABORATORY FORMS AND LOGBOQ
5.1.1 All documents produced by the Contrac^fcQr whi4h are directly related
to the preparation and analysis of EPA samples stmll Become the property
of the EPA and shall be placed in the complete samp^te delivery group file
(CSF). All observations and resul£srecorded by the la^prapbry but not on
preprinted laboratory forms shall beentST*e-dL_into permanerre laboratory
logbooks. When all data from a\SDGr^«^__compiled7^3tt--ociginal laboratory
forms and copies of all SDG-relar^d i^gbooE~~57i£r/ifi_s shal/ be included in
the documentation package.
5.1.2 The Contractor shall identify She activity recorded on all
laboratory documents which is directly B^lat^d to the preparation and
analysis of EPA samplesx
5.1.3 Pre-printed latfora'fbry^forms shall co\\taili the name of the
laboratory and be daced/(month/eay7year>xand signed by the person
responsible for peyiorjning the yactpti^v at^feh^ time an activity is
performed.
5.1.4 Logbook entries stvajy be/dated (month/day/year) and signed by the
person responsible fOTv^erformang the activity at the time an activity is
performed.
5.1.5 Logb/fo'k entries'^Stiall beNLn ch^nological order. Entries in
logbooks,/with^Ehe^S>«fiT)tibo of ins^wument run logs and extraction logs,
shall injjflud* only one S^G per page.
5.1.6 /Pages in both bound ^nd \unbound logbooks shall be sequentially
numbeed.
5.1,7 InstrumeiJtsrun logs/shall be maintained so as to enable a
reconstructio
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
laboratory may exercise the option of using only
identification numbers in the logs for sample ID
agency or commercial client names to preserve the c
commercial clients.
labor.
rat
or EPA sample
lan government
of
5.1.8 Corrections to supporting documents and r
drawing a single line through the error and ent,
information. Corrections and additions to
data shall be dated and initialed. No informatin shall be
rendered unreadable. All notations shall be/re/orded in ink.
portions of documents shall be crossed out
lade by
5.2 CONSISTENCY OF DOCUMENTATION
5.2.1 The Contractor shall assign a
for the organization and assembly of the
5.2.2 All copies of laboratory documents shall
5.2.3; Original documents which
one SDG shall be filled in the
shall be placed in the other CS
following information on the copy
ORIGINAL IS FILED IN CSF
The Contractor shall
on/rol/officer responsible
^e and legible.
to more than
number. The copy(s)
11 record the
to the copy(ies).
5.2/4 Before rele
shall assemble an<
records, lab ben
relevant data t
sample delivery
5.3 DOCUMENT NUMBERING AND
document control officer
on sample tags, custody
ument logs, and other
fa pertaining to each particular sample or
throughout the CSF.
5.3.1 In
analysis
serialized
5.3.2 "fc^l do
logbook pa
records, re-
attempted analysi
be inventoried.
:countability of the completed
LtemNin a CSfshall be inventoried and assigned a
described in Exhibit B.
number (For example: 75-2-0240).
bo each sample delivery group, including
ts, Xnass spectra, chromatograms, screening
tecords, re-analysis records, records of failed or
.custody records, library research results, etc., shall
January, 1992
Page E-18
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
5.3.3 The Document Control Officer (DCO) shall be
ensuring that all documents generated are placed
and are delivered to the EPA. The DCO shall place
plastic bags in the file. Figure E-l is an exampl
inventory.
res
.ble
in
for
for
inventory
tags in
document
Figure E-l ^
/ /
Document Control #*
Example
DOCUMENT INVENTORY
Document Type
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
etc.
0001
0002
0003
0004
0005
0006
0007
0008
Case File Document Invento
Chain-of-Custody Records
Shipping Ma:
Sample Ta
SMO Organi'
Analysis
Analysts' Orga^ic\ Notet>o
GC/MS
etc.
50
10
41
14
gbook Pages 12
etc.
•«This number is to be rec
5.4 STORAGE OF EPA F
The Contractorxshal
location.
5.5 SHIPPING DA1
ntafin EPA laboratory documents in a secure
document/shipment of deliverables packages to
ts require custody seals on the containers
opened without damaging or breaking the
ument what was sent, to whom, the date, and
5.5.2 ThexCont
EPA Region
tor shaM ptfrge the CSF deliverable to the appropriate
te the report submission.
January, 1992
Page E-19
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Exhibit E
Seraivolatile Organics Analysis of Ambient Air
5.5.3 A copy of the transmittal letter for the CSF wil]
NEIC and the SMO.
5.5.4 The Document Control form is used •"> document/
inspection of shipping containers and san .:s. The
submit one (1) original FORM AADC-1 for e^eh ship]:
5.5.5 The Contractor shall sign and date the
examine the shipping containers, record the
seals and their conditions.
5.5.6 The Contractor shall note any probl€
the instructions explained in Exhibit B,
5.5.7 The Contractor shall submit a cop
each SDG package.
sent to the
receipt and
ctor shall
the^samples and follow
eet.
Control Form with
January, 1992
Page E-20
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 6
ANALYTICAL STANDARDS REQUIREMENTS
The U.S. Environmental Protection Agency will not/su
reference standards either for direct analytical me
purpose of traceability. All contract laboratories/wi,
prepare from neat materials, from cylinders of co:
NIST Standard Reference Materials.or NIST/EPA appfi:
material, or purchase from private chemical supply
necessary to successfully and accurately perfo,
protocol.
be
gases
1
sed
'ed certified
ouses those standard
e analyses required in this
6.1 PREPARATION OF CHEMICAL STANDARDS FROM7 THE NEAT
PURITY BULK MATERIAL
6.1.1 A laboratory may prepare their "fefeemicals^s'fcandards from neat
materials. Commercial sources for neat cHtemical standards pertaining to
analytes listed on the TCL are given in Appendix C oS^the "Quality
Assurance Materials Bank: Analytical Reference St^ndardsv!! Seventh
Edition, January 1988. Laboratories should obtain th^higfiest purity
possible when purchasing neat ofnemicSt—standards; standa^is purchased at
less than 98% purity -must be 6x^cuiH^a£e_d as to~why—a~higher purity could
not be obtained.
6.1.2 Neat chemical standards must
used in the preparation of standard
chemicals is essential in order to saf
ifrigerated when not being
rioBts. Proper storage of neat
them from decomposition.
6.1.3 The purity of
chemical supply hous
the concentration
laboratory's resp$
that the purity
confirmation,
calorimetry,
performance liquid
compounoXcan sometimes\be misrepresented by a
^knowledge of^ouryty is needed to calculate
hsolubi^n stajjaard, it is the contract
>ility to have_^analytica.l documentation ascertaining
compdund/is correctly stated. Purity
jcformeji, should use either differential scanning
with flame ionization detection, high
infrared spectrometry, or other
jpmatog
appropriate techniques.
rec ommended .^^Hw—sojrrectiJ
materials /in the preparation 61
—N«
impure^
^two or more independent methods is
for impurity when weighing neat
lion standards is:
ft. of pure compound
, percent purity*
100
Eq. E-l
volume
so
pure compbunfl" is that required to prepare a specific
;ion stanaarjd of a specified concentration.
January. 1992
Page E-21
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
6.1.4 Mis-identification of compounds occasionally occurs/and it is
possible that a mislabeled compound may be received from/a chemical supply
house. It is the contract laboratory's responsibility eo have analytical
documentation confirming that all compounds used in/thek^reparation of
solution standards are correctly identified. Identification confirmation,
when performed, should use GC/MS analysis on at ^eas/cfcHp
analytical columns, or other appropriate techniques
6.1.5 Calculate the weight of material to b«
volume taking into account the purity of th<
concentration. A second person must verify
calculations. Check balances for accuracy
All weighing should be performed on an
0.1 mg and verified by a second person./
solute should be compatible with the
be used; the solute should be soluble,
solvent. In the case of a multicomponent
not react with each other.
ghed out for a
ound and the desiret
accuracy of the
standard weights.
e to the nearest
to dissolve the
the standard is to
mreactive with the
;ution^ the components must
6.1.6 Log notebooks are to be kejjt: for all weighing^md dilutions. All
subsequent dilutions from the p/rima:ry~~"S"fcan4aj:d and the calculations for
determining their concentrations a^a-«tc^be recor
-------
Exhibit E
Semivolatile Organics Analysis of Ambient Air
results for the high standard and low standard are consistent with the
difference in theoretical concentrations. This is/dope by the
Student's t-test in part 6.3.1.3 which follows.
the supplier must then demonstrate that the cone
lis is achieved,
Nation of the
target standard lies midway between the concentrations of the low and
high standards. This is done by the Student's7 t-
is certified to be within 10 percent of the garget
The standard
ipncerttration.
6.2.1.3 If the procedure above is used, mesupplier mus
that the following have been achieved.
Two solutions of identical concentration must be prepared
independently from neat materials/ Mi aliquo/f^f the first
solution must be diluted to the ^nterided concentration (the
"target standard"). One aliquo,
and diluted to a concentration/ten^percentf gr/eater than the target
standard. This is called the ^high s tSQdaror. One further
aliquot is taken from the second s&iution amd diluted to a
concentration 10 percent less that the^t^argetXs^tandard. This is
called the "low standard";
; the second solution
Six replicate analyses
must be performed in t.
high standard, low stan*
The mean and variance of th
calculated.
Me.
Variance/^
The value
analyses of
standards are
vari
V
iard (a totar>s/f 18 analyses)
2wing sequerTC-e--—l^w__ standard, target,
standard; and
r^su/ts for each solution must be
Eq. E-2
Eq. E-3
represent the results of the six
The means of the low, target, and high
, M2, and M3, respectively. The
and high standards are designated
Additionally, a pooled variance,
Page E-23
-------
Exhibit E
Semivolatile Organics Analysis of Ambient Air
Eq. E-4
If the square root of Vp is less than o/ie percent'
M22/10,000 is to be used as the value
calculations.
The test statistic must be calculated
If the test statistic exceeds 2.13 thet
demonstrate a twenty percent difference be"i
standards. In such a cas^^ the standards are""
The test statistic mus
TARGET STANDARD = M.± (2 . 13 ) ( —£ )
6
NTERNAL FOR/HI Oft STANDARD =
Eq. E-5
lier has failed to
.e high and low
ceptable.
Eq. E-6
If the test s
demonstrate
between the,
are not a
The 95
standard"
:eeds 2.l!k tlte supplier has failed to
garget standard co/ioentration is midway
Lstand>*rds _ \y\ such a cr.se. the standards
for the mean result of each
Eq. E-7
Eq. E-8
Eq. E-9
These rht^rvatV must not overlap. If overlap is observed, then
the supplietxhas /tailed to demonstrate the ability to discriminate
January, 1992
Page E-24
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
the 10 percent difference in concentrations. In,such a case, the
standards are not acceptable. In any event, tjie^aboratory is
responsible for the quality of the standards /employed for analyses
under this contract. / /
6.3 REQUESTING STANDARDS FROM THE EPA STANDARDS REPOSITORY
Solutions of analytical reference material
U.S. EPA Chemical Standards Repository, depen
Contractor can place an order for standards
these standards are not available from comme'rcj
solution or as a neat material. /
' cart be ordered Ts^>m
on availability.
after demonstrs
I vendors either in"
6.4 DOCUMENTATION OF THE VERIFICATION AND PREPARATION
itory t/
.stano
thexrequirements
It is the responsibility of each Yabo
documentation to show that the chemica
performance of CLP analysis conform to
Weighing logbooks, calculations, chromatogram
produced by the laboratory or purchased from che
be maintained by the laboratory and may be subject
m.
mas:
standards
on-site inspection visits. Do
required to be sent to EPA fo
those cases where the documenta"
results of data packages sent toNjPAV such
file by the laboratories for a per\od\f one /year.
1ICAL STANDARDS
intain the necessary
ey have used in the
previously listed.
ectra, etc, whether
houses, must
during
Daration may be
compliance. In
analytical
is to be kept on
January, 1992
Page E-25
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 7
METHOD SPECIFIC QA/QC REQUIREMENT;
7 1 The purpose of this section is to outline the minimum quality control
(OC) operations necessary to satisfy the analytical
with the determination of the semivolatile organic
C. using the procedures in Exhibit D. This sectij
comprehensive quality control document, but
OC operations that must be addressed during i
on PUF/XAD-2. The laboratory is expected to
; :.p.-iring the quality assurance plan and Star
in Sections 2 and 3.
rathe
7.2 The specific QC operations that must
oi'ganics analysis include the following:
7.2.8.1 As par
-------
Exhibit E
Semivolatile Organics Analysis of Ambient Air
> ensn
meets the instrument performance criteria specified in
purpose of this instrument performance check is
calibration, mass resolution, and mass transmission
through the analysis of decafluorotriphenylphosph
7.2.9.2 The required frequency of DFTPP analysis
each GC/MS system) is described in detail in Exl
7.2.9.3 The key ions produced during the anal;
respective ion abundance criteria are given Yn
ibit D. The
mass
accomplished
7.2.9.4 The documentation includes Form I,
7.2.10 Initial Calibration of the GC/MS Sy
7.2.10.1 Prior to the analysis of s
instrument, performance criteria have
initially calibrated using calibration
compounds, surrogates, and internal standards"^
7.2.10.2 The detailed procedur
7.2.10.3 The GC/MS is calibre
PUF/XAD-2 cartridge assemblies,Nanc
relative response factor (RRF) met
on
7.2.10.A Calibration standards cont£
interest are prepared as outlined in
Pt'F/XAD-2 cartridges.
7.2.10.5 The PUF.
internal standards
7.2.10.6 The ca,
7.2.11
tatio
printout rbr the a
spectrum
GC/MS/Continuing Cal
red blanks and after
IS system must be
Jntaining the target
s spiked onto the
ations by the
e target compounds of
D and spiked onto the
th known concentrations of
escribed in Exhibit D.
7.2.10.7 Relati
Exhibit D.
7.2.10.8
data syst
described in Exhibit D.
factors (RRFs) are calculated as described in
Form V-AASV, Form VII-AASV, a GC/MS
of each semivolatile calibration
ach target and surrogate compound.
vCnce the GC/MS system has been calibrated, the calibration must
12-hour Dime/period for each GC/MS system.
7.2.11.2
cic the frequenc
ird is to be analyzed according to the procedures and
'iverr in/Exhibit D.
Page E-27
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Exhibit E
Semivolatile Crganics Analysis of Ambient Air
7.2.11.3 The continuing calibration of the GC/MS system j!s evaluated on
the basis of the magnitude of the response factors ana tKe percent
difference between the average RRF of each compoundAxcm the initial
calibration and the RRF of that compound in the continuing calibration
standard. The minimum response factors of each compound wi
-------
Exhibit E
Semivoiatile Organics Analysis of Ambient Air
of
the
hours
sampling. The laboratory method blank cartridge never ,£«aves the
laboratory. The purpose of a laboratory method blank
levels of contamination"associated with the process!
samples at the laboratory, while the field blank moji
due to cartridge handling during sampling.
7.2.13.2 A laboratory method blank shall be an
on each GC/MS system while a field blank must
per SDG, as described in detail in Exhibit D.
/
7.2.13.3 For the purposes of this protocol/ an acceptable blank mus^l
contain less than or equal to the Contract/Required Quantitation Limit
(see Exhibit C) of any single target compoun/l, or le/s^han 10
/zg/cartridge for total semivolatiles, wb/ictyever is
7.2.13.4 If a laboratory blank exceeds the^imips f/6r contamination
above, the Contractor shall consider tne\analybo/cay system out of control.
The source of the contamination must be invte^tigat4d and appropriate
corrective actions taken and documented before^Curthe^xsaraple analysis
proceeds. The requirements for reanalysis of assote^ted^xajnples are given
in Exhibit D.
7.2.13.5 The documentation inau
I-AASV for the blank analysis,
blank, Form IX for surrogate reco
system printout for the analysis o
.2.14 Surrogate Compound Recoveries
II-AASv~Bta«lc7Suniroary Form, Form
fac_internal standards in the
isrifes inxthe/blankvand a GC/MS data
.theXbianlj
7.2.14.1 The recovery
the analysis of each/sai
compounds is to evaluate the
and GC/MS system. /Poor extra
transfer lines apre only a fe
these compounds
the^urrogate Vompounds are calculated from
,d olajak. Thexpurpose of the surrogate
rformanb&of tbe entire PUF/XAD-2 cartridge
tion~*fficie~ftey, leaks, and cold spots in
of/the po*6ent.tal causes of poor recovery of
7.2.14.2 Three surrogate confoounds are added to each PUF/XAD-2 cartridge
assembly prior to field s^mplihgat the concentrations described in
Exhibit D. ^FiTve
cartr idge^j ust_jvrir tbxextractipn . ,
compounds are added to the
:he surrogate compounds are calculated
Exhibit D. The recoveries must be within
;en in Exhibit D. If the recovery of any one
these limits, the Contractor shall follow
D.
7.2.14.4 The^NdocumeTVtatzlon/includes Form IX-AASV and a GC/MS data system
printout for thes-analysis x>f. each sample and blank.
January, 1992
Page E-29
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
7.2.15 Performance Evaluation (PE) Samples
7.2.15.1 Performance evaluation samples are intended td assist the Agency
in monitoring Contractor performance. The laboratory wi^l not be informed
is to which compounds are contained in the PE saiwAe^ or
concentrations.
7.2.15.2 The Laboratory shall extract, analy^
che PE sample once per sample delivery group/
»nd
available
report
7.2.15.3 The laboratory will receive PE s/mpLes on PUF/XAD-2 cartridges
from the Agency. The samples will come w/th/ins true toons concerning the
oxtract ion procedure required for the PE/samples. The/Laboratory shall
add internal and surrogate compounds to'th^ PE sample/following
procedures in Exhibit D.
7.2.15.4 Each laboratory shall extract and^soncenl^ate the PE sample
using the procedure described in Exhibit D fortlipse s«nnivolatile target
compounds listed in Exhibit C.
7.2.15.5 The laboratory shall/meet
acceptance criteria as detaile
technical
7.3.8.5.1 The PE sample musti^e analyzed j6n a GC/MS system .meeting
the DFTPP tuning and initial calibration >or continuing calibration
technical acceptance criteria at \he frequency described in Exhibit D.
7.3.8.5.2 The PE
be desoxbecL according to Exhibit D.
7.3.8.5.3 The EE sample nmsdbje^Drepared and analyzed with a
laboratory method ^lank th£t meetsXtje blank technical acceptance
criteria.
7.3.8.5.4 The percent Recovery for each of the surrogates in the PE
sample must oexwithrtw^acceptable windows as outlined in Exhibit D.
7.3.8.5.5 The area"t^sponsia^change between the PE sample and the most
recent caiT5raTi«n standard analysis for each of the internal
standards mu&tbe wl
-------
Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 8
REGIONAL DATA REVIEW
8.1 Contract laboratory data are generated to meet th^ sgecii
Regions. In order to verify the useability of data
each Region reviews data from the perspective of en
functional aspects of data quality. General guide!
been developed jointly by the Region and the Nati
Region uses these guidelines as the basis for datfa
Regions may augment the basic guideline review pro
based on Region-specific or site-specific concur
the sites under investigation, vary based on/the/nature
investigation and the Regional response apppopr/ate to
circumstances.
8.2 Regional data reviews relating useability of^the d^ta to a specific site
are part of the collective assessment process. They^compEament the review
done at the Sample Management Office, which is designeJK^p ioteijtify
contractual discrepancies, and the rejriew done at EMSL/LV^whicly is designed
to evaluate Contractor and method perforina?Rre-r-^£hese individual evaluations
are integrated into a collective re\iew(>th^tis necesSsry^for program and
laboratory administration and managementX^ndraayHse used to^fake appropriate
action to correct deficiencies in the <$Lonrractor/s .performance.
.needs of the
purpose,
m>oi
for data rfevj-ew
Program Office/^vEach
aluation. Individual
ss with additional review
Regional reviews, like
f the problems under
e/specific
January, 1992
Page E-31
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 9
LABORATORY EVALUATION SAMPLES
9.1 Although intralaboratory QC may demonstrate Con
performance that can be tracked over time, an exte
program is an essential feature of a QA program.
Contractor and method performance, Contractors p
comparison studies conducted by the EPA. Resul
laboratory evaluation samples will be used by
Contractor's continuing ability to produce ac
results are also used to assess the precisi
methods for specific analytes.
9.2 Sample sets may be provided to particip
on an SDG-by-SDG basis as a recognizable QC samp
recognizable QC sample of unknown composition; or n
material. The laboratory evaluation samples may be
kation
Regional client or the National Prog
action.
the
cal data. The
the analytical
:tors as frequently as
composition; as a
Lzable as a QC
the
)ffice, and may be>ised/ror contract
9.3 Contractors are required to analvzeNthe salni
package and all raw data within the coftpra\t re?
es—andretiurn the data
itfed turnaround time.
9.4 At a minimum, the results are evaluated for/compound identification,
quantification, and sample contamination. GonfMence intervals for the
quantification of target comp"o"un3s>vare based\n reported values using
population statistics. EBA raay_adjukt the scores on any given laboratory
evaluation sample to comtfen&ate fb^r uiianticipateol difficulties with a
particular sample. Normally, a frajction of^he compounds spiked into the
ss
sample are not specifi
to use the NIST/EPA/i
maximum number of n
a minimal response.
contractually described
integrated into the evaluate
, a frs
listed;
.conti
. Contractors are required
tentatively identify a
raction that are present above
tification of these compounds based on
ctral Interpretation procedures is evaluated and
con
Ldev
9.5 A Contracy6r's results^ap the^baborajtory evaluation samples will
determine the/Con4fractor**<* performance^/ follows:
9.5.1
for a score of 90 percent or above.
89] the Contractor shall describe the
recytive action(s) taken in a letter to the APO,
ys of receipt of notification from EPA.
9.5.3 For a scofc«Lless^than 75, the Contractor shall be notified by the
APO or TPO concernirtgsthe/remedy for its unacceptable performance. The
January, 1992
Page E-32
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
Contractor may expect, but EPA is not limited to, the following actions:
reduction of the number of samples sent under the contract/; suspension of
sample shipment to the Contractor, a site visit, a fuVl data audit,
analysis of remedial PE samples, and/or a contract s^nc^aon, such as a
Cure Notice.
NOTE: A Contractor's prompt response demonstrating
has .been taken to ensure the Contractor's capabi/iity to mee>6scont
requirements will facilitate continuation of fi&l/sample delivfe
January, 1992
Page E-33
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 10
GC/MS TAPE AUDITS
10.1 Periodically, EPA requests from Contractors the/
corresponding to a specific Case in order to accomp]
Generally, tape submissions and audits are requested
reasons.
10.1.1 Program overview;
10.1.2 Indication of data quality problems /rom
data reviews;
10.1.3 Support for on-site audits; and
10.1.4 Specific Regional requests.
GC
ignel
tapes
tape av
the follc
, SMO, or Regional
10.2 Depending upon the reason for anaudit, the
specific Case, or a laboratory evaluation
audits provide a mechanism to assesV. adhecegice to
to ensure the consistency of data reported on?!
on the GC/MS tapes. This function pro\ide\ ext«
requirements and checks adherence of the\Conera6t<
In addition, tape audits enable EPA to evaj.uace
accuracy of the analytical methods.
tapes from a recent Case,
be requesrod. Tape
requirements and
haxdcopy wth that generated
monttwing of Program QC
to internal QA procedures.
utility, precision, and
10.3 The GC/MS tape shall/include r>w data anH. quantitation reports for
samples, blanks, laboratory ffvaluSkriom samples, \niuLal calibrations,
continuing calibration,/and/DFTPP ninrngas>&pcia ted/with the Case requested.
The specific requiremeprcs ytor submyssiojas^of G6/M£ tapes are discussed in
Exhibit B.
10.4 Upon request orvt(he AJhB^n/stnative Project Officer or EMSL/LV, the
required tapes and all n&cessary documentation shall be submitted to EPA
within seven (7) days of nocificatl
January. 1992
Page E-34
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 11
ON-SITE LABORATORY EVALUATIONS
11.1 At a frequency dictated by a contract laboratory's oerfor«ance, the
Administrative Project Officer(APO)/Technical Projecc'Of/icex^TPO^Qr their
authorized representative will conduct an on-site l^borXtory ev&iuatii
On-site laboratory evaluations are carried out to
ability to meet selected terms and conditions speifil
evaluation process incorporates two separate cai^egoj
Evaluation and an Evidentiary Audit.
tor the Contractor1
^ed in-the contract
Cies: Quality Assuranfc
11.2 QUALITY ASSURANCE ON-SITE EVALUATION/
11.2.1 Quality assurance evaluators ittspecbsthe Contractor's facilities
to verify the adequacy and maintenance o&sinstr"i«i(entation, the continuity
of personnel meeting experience or educationxrequir«raents, and the
acceptable performance of analytical and QC profe^duresv. The Contractor
should expect that items to be monitored will include butNapt be limited
to the following items:
Bench she
Review of the
proce "
Size and appearance of
Quantity, age, availabilit;
of instrumentation;
Availability, appropriateness,
Staff qualiflegations,
Reagents, syanc
Standard
ce and performance
Utilization of SOPs;
rsonnel training programs;
I
facilities;
data;
Leal logbook maintenance and review, and
's sample analysis/data package inspection
evaluation, various documentation pertaining
Contractor is integrated in a profile
fhe evaluation. Items that may be included
aboratory evaluation sample scores,
al QA materials, GC/MS tape audit reports,
January. 1992
Page E-35
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
aluation to
to satisfy
is comprised
11.3 EVIDENTIARY AUDIT
11.3.1 Evidence auditors conduct an on-site laboratc
determine if laboratory policies and procedures are
evidence handling requirements as stated. The evic
of the following three activities.
11.3.1.1 Procedural Audit
The procedural audit consists of
standard operating procedures and accoi
following laboratory operations:
• Sample receiving;
Sample storage;
• Sample identification;
• Sample security;
• Sample tracking (fr
• Analytical project fil
11.3.1.2 Written SOPs Audit
The written SOPs
written SOPs to de
following laborat
sample identifie
to completion
and assembly.
11.3.1.3 Ar
The analytical
examinatio
auditor
documentation for the
of analysis); and
mbly.
and examination.of the
te and complete for the
iving, sample storage,
e tracking (from receipt
project file organization
File Evidence Audit
Lie evidence audit consists of review and
file documentation. The
Lne:
pcuraent inventory;
file;
quacy and accuracy of the document numbering system;
.aceabv^ity /f sample activity;
of activity recorded on the documents; and
Identi
January, 1992
Page E-36
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Exhibit E
Semiyolatile Organics Analysis of Ambient Air
11.4
Error correction methods.
DISCUSSION OF THE ON-SITE TEAM'S FINDINGS
The QA and evidentiary auditors discuss their
Administrative Project Officer (APO)/Technical Pr
to debriefing the Contractor. During the debrie
their findings and recommendations for correct
Contractor personnel.
11.5 CORRECTIVE ACTION REPORTS FOR FOLLOW-1]
EVIDENTIARY AUDIT REPORTS
with the
(TPO) prior
audltQrs present
to the
TO QUALITY ASSURANC
11.5.1 Following an on-site evaluation,/QA/and evidentiary audit reports
which discuss deficiencies found during/thaf on-sitar evaluation will be
forwarded to the Contractor. The Cont^actofc^ust/discuss the corrective
actions taken to resolve the deficiencie^fc^discbs/ed/miring the on-site
visit and discussed in the on-site reportsl^a letter to the APO/TPO,
EMSL/LV (response to the QA report) and NEIC (r>^ponsex£o the evidentiary
report) within 14 days of receipt of the finding otswithrtKthe time agreed
upon between APO/TPO and the Contxgctor. If SOPs arevs^qui^?ed to be
written or SOPs are required' to/be am^n7te^>uiie_^ntractoVmust provide
the SOPs to the TPO, EMSL/LV (-O^/teMtoica^OPsT^nTWitEIC (evidentiary
SOPs) within 30 days of receipt fcf ct^e fimlTyig oj^withip7the time agreed
upon between the APO/TPO and the Ctmtractor/
11.5.2 If the Contractor fails to taVe appropriate corrective action to
resolve the deficiencies discussed in Che o.(6-site reports, a Contractor
may expect, but the Agejtey^TSxqpt limite^toj^the following actions:
reduction
suspensio;
a folio
analysis of
& Cure Notice.
nt/under the contract;
J
ontractor;
audit; and
E samples and/or contract sanction, such as
January, 1992
Page E-37
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 12
QUALITY ASSURANCE AND DATA TREND ANALYSIS/
12.1 Data submitted by laboratories are subject to
aspects: compliance with contract*required QC, usa
package evaluation. ~•-•"K1 -us resulting from any o
determine the need foi J/MS tape audit, an on-
and/or a remedial laboratory evaluation sample. /In/addition
the methods provides information that is continually used by the Agency to
"assess sample data quality, Contractor data qualify and P^Wam data quality
via data trend analysis. Trend analysis is accopplished/by/entering data into
a computerized data base. Statistical reports/chat evaluate specific
anomalies or disclose trends in many areas^inc'kvdj.ng^he/following, are
generated from this data base:
in
12.1.1 Laboratory Control Sample;
12.1.2 Blanks;
12.1.3 GC/MS Instrument Perfo:
12.1.4 Initial and Continuing
12.1.5 Other QC and Method Parameter
12.2 Program-wide statist!
to observe the relative
against its peers. The
laboratories. The re
overall evaluation of
determine if correct!
indicated in .order
rank laboratories in order
using a given protocol
tify trends within
nalyses are included in
and are reviewed to
oratory evaluation is
's of the contract.
12.3 Contractor performance over/time is monitored using these trend analysis
techniques to detect departvfr^s of^Gtjntractor output from required or desired
levels of QC, and^JEe •••provide an^uarlyVarning of Contractor QA/QC problems
which may not be apparent rtom theiJejsult^ of an individual case.
12.4 As a
informatio
analytica
vas t emp
analyzed,
performance c"
performance crit
expected of enviro
Program, the data base provides the
formance-based criteria in updated
y criteria have been previously used. The
contract laboratories is carefully
ng theoretical and research-based
is a' continuously monitored set of QC and
ti^ns of; what is routinely achievable and
try laboratories in mass production analysis
January, 1992
Page E-38
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
of environmental samples. This, in turn, assists the Agency/^tn^ meeting its
objectives of obtaining data of known and documented qualit
January, 1992
Page E-39
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 13
specl
DATA MANAGEMENT
13.1 Data management procedures are defined as procedy
acquisition or entry, update, correction, deletion, si
computer readable data and files. These procedures .shot,
and contain a clear definition for all databases anovf^/les used
resubmit deliverables. Key areas of concern incliroe!
(including personnel and security), documentation/o^rations, traceabilitS
quality control.
Ld be
ritt
system organization
13.2 Data manually entered from hard-copy mu£t J/e qualify controlled and the
error rates estimated. Systems should prevent entry of/inoorrect or
out-of-range data and alert data entry peraronnelNof errorsr. In addition, data
entry error rates must be estimated and recorded orNa/mooithly basis by
reentering a statistical sample of the data entefc^d and Calculating
discrepancy rates by data element.
13.3 The record of changes in the fotffl^of corrections andNtgdal^s to data
originally generated, submitted, and/or resubmittedmust be documented to
allow traceability of updates. Doc^em^atii^^ustinclTtds-Jiie following for
each change:
13.3.1 Justification or rationale
iha/ge;
13.3.2 Initials of the person making the change or changes. Data changes
must be implemented and j=evTe>«d by a person\r group independent of the
source generating the deliverable
13.3.3 Change doci
the original delive
intuition mufet •6erestained nccording to the schedule of
rabZe;
skettesr or,
13.3.4 Resubmittfed
a part of the labbtatorj
resubmission. The entire deli
inspected;
13.3.5 The/Laboratory'ftenager
submitted/tie li^erabT>«: ami
erables must be reinspected as
nal inspection process prior to
•erable, not just the changes, must be
irove changes to originally
13.3.6 /Do^ftimentation of
auditors.
itaNchanges may be requested by laboratory
13.4 Lifeto^cle^management procy&dui?es must be applied to computer software
systems developed bys^he laboratory to be used to generate and edit contract
deliverables. Sush sysbajris ipust/be thoroughly tested and documented prior to
utilization
January, 1992
Page E-40
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
13.4.1 A software test and acceptance plan including t<
test results and acceptance criteria must be developed
available in written form.
13.4.2 System changes must not be made directly
generating deliverables. Changes must be made fi
system and tested prior to implementation.
13.4.3 Each version of the production system
identification number, date of installation,
archived.
requirements,
lowed, and
ction systems
13.4.4 System and operations documentation
maintained for each system. Documentat^
and an operations and maintenance manu
^
13.5 Individual(s) responsible for the fol
identified:
13.5.1 System operation and maintenance including^d^cume^ation and
training;
oped and
user's manual
13.5.2 Database integrity, i
quality control; and
13.5.3 Data and system security, b
dating and
January, 1992
Page E-41
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
SECTION 14
REFERENCES
14.1 Fisk, J.F. and Manzo, S.M. "Quality Assurance
Organics Analysis", Proceedings from the Water Pollution
Meeting, May 1986.
14.2 Office of Monitoring Systems and Quality
Protection Agency, "Interim Guidelines and Specific
Quality Assurance Project Plans", QAMS-005/80, pfece^ber 1980.
Preparing
14.3 Office of Solid Waste and Emergency
Protection Agency, Test Methods for Evaluat:
SW-846, November 1986.
ispctase, U.!
ig ?olid Waj/te,
Tvironmental
'Third Edition,
14.4 Laidlaw, R.H. , "Document Control and Cha1?o of CuCstody Considerations
for the National Contract Laboratory Program," Qualify Cor^ol in Remedial
Site Investigations: Hazardous and Industrial Solid Wa^e TesX^g, Fifth
Volume, ASTM STP 925, C.L. Perket, ed^^^American Society fbx^Tes/ing and
Materials, Philadelphia, 1986.
14.5 Health Effects Research LaborXtoiy, U.!
Agency, Manual of Analytical Methods for ttve An;
and Environmental Samples, EPA-600/8-80-t
£nvi£onmentafl. Protection
[ys/s or^Testicides in Humans
ie/1980.
14.6 Environmental Protection Agency, "Guidelines Establishing Test
Procedures for the Analysis o£-To"iiut:ants Und\r o^e Clean Water Act; Final
Rule and Interim Final Ruler and Proposed Rule"\40\;FR Part 136, Federal
Register. Vol. 49, No. 20/. . yf>p~^T>234 -\43442 , Octbber>26, 1984.
14.7 Health Ef f ects iCesykrch Lab/bratpj^r, U^B^^Environmental Protection
Agency. Manual of Analyti/al QualLcy Oontrolxfor /Pesticides and Related
Compounds In Human ana Envmronme9^avs ample s-Serond Revision,
EPA-600/2-81-059. Ap
14.8 Environmental Monito
Protection Agency -
Pesticides and Jhdustrial
1984.
ig Sy^s^ems Laboratory, U.S. Environmental
Re*§erencexStandards and Supplemental Data: The
iicalsx*eposbtory, EPA-600/4-84-082, October
14.9 Ame/ic»h Chemical Socrsty^Committee on Environmental Improvement, and
Subcommitt/e on Environmental Atsalyltical Chemistry, "Guidelines for Data
Acquisition artd Data Quality Evaluation in Environmental Chemistry",
AnalyticaVvQhenu^ry, Volume 52/ Ndmber 14, December 1980.
14.10 Moore, J .PK^noT^^arso^/, V.G. "Quality Assurance Support for the
Superfund Contract E&tiorato^sy Program", Quality Control in Remedial Site
Investigation: Hazardotts^and /ndustrial Solid Waste Testing, Fifth Volume,
January, 1992
Page E-42
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Exhibit E
Semivolatile Organics Analysis of Ambient Air
ASTM STP 925, C.L. Perket, ed. , American Society for Testing
Philadelphia, 1986.
id Materials,
January, 1992
Page E-43
-------
January, 1992
-------
SECTION 1
1.1
1.2
1.3
1.4
SECTION 2
2.1
2.2
2.3
2.4
2.5
SECTION 3
3.1
3.2
EXHIBIT F
EVIDENTIARY REQUIREMENTS
TABLE OF CONTENTS
SAMPLE CHAIN-OF-CUSTODY
SAMPLE IDENTIFICATION
CHAIN-OF-CUSTODY PROCEDURES
SAMPLE RECEIVING PROCEDURES
SAMPLE TRACKING PROCEDURES
DOCUMENT CONTROL PROCB
PREPRINTED LABORATORY FOJ
CONSISTENCY OF DOCUMENTATIC
DOCUMENT NUMBERING AND INVENTS
STORAGE OF EPA,
SHIPPING DATA PA2KR6ES
STANDARD
SPECIFKATlbHS FOR IfRITTEN
STANDARDNJPERAT51JG/PR(rcEDURES
7
8
8
10
12
Januarv. 1992
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
SECTION 1
SAMPLE CHAIN-OF-CUSTODY
A sample is physical evidence collected from a fa
environment. An essential part of hazardous waste inv<
that the evidence gathered be controlled. To accompl,
sample identification, chain-of-custody, sample rec
procedures have been established.
1.1 SAMPLE IDENTIFICATION
1.1.1 To assure traceability of samples
Contractor, the Contractor shall have a
identification of samples throughout the
1.1.2 Each sample and sample preparal
with the EPA sample number or a unique labth
unique laboratory identifier is used, it shall
EPA sample number.
1.2 CHAIN-OF-CUSTODY PROCEDURES
1.2.1 Because of the nature
of EPA samples must be traceable
until they are introduced as evident
Contractor shall have procedures ensuring
maintained and documented.
1.3
'd, the custody
es are collected
proceedings. The
't EPA sample custody is
or from the
effort is
following
Bracking
ssion of the
for maintaining
shall be labeled
ntifier. If a
-referenced to the
1.2.2 . A sample is
1.2.2.1 It is i
1.2.2.2 It is An /our
1.2.2.3 It
1.2.2.4 It is in a
accessible t
1.3.
samples
condition o
wing applies:
your possession.
ssion and you locked it up.
secure area (secure areas shall be
tel only).
X?
llXdesignate a sample custodian responsible
.esignate a representative to receive
sample custodian is not available. The
tainers and sample bottles shall be
January, 1992
Page F-l
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
inspected upon receipt by the sample custodian or his
epresentative.
1.3.3 The condition of the custody seals (intact/nbt intact) shall be
inspected upon receipt by the sample custodian or hils/h&i^representative.
/ <^
1.3.4 The sample custodian or his/her represet
the presence or absence of the following documei
sample shipment:
1.3.4.1 Airbills or airbill stickers.
1.3.4.2 Custody seals.
1.3.4.3 EPA custody records.
1.3.4.4 EPA traffic reports or SAS
1.3.4.5 Sample tags
er representative
1.3.5 The sample custodian or
date all forms (e.g., custody
and airbills) accompanying the
sign and
Backing lists,
le receipt.
1.3.6 The Contractor shall contact SMO to/re^olve~~3lrfcrepancies and
problems such as absent documents, cWfr^cOina' information, broken
custody seals, and unsatisfactory sample condition (e.g., leaking sample
bottle).
1.3.7 The Contrac to if shall re
problems on Telephone/Copf£act
ion of discrepancies and
1.3.8 The followtnj
the sample custodian
and inspected:
1.3.8.1
1.3.8.2
and/or s
Lon>faall 6e^>eacorded on Form AADC-1 by
his/hjfr ijepreseh^atiye as samples are received
lipping container.
ondition of custody seals on shipping
, when present.
nple bottles.
of airbills or airbill stickers.
sticker numbers.
January, 1992
Page F-2
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
1.3.8.7 Presence or absence of EPA custody records.
1.3.8.8 Presence or absence of EPA traffic reports' or/SAS packing
lists.
1.3.8.9 Presence or absence of sample tags.
1.3.8.10 Sample tag identification numbers c
sample numbers.
e EPA
1.3.8.11 Verification of agreement or non/agreement of information*
recorded on shipping documents and sample/coyitainers.
1.3.8.12 Problems or discrepancies.
1.4 SAMPLE TRACKING PROCEDURES
The Contractor shall maintain records docuwfijitini
handling from receipt to final analysis. The reco
documentation of the -movement of samples and prepared
designated laboratory storage areas
phases of sample
include
nto and out of
January, 1992
Page F-3
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
SECTION 2
DOCUMENT CONTROL PROCEDURES
The goal of the laboratory document control pro,
aj.x documents for a specified SDG will be accounted
completed. Accountable documents used by contract
but not be limited to logbooks, chain-of-custody
rich sheets, and other documents relating to the
The following document control procedures have
all laboratory records are assembled and store
available upon request from the EPA prior to
2.1 PREPRINTED LABORATORY FORMS AND LOG
2.1.1 All documents produced by the
related to the preparation and analysis of
property of the EPA and shall be placed in
group file (CSF). All observations and results
laboratory but not on preprintedrJ^boratory forms
permanent laboratory logbooks. /WhenaTT^dftta^from a
all original laboratory forms and top-iasof all
entries shall be included in thexlocbunentatT^n package.
to the EPA or are
dule.
2.1.2 The Contractor shall identi
laboratory documents which is directl^
analysis of EPA samples.
ch are directly
shall become the
sample delivery
the
'ntered into
compiled,
ed logbook
.vity recorded on all
id to the preparation and
2.1.3 Pre-printed
laboratory and be da
responsible for
performed.
2.1.4 Logboo
the person respo"
activity is performe
2.1.5 Lori
logbooks, with the exceV^ion
shall incAude^only*^me SDGSper page
forms shal\ contain the name of the
(monQv/day/year) anovsighed by the person
thes/time an activity is
th/day/year) and signed by
the activity at the time an
chronological order. Entries in
nt run logs and extraction logs,
2.1.6 / P/ges in both bo
numbe/ed
d unbound logbooks shall be sequentially
2.1. 'Tx. Insts^jment run lorfs shall be maintained so as to enable a
reconstrurs^ion ofthe runAequence of individual instruments. Because
the laboratotjt mustNgrov/de /copies of the instrument run logs to the EPA,
the laboratory ritaj^ exeWisjf the option of using only laboratory or EPA
January, 1992
Page F-4
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
2.2
2.3
sample identification numbers in the logs for sample ID
government agency or commercial client names to preserve
confidentiality of commercial clients.
her than
e
2.1.8 Corrections to supporting documents and ra# da%a shall be made
by drawing a single line through the error and entzerinE thexcprrect
information. Corrections and additions to supporting dbcuraeivfeSxand raw
data shall be dated and initialed. No information /shall be^obliterated
or rendered unreadable. All notations shall heXrereorded in inky. Unused
portions of documents shall be crossed out.
CONSISTENCY OF DOCUMENTATION
2.2.1 The Contractor shall assign a date
responsible for the organization and as.se
2.2.2 All copies of laboratory docume
legible.
2.2.3 Before releasing analytical results, the
officer shall assemble and cross*fit»eck the
custody records, laboratory bench shee
and other relevant data to ensure
sample or sample delivery group \s c\nsisten> tto_u;
DOCUMENT NUMBERING AND INVENTORY
nt control/officer
y of tUe OSF.
2.3.1 In order to provide document aXeoui(tability of the completed
analysis records, each ieSnTtRva CSF shalsl bev inventoried and assigned a
serialized number as described rn Exhibit \, Section 2.
ontrol
le tags,
rument logs,
each particular
the CSF.
CSF # - Region -
2.3.2 All doc
bench sheets, m
preparation reco
analysis, custody
inventoried.
2.3.3
ensuring
and are
plasti
docum
2.4 STO:
The Contra
location.
e: 75-2-0240).
including logbook pages,
creening records, re-
records, records of failed or attempted
research results, etc., shall be
;icer/(DCO) shall be responsible for
generabejd are placed in the CSF for inventory
The DCO shall place the sample tags in
Figure E-l of Exhibit E is an example of a
.ntaiin EPA laboratory documents in a secure
January. 1992
Page F-5
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
rabies packages
on the
ging or
to whom,
2.5 SHIPPING DATA PACKAGES AND CSF
2.5.1 The Contractor shall document shipment of
to the recipients. These shipments require custody
containers placed such that they cannot be opened
breaking the seal. The Contractor shall documen
the date, and the method (carrier) used.
2.5.2 The Contractor shall purge the CSF
appropriate EPA Region 180 days after the
2.5.3 A copy of the transmittal letter
NEIC and SMO.
2.5.4 The Document Control form is
inspection of shipping containers and s
submit one original FORM AADC-1 for each
2.5.5 The Contractor shall sign and date the
examine the shipping containers,/-record the presence
custody seals and their condit
2.5.6 The Contractor shall not
follow the instructions explained'
2.5.7 . The Contractor shall submit
with each SDG package.
the receipt and
Sontractor shall
present),
ce of
the/samples and
g-In Sheet.
:ed Document Control Form
January, 1992
Page F-6
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Exhibit F
Semivolatile Organics Analysis of-Ambient Air
SECTION 3
STANDARD OPERATING PROCEDURES
The Contractor must have written standard operatl
for receipt of samples, maintenance of custody, sampley
storage, tracking the analysis of samples, and assei
3.1 SPECIFICATIONS FOR WRITTEN STANDARD OPERATI
3.1.1 An SOP is defined as a written narr>
description of laboratory operating proced
laboratory documentation. The SOPs must
procedures used in the. laboratory, and c
be available to the appropriate laborat:
are necessary to ensure that analytic
are acceptable for use in EPA enforceme
litigation.
(SOPs)
, sample
data.
itive step-by-step
including examples of
ribe the actual
ftten SOPs shall
procedures
'under this contract
ration and
3.1.2 The Contractor's SOPs shall provide mectu
to meet each of the following specifications and
the basis for laboratory evider
written standard operating
3.1.2.1 Sample receipt and lo§
3.1.2.2 Sample storage.
3.1.2.3
3.1.2.4
3.1.2.5
3.1.2.6
3.1.2.7
3.1.2.8
documentation
'ed by EPA as
st have
3.1.2.
id. logbooks.
data control systems.
t
eview of laboratory operation and
contractually-required quality assurance
each individual data package.
fata handling, and reporting.
January, 1992
Page F-7
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
3.1.2.12 Chain-of-Custody.
3.1.2.13 Document control, including Case file
3.1.3 The Contractor shall have a designated s
responsible for receipt of samples and have writ
his/her duties and responsibilities.
3.14 The Contractor shall have written
in of the samples. The procedures shall in<
documenting the following information:
3.1.4.1 Presence or absence of EPA c
3.1.4.2 Presence or absence of airl
pr
receiving anc
but not be limited
3.1.4.3 Presence or absence of EPA
lists.
3.1.4.4 Presence or absence gf___custody seals on s
containers and their conditio
3.1.4.5 Custody seal numbers^
3.1.4.6 Presence or absence of
3.1.4.7 Sample tag ID numbers.
3.1.4.8 Condition 0tt the
3.1.4.9 Conditit
Tra
3.1.4.10 Verifj
receiving doc
and/or sample
rcement of information on
3.1.4.11 Resolut
3.1.4.12
upon rec
ems or discrepancies with SHO.
used to describe sample condition
have written SOPs for maintenance of the
in and shall demonstrate security of the
reas. The SOPs shall specifically include
as for EPA samples in the laboratory, and
ontamination. The SOPs shall include a
10 have access or keys to secure storage
January. 1992
Page F-8
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
3.2
3.1.6 The Contractor shall have written SOPs for
performed on any particular sample. The tracking SOP
following:
3.1.6.1 A description of the documentation used
receipt, sample storage, sample transfers, sampl
sample analyses.
trai
ig the work
include the
3.1.6.2 A description of the documentation
calibration and other QA/QC activities^.
3.1.6.3 Examples of the document format
used in the sample receipt, sample stor
analyses.
3.1.7 The Contractor shall have wri
identification of EPA samples throughout
cord sample
ons. and
laboratory documentation
fer, and sample
3.1.8 If the Contractor assigns unique laboratory"Identifiers, written
SOPs shall include a description of the method usettyto as^s^gn the unique
laboratory identifier and cross-reference to the EPA sample/humber.
in taming
3.1.9 If the Contractor usesV premises or
sample identification numbers,
definitions. The Contractor shalr\ha-*e writ
method by which the laboratory maim
addition -to
fs shall inZlude their
sOPTTieScribing the
\ks under custody.
3.1.10 The Contractor
assembly of all documen
and managerial review
basis. The procedur
pages. sample tracking
printouts, raw dat
documents having .ref
submission to E
inventory proce
shall have wri
^ing to
Documents shall beN^fi
isurte that all
tst
records^
iries,
ence to>
ie system
Case
en TOPs for organization and
ERA Case, including technical
d on a Case-specific
cqments including logbook
charts, computer
and any other written
re compiled in one location for
it inclvute-'a document numbering and
3.1.11 The Contractor^shall Tvave written SOPs for laboratory safety.
3.1.12
used in
hall^have written SOPs for cleaning of glassware
zing samg/es under this contract.
llXhave SOPs for traceability of standards
CONFIDENTIAL INFORMATION
3.2.1
conraucjting work under this contract may receive
January, 1992
Page F-9
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Exhibit F
Semivolatile Organics Analysis of Ambient Air
do
EPA-designated confidential information from the Agenc
information must be handled separately from other
under this contract. To accomplish this, the folio
the handling of confidential information have been
3.2.2 All confidential documents shall be und
designated Document Control Officer (DCO).
mfidential
Station developed
for
Lished.
3.2.3 Any samples or information received
confidentiality shall be handled as "confid
file shall be maintained to store this inf
segregated from other nonconfidential inf<
confidential samples shall be treated as/co
confidential information, the DCO logs
Confidential Inventory Log. The info
authorized personnel but only after it "has bee*1
by the DCO. The documents shall be returne*
conclusion of each working day. Confidential
reproduced except upon approval by the.EPA
will enter all copies into the
this information may not be dii
Contracting Officer. The DCO
any confidential information dii
record of the disposition in the
Contra
£ument control syst
upon appr
A separate
ion and shall be
ion. o£b& generated from
idential. /Upon receipt of
documents/into a
is tpen/made available to
out to that person
to th«C locked file at the
may not be
cer. The DCO
he
addition,
•by the EPA
cover page of
shall keep a
Log.
January, 1992
Page F-10
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January, 1992
-------
Exhibit G
Semiyolatile Organics Analysis of Ambient Air
EXHIBIT G
GLOSSARY OF TERMS
Aliquot - A measured portion of a field sample taken for
Analysis Date/Time - The date and military time (24/noyr clodcjv^f tfi>
introduction of the sample, standard, or blank int^ys^e GC/MS systt
Analysis Group - An analysis group is a set of
'samples (as defined below) for the purpose of
Control (QA/QC), such that the QA/QC required/by
prepared and analyzed at a frequency of once/pe]
re than twenty analytical
id Quality Assurance/Quality
ibit yEi*, at a minimum,
twenty/ana/ytical samples.
Analysis Run - The actual instrumental ana^ysis^Qf the sample preparations
from the time of instrument calibration through tHex/unr/lng of the final
sample. All sample preparation analyses duringN&e ana4ysis run are subject
to the QC protocols set forth in Exhibit E of thisTscntrab<^unless otherwise
specified in the individual methods.
thod
Analytical Preparation Method - A
otherwise release the compound(s)
final solution containing the compov
or other analysis methods.
Analytical Sample - Any solution or media
which an analysis is performed excluding
calibration standards. Note«-CftE*-£<>llowing
samples: undiluted and dilated sampTes (EPA
laboratory control samply (L£s)?''sand planks.
^traction)
litable
. "to dissolve or
and provide a
for instrumental
ItiaZ
ed into an instrument on
calibration and continuing
defined as analytical
no-EPA), duplicate samples,
ASTM Type II Water - D/sti/lled w
/mho/cm at 25°C. For/additional
"Standard Specifica
?ns
:tivity of less than 1.0
fefer to ASTM D1193-77,
on
Background Correction -
contribution to the instn
compounds.
Batch - A
Breakthrou;
will be i
Calibrate
Reagent/Jater"
vtechniqXfe to compensate for variable background
signal in the determination of target
ared at
lie same time.
le\rolume at which point a particular component
luate from the PUF/XAD-2 cartridge.
an analytical curve based on the response
January, 1992
Page G-l
-------
Exhibit G
Semivolatile Organics Analysis of Ambient Air
or other measured characteristic of known standards.
Calibration Standards - A series of known standard solutions/used to determine
instrument stability and reliability (preparation of thy analytical curve).
Case - A finite, usually predetermined number of samp
given time period from a particular site. Case numby
Sample Management Office. A Case consists of one
Groups.
Coefficient of Variation (CV) - The standard deyia^lon as a^ percent of the
arithmetic mean.
Continuing Calibration - Analytical standar
verify the initial calibration of the anal
Contract Required Quantitation Limit (CRQL) - M
acceptable under the contract. Generally defined
standard deviation of seven replicate analyses of the
Control Limits - A range within whi
to be compliant. Control limits ma;
if exceeded, or advisory, requiring
Correlation Coefficient - A number (r) wh
dependence between two variables (e.g., cc
dependent they are the closer the value to
the least squares line.
Cryogen - A liquified gas/us
cryogenic trap of the
(bp - 195.8°C).
of quantitation
more) times the
asurement reXilts must fall
corrective action
flagged.
ic/tes the degree of
ration - absorbance). The more
Determined on the basis of
eratures in the
'cryogen is liquid nitrogen
Data System - For th
the continuous acquis
the chromatographic
Day - Unless othe
DDI - Deioniz
Deuterated
isotope tl
quality
Duplicate -
original sample
omputer system that allows
of time vs. intensity data throughout
11 mean calendar day.
als which contain deuterium (hydrogen
drogen); used as tracers for system
ample that is treated the same as the
ine the precision of the method.
January, 1992
Page G-2
-------
Exhibit G
Semivolatile Organics Analysis of Ambient Air
EBCDIC - Extended Binary Coded Decimal Interchange Code.
External Standards - Target analytes analyzed at a known
to sample analysis, to determine calibration factors.
Extractable - A compound that can be partitioned into
the sample matrix and is amenable to gas chromatograj
semivolatile organic compounds.
Field Blank - Any blank PUF/XAD-2 cartridges spiki
and sent to the field, along with cartridges for,
which ambient air is not sampled.
Field Sample - Material received to be anal
multiple containers and identified by a uni
Holding Time - The elapsed time expressed
the sample by the Contractor until the date
In-House - At the Contractor's facility.
ntration prior
solvent from
include
ained in single or
iber.
e date of receipt of
is.
Internal Standards -
extract at a known ctfnce
used as the basis for'xiuant
Laboratory - Synonymous wit
Initial Calibration - Analysis of
different specified concentrations;
range of the response of the analy
Instrument Detection Limit (IDL) - Dete
standard deviation obtained for the analy
analyte in reagent water) at a concentratio1
nonconsecutive days with sevj
Interferents - Substance
interest.
ies of
rity and dynamic
get analytes.
Itiplying by three the
solution (each
x-5x IDL on three
per day.
or the compound of
ever>yStanraard, blank, and sample
Lor,, to -analysis. Internal standards are
>f the target and surrogate compounds.
*••
tor as used herein.
Laboratory Cont/ol Sample T*>QS) - fti^uot^spiked with known concentration of
specific anaiytes^dnd ^ttbjectelL to the^ejitire analytical procedure in order to
monitor method and contractor performance.
Laboratory" Method Blank (LMB) A A solut-ion produced by performing the
analytical preparation method without the addition of a sample. The solution
thus contains tJifexsame concentrations of reagents as all other analytical
preparationspj^as ahy^impurities Derived from the preparation process. For
preparations conbainingXeagents/of variable concentrations, the LMB should
January, 1992
Page G-3
-------
Exhibit G
Semivolatile Organics Analysis of Ambient Air
match the maximum reagent concentration used in the sample
Laboratory Receipt Date - The date on which a sample is
Contractor's facility, as recorded on the shipper's de
sample Traffic Report. Also referred to as VTSR (vali
receipt).
Linear Range - The concentration range over which
linear.
'action.
at the
jceipt and
sample
Mass Spectral Interference - Defined as the i:
standard quantification ion due to presence o
"noise" at the same mass.
Matrix - The predominant material of which
composed.
Megabore® Column - One of two types of capillary
narrow bore, for the analysis of target compounds unde
Method Detection Limit (MDL) - The
signal, due to an analyte, which is
standard deviation of a series of me
method blanks. In practice, a method detection
higher than an instrumental detection limit.
ns
to detect the internal
mass spectral
analyzed is
other being the
tract.
?
reduces a
times the
•en separate
e substantially
MS-SCAN - The gas chromatograph (GC) is cot.
where the instrument is proj
to disregard all others.
Narrative (SDG Narrativi
laboratory, contract,
documentation of any
with corrective act!
specifications are included
a mass selective detector
for target analytes and
ge which includes
fication, and descriptive
ssing the samples, along
ion. Complete SDG Narrative
Narrow-Bore Capillary Column
the wide-bore
under this con
Performance
EPA for Co
Protocol
sample re
deliverables^
two capillary columns, the other being
, for the analysis of compounds
- A sample of known composition provided by
by EPA to evaluate Contractor performance.
edures to be followed with respect to
ical methods, data reporting and
January, 1992
Page G-4
-------
Exhibit G
Semivolatile Organics Analysis of Ambient Air
Qualitative Accuracy - The ability of an analytical system
identify compounds.
Quantitative Accuracy - The ability of an analytical sys
measure the concentration of an identified compound.
Reconstructed Ion Chromatogram (RIC) - A mass spectr
representation of the separation achieved by a gas
total ion current versus retention time.
(spi
Recovery - A determination of the accuracy of ti
comparing measured values for a fortified
spike values. Recovery is determined by the
%Surrogate Recovery = measured
ialytical
against
spiked
Relative Response Factor (RRF) - A measure of tfesvrelative mass spectral
response of an analyte compared to its internal stahdard.^Relative Response
Factors are determined by analysis of standards and areXused r*L the
calculation of concentrations of ana^ttes^in samples. RRFN\^ determined by
the following equation:
procedure mao»/by
the known
on:
where: A
C
is
x
Resolution - Also terme
chromatogram, calculated
peaks by the peak height
100.
area of the characterise
concentration;
internal stanza
compound >of interes>
between peaks on a
the valley between the
.bei/fg resolved, multiplied by
Retention Time (RT) - TheX^ime to/elute a specific chemical from a
chromatographic column for aX^peci^Fic carrier gas flow rate, measured from the
time the chemical^**—rr*j
-------
Exhibit G
Semivolatile Organics Analysis of Ambient Air
Rounding Rules - The following are the rules for rounding aff^numbers.
If the figure following those to be retained is 1«
is dropped, and the retained figures are kept unc
11.443 is rounded off to 11.44.
lan 5, the figure
As an example,
If the figure following those to be retained
figure is dropped, and the last retained fi§
example, 11.446 is rounded off to 11.45.
ifs greater tR5n^ 5 ,
/is raised by
As
If the figure following those to be retayned/is 5, and if there are no
figures other than zeros beyond the fiver, tfte figure^ 5^is dropped, and
the last-place figure retained is increase/a by one/if/it is an odd
number or it is kept unchanged if an /vet/numberJ As an example, 11.435
is rounded off to 11.44, while 11.42^is rbMndetfoff. to 11.42.
If a series of multiple operations is to beNgerfofcrned (add, subtract,
divide, multiply), all figures are carried thrtxtgh the^calculations.
Then the final answer is rounded to the proper nu&ibej: or^ignificant
figures.
See forms instructions guide
Run - A continuous analytical sequenceNiot
associated quality assurance measurement^
for except
prepared samples and all
red by this contract.
Sample Delivery Group (SDG) - A unit within^a sample Case that is used to
identify a group of s amp1e s ./for 3e^ive ry. An\SDG\is a group of 20 or fewer
samples within a Case, receivejl^over^i period o'f up\to 14 calendar days. Data
from all samples in an SDG aj^e dueS.concuzrently,\ A^ample Delivery Group is
defined by one of the fc/llowing, whichever oscurs virst:
Case; or
Each 20
Each 14-dl
received,
or SDG.
Samples
method.
Sample
by EPA fo
Report
Selected Ion
with/n af Case; or
period during which samples in a Case, are
jinningArith receipt of the first sample in the Case
to Sam^^e Delivery Groups by sample collection
Numb\r)V A unique identification number designated
Sample Number appears on the sample Traffic
on Ion that sample.
ICf) - A plot of ion abundance vs. time or scan
January, 1992
Page G-6
-------
Exhibit G
Semivolatile Organics Analysis of Ambient Air
number for ions of a specified mass.
Semivolatile Organic Compounds - Target compounds with no
between 1 x 10"1 and 1 x 10~7 mm Hg, and which are amenab
method.
Standard Analysis - An analytical determination made
target compounds; used to determine response factor
4
Static Calibration - Calibration of an analytical/system with known
concentrations of calibration gas, obtained from'a pource such as gas
cylinders or prepared from standard stock soluolor
vapor pressures
analysis by this
Stock Solution - A standard solution which c?in
standards.
dilute-d tp derive other
Surrogates Compounds - Compounds added to evfesy bla'hi^, s&mple, and standard;
used to evaluate analytical efficiency by measuring rec4yery. Surrogates are
brominated, fluorinated, or isotopically labelled cbwgounoSs.not expected to be
detected in environmental media.
Target compound - The Semivolatile y6rganic
determine; the compound of interest
jdan analysis 'seeks to
Tentatively Identified Compounds (TIC)\- CtMnpoupfasyftetecteTT' in samples that
are not target compounds, internal stanaards\oif svnrrogate standards. Up to 10
peaks are subjected to mass spectral library sea/ches for tentative
identification.
Time - When required to record time^n any deliverable item, time shall be
expressed as Military Tirte, /Te.^Na 2V-hour clocli
sampl<
Traffic Report (TR) - An
sampler, which accomnani/s the s
which is used for docume
form filled out by the
ler duringxshLpment to the laboratory and
condition and receipt by the laboratory.
Twelve-Hour Time Period "XThe twe/ve (12) hour time period for GC/MS system
tuning, standards calibratiohsXinitial or continuing calibration) begins at
the moment of inj^etirm-Qf the DKTPP analysis that the laboratory submits as
documentation yr complianto^e. The tinyfe period ends after 12 hours has
elapsed accoBflinft^Eb tKSxsjystebi^ clock.
Validated Tim<
received ait
receipt
t KVTSR) - The date on which a sample is
illj.ty, as recorded on the shipper's delivery
t.
January, 1992
Page G-7
-------
ATTACHMENT VI
-------
USEPA CONTRACT LABORAT08Y
-------
-------
TABLE OF CO!
PREFACE
EXHIBIT A SUMMARY OF REQUIREMENTS FOR METAL ANALYSIS
EXHIBIT B REPORTING AND DELI
EXHIBIT C TARGET COMPOUND LIST . .
EXHIBIT D PREPARATION AND ANALYSIS
EXHIBIT E QUALITY ASSURANCE/QDALITY CONTROL REQUIREMENTS
EXHIBIT F EVIDENTIARY
EXHIBIT G GLOSSARY OF
AIR
PAGE NO.
. i
A-l
B-l
C-l
D-l
E-l
F-l
G-l
-------
PREFACE
The purpose of this contract is to provide the U.S. Environmental
Protection Agency (EPA) with chemical analytical services/ quality control
procedures, and an analysis structure which will generates data of known and
documented quality. The methods for the analysis of ambiejit air was developed
with the guidance of the air toxics workgroup to ensure tHat the needs of
regional, state and local air pollution programs were1 address
The samples to be analyzed are of ambient air' collectedNat or
vicinity of known or suspected hazardous waste sic«s/and may con
potentially hazardous organic and/or inorganic mat?
concentrations. The Contractor should be aware
associated with the handling and analyses of tmes/
Contractor's responsibility to take all necessai
ensure the health and safety of its employees./The Co
for providing a safe working environment and making
potential hazards of working with and analyzing^thes
^ the
iba4ji
ial in high
the potential hazard!
samples. It is the
.nd precautions to
tor is responsible
iployees aware of the
les.
measui
Procedures specified herein shall be usedxin the^preparation and
analysis of air samples for the presence and quanfci^atiohxPf inorganic
parameters. The Contractor shall employ safe handling>dures and
generally accepted laboratory practi^esin the performancxof Contract
requirements and shall follow the yquality~~a»surance and quality control
(QA/QC) program specified herein.
The data obtained under this contract will be usea"-fty EPA to determine
the existence and extent of risk posedNby naz^xdrius waste disposal sites to
the public, individuals involved in Supe\furra site cleanups, and the
environment. The data may be used in civnSL ana/or criminal litigation which
requires the strictest adh.ejfeTlce-x.to chain-oS^cuVfody protocol, document
control, and quality assurance procedures.
December, 1991
Revision MAA01.0
Page i
-------
EXHIBIT A
SUMMARY OF REQ
FOR
December, 1991
-------
EXHIBIT A
SUMMARY OF REQUIREMENTS FOR METAL ANAXYS1S OF AMBIENT AIR
TABLE OF CONT:
SECTION 1 GENERAL REQUIREMENTS >x. . . S^. A-l
SECTION 2
2.1
2.2
2.3
SECTION 3
3.1
3.2
3.3
3.4
3.5
Requirements A-12
SPECIFIC REQUIREMENTS
Receive and Prepare
Analyze Samples for till
Quantitation of Specifi*
Perform Required Quality
Quality Control Procedures
DETAILED TECHN
Personnel
Facilities
Instrum
Data
Laborato
December, 1991
-------
Exhibit A
Metal Analysis of Ambient Air
SECTION 1
GENERAL REQUIREMENTS
The Contractor shall employ procedures specified in tn~is Contract in the
preparation and analysis of the ambient air samples for/Che presence and
quantitation of the metal parameters indicated in Exhibit
fed
The Contractor shall employ proven techniqutsT^to identify anc
the metal parameters presented in the Target Compound List (TCL) as
in Exhibit C. The Contractor shall perform sample7preparation, analysis
procedures, and quality control procedures as/preScribed/io Exhibit D, and
meet specified sample preservation and holding £'ime requirements.
For all samples analyzed under this /contract, ttfe Contractor shall
adhere to the quality assurance/quality cda^rol c^A/QC)/protocols specified in
Exhibit E and abide by the evidentiary protocols specified in Exhibit F.
Following sample analysis, the Contractor shaTlxperfcJlsn data reduction
and shall report analytical activities, sample data, andxqualifcy control
documentation as designated in Exhib"TE~~frr-~JExhibit B contaihe^ll reporting
and deliverables requirements for ^hist_^ntracFT~±ne4u4ing copies of the data
reporting forms and forms instruction
To ensure proper understanding o£ tlie lang'
G contains a glossary of terms. When a
explanation, the glossary meaning shall bVapp]
do not replace or take precedency over specific*
Contract text.
ge in this contract, Exhibit
sed in the text without
cable. Glossary definitions
information included in the
The samples to be/anadyzed
hazardous waste sites
at high concentration/levels.
hazards associated with/the hand4.ii
Contractor's respoi
health and safety of it
itrac£or/are from known or suspected
in hazarcteusprganic and/or metal materials
Cpfitrketor should be aware of the potential
and analysis of these samples. It is the
all necessary measures to ensure the
In addition, the Contractor must be aware of the importance of
maintaining thexiStegrrEy^pf the^data generated under this contract, as it is
used to make «(ajoju-4ecisionsNregardih« public health or welfare and the
environment/ Ijsaddition>xdata\ generated under this contract may be used in
litigation/against potentially responsible parties in the enforcement of
Superfund/
December, 1991
Page A-l
-------
Exhibit A
Metal Analysis of Ambient Air
SECTION 2
SPECIFIC REQUIREMENTS
For each sample, the Contractor shall perform
2.1 TASK I: RECEIVE AND PREPARE AMBIENT AIR
2.1.1 The Contractor shall receive and
of-custody and document control procedure
2.1.2 The Contractor shall provide t:
and instrumentation for analyses of th
than the quantitation limits specific
provides the Contractor with the spec
for ambient air samples and an appropria
that shall be used.
2.1.3 The Contractor shall prepare and analyze sasroles yithin the
maximum holding time specif ied/irT'fetliiJkitl), even if thss^s times are less
than the maximum data submission time alloweH—-i»-£h.is contract.
idle samples under the"
'described in Exhibit F.
ftical expertise
^qual to or lower
Exhibi^C./ In Exhibit D, EPA
preparation techniques
ilytical procedures
2.1.4 The Contractor is advis
contract are usually from known o
may contain high levels of organic
hazardous nature and of unknown
be handled throughout the—preparation
caution. The Contractor sha]Lt\be respori
and precautions to
strui
eived under this
ardous waste sites and
materials of a potentially
concentration, and should
lysis with appropriate
for all necessary measures
sur-e~fche health and gafetv of laboratory employees.
2.2 TASK II:
ANALYZE
SPEC]
PLES FOR THE IDE
WON AND QDANTITATION OF
PARAME1
2.2.1 For e
perform the analyi
accompanies the samp
specific analytical
Cs) tc
requi
red, the Contractor shall be required to
as follows. The documentation that
Contractor facility shall indicate
^or that sample or set of samples.
2.2.2 /6xhibie-41spec"rCies thevvana/lytical procedures that shall be
used. Exhibit D contains instructions and references for preparation of
ambient air samples containing low-to-medium concentrations of metals for
ICP./1CP/MS, or AA analysis.
2.2v3 "Ml samples must Initially be run undiluted (i.e., final product
of sampJ^e preparation procedure). When an analyte concentration exceeds
the calibrated otxlinear/raiige, appropriate dilution [but not below the
contract required qilanjn.tacion limit (CRQL) ] and reanalysis of the
prepared sample rs^requiped, as specified in Exhibit D.
December, 1991
Page A-2
-------
Exhibit A
Metal Analysis of Ambient Air
2.2.4 For the purpose of this contract, a full s
defined as analysis for all of the TCL constituents
C in accordance with the methods and quality contro^
Exhibit D and performance of related QA/QC as
Laboratory Control Samples (LCS) and spike sample,
considered a separate full sample analysis. Al
are considered an inherent part of this Contra
contract sample unit price.
2.3 TASK III:
PERFORM REQUIRED QUALITY ASS
PROCEDURES
Analysis is
iified in Exhibit
procedures in
in Exhibit E.
shall each be
requirements
in the
2.3.1 All specific QA procedures pre
procedures prescribed in Exhibit D sha
Contractor. Records documenting the
maintained in accordance with the doc
in Exhibit F, and shall be reported in ac
requirements.
AND QUALITY CO!
ts
fdhered
E and QC
to by the
ot^col shall be
rocedures prescribed
1th Exhibit B
2.3.2 The Contractor shall establish and use on a^contihuing basis
QA/QC procedures, including thfiT3aliy-~oi^(as required)'"'mojte frequent use
of standard reference solutioi4 fremEPArNl5T7--ec_jgecondary standards
traceable thereto, where available\at~~3pp*onriate concentrations (i.e.,
standard solutions designed to ensurte that .operating-parameters of
equipment and procedures, from samVLeNrecelpC' through identification and
quantitation, produce reliable data)\ Eaoiiblts D and E provide specific
QA/QC requirements.
2.3.3 Additional
i.e., with each Cast
Laboratory Control
for metals submitted
verification of
shall, be required (Quarterly or more frequently;
or/Sample Delivery Grfcup \SDG), in the form of
les (L&S)Uafiaseerforn^n6e Evaluation Samples (PES)
EPA for Contracbsr^analysis, and in the form of
snt pafrramnftersy^as described in Exhibit D and E.
2.3.3.1
of data (Exhibit
and returning analys'Ss dat.
Contract andwithin the
Delivery/Schedule.
to the Contractor formats for the reporting
•ntractor shall be responsible for completing
;heets in the format specified in this
me st>^cified in the Contract Performance/
2.3.3^2 / Use of"f
-------
Exhibit A
Metal Analysis of Ambient Air
2.3.4 The Contractor shall provide analytical equ}
expertise for this contract as specified by the fol
2.3.4.1 Inductively coupled plasma (ICP) emis
the capability to analyze metals sequentially 0r
2.3.4.2 Inductively coupled plasma-mass sp
capability to analyze metals (optional).
2.3.4.3 Atomic absorption (AA) spectroi;
furnace and flame analysis capabilities;
,t and technical
£rometer with
.sly.
:h the
equipped with graphite
2.3.4.4 The Contractor shall have, In-b/ouse, the appropriate standards
for all target compounds listed in Exhibit C -prior /to accepting any
samples from the Sample Management OSfice cfiMQ/. /Standards provided by
EPA for use in the Preaward Performance^EyaluatiMi may not contain all
the target compounds and thus shall not bemused fcH^routine analyses
unless or until they have been supplemented with^commfe^ially-available
standard materials.
2.3.5 The minimum function
and conditions of this contract
designate and use qualified key
The EPA reserves the right to revfn
experience.
Project Mana
Inorganijz LabtJTatpry
Quali
Systems
Progr
ively
Assurance 6
Inductively
Inductively
to meet the terms
ontractor shall
ese functions.
qualifications and
(ICP) Operators.
(ICP) Spectroscopist.
d Plasma-Mass Spectrometer (ICP-MS)
'd Plasma-Mass Spectrometer (ICP-MS)
2. 3.5.10 Gtaphite^
2.3.5.11 Sample
ration
Atomic Absorption (GFAA) Operators.
Laboratory Supervisor.
December, 1991
Page A-4
-------
Exhibit A
Metal Analysis of Ambient Air
2.3.5.12 Sample Preparation Specialists.
2.3.5.13 Chemist (back-up).
NOTE: The Contractor shall designate a Sample Custodiahx^and a Document
Control Officer. /
/
2.3.6 The Contractor shall respond within 3^0 d^
data recipients for additional information oir^tplanations thai
from the Government's inspection activities/ /
2.3.7 The Contractor is required to regain' unused,
used sample containers for a period of &6 days aftei
unless otherwise instructed in Exhibit/B or Exhibit D/
>le volumes and
-a. submission
2.3.8 The Contractor shall adhere "to the"~tehaln-of'-custody and document
control procedures described in Exhibitrv. Documentation, as described
therein, shall be required to show that all ptoceduses are being strictly
followed. This documentation shall be reporteo-in^ theXJomplete Case File
Purge (Exhibit B).
2.3.9 Sample shipments to ttfie ContractoTrr3H&acility will be scheduled
and coordinated by SMO, acting\on^eKair§~oi the Administrative Project
Officer (APO) . The Contractor sfealV^communaca£e~-withJ5MO personnel by
telephone as necessary throughout^he^rooess/of sample scheduling,
shipment, analysis, and data reporting/\#o erisure that samples are
properly processed.
2.3.9.1 If there are prob
containers broken)/or
Reports not with /hipment,
correspond) the yConCractor
The Contractor/sha/l immedi
laboratory conait/ons tha
reporting.
advance regardirg^samp
specify the estimate^ deli
:S with tfte samples (e.g., mixed media,
e documentation/paperwork (e.g., Traffic
and Traffic Report numbers do not
11 immediately contact SMO for resolution.
tely'~nby/a unique EPA Case number assigned by
coup of samples collected at one site or
finite time period, and will include one or more
with associated; blanks. Samples may be shipped to the
or multiple shipments over a period of
oC the Case. A Case consists of one or more
by the following:
2.3.10.1 E"a«h, Castex^ field samples received; or
2.3.10.2 Each 20 fiel
-------
Exhibit A
Metal A:
.nalys i
sis of Ambient Air
2.3.10.3 Each seven calendar day period during whyfh field samples in a
Case are received (said period beginning with the/receipt of the first
sample in the SDG).
2.3.11 Data for all samples in an SDG must be
one package) in the order specified in Exhibit
EPA number of the first sample received in theCS
are received together in the first SDG shipm
lowest sample number (considering both alp
the first group of samples received under
reported on all data reporting forms.
that the last sample in the SDG is receve
together (in
The SBG^numfci&r is the
When several samples
the SDG number"
numeric designations)/in
e/SDG. The SDG number is
SJ5G ReceijFfcsJJate is the day
2.3.12 The Contractor is responsibly
samples are received, through proper
and communication with SMO personnel.
jle
each SDG as
ation (see Exhibit B)
2.3.13 Each sample received by the Contractor ^ill bevjabeled with an
EPA sample number, and accompanied by a Traffic Repo-Kt (Tib form bearing
the sample number and descriptivei?rfo«naEi.on regardingN^ie sample. The
Contractor shall complete and\sign,j:he TR, rec&rttingtit\e date of sample
receipt and sample condition on\re\eipTT~1:roi?-7each sample^ container.
2.3.14 The Contractor shall submXt sXgneft o6pies of TRs for all samples
in an SDG to SMO within three calendar MVS /fo 1 lowing receipt of the last
sample in the SDG. TRs shall be subm\tted/in SDG sets (i.e., all TRs for
a SDG shall be clipped cegether) with an SDG Cover Sheet containing
information regarding/the SDGXas specified 1*1 Exhibit B.
2.3.15 EPA Case numbers (initlulifrig^SDG nunJ^e^rs) and EPA sample numbers
shall be used by /he /Contractor in identifying samples received under
this contract both verbally ^ind/£n re>ng picK**qj/of samples at the nearest servicing
airport/ bus stationT^r o\her carrier service within the Contractor's
geographical area.
2.3/17 CThe Contractor s
provided that the total
does n&t^excefed the monti
the Contractor eiiect to/ac
remain bound By^ alloojitrc
accepted.
11)accept all samples scheduled by SMO,
tbefr of samples received in any calendar month
y ^limitation expressed in the contract. Should
pt additional samples, the Contractor shall
t requirements for analysis of those samples
December, 1991
Page A-6
-------
Exhibit A
Metal Analysis of Ambient Air
SECTION 3
DETAILED TECHNICAL & MANAGEMENT REQU]
The Contractor shall have the following technical and"
capabilities:
3.1 PERSONNEL
3.1.1 Project Manager
3.2.1.1 Responsible for all technical
meet all terms and conditions of the
3.1.1.2 Education: Minimum of Bac
scientific/engineering discipline.
3.1.1.3 Experience: Minimum of three yeai
including at least one year in a supervisory pc
3.1.3
Quality
3.1.3.1 Res
data generation
3.1.3.2 Education:
scientif
3 . 1 . 3 ./3 /Experienci
including at least one
pra
laboratory to
n chemistry or any
oratory experience
tion
3.1.2 Inorganic Laboratory
3.1.2.1 Responsible for all
laboratory to meet all terms
3.1.2.2 Education: Minimum of Ba<:he
scientific/engineering discipline.
3.1.2.3 Experience/' Minimi
in operating a ICP/1C,
supervisory posit
degree in chemistry or any
of laboratory experience
t least one year in a
rseeing the quality assurance aspects of
direptly to upper management.
Bachelor's degree in chemistry or any
^
Minimum of three years of laboratory experience,
of applied experience with QA principles and
.aboratory.
3.1.4.1
computing s
generating, up
deliverables .
:he management and quality control of all
software, documentation, and procedures),
I'd performing quality control on automated
December, 1991
Page A-7
-------
Exhibit A
Metal Analysis of Ambient Air
3.1.4.2 Education: Minimum of Bachelor's degree xritm four or more
intermediate courses in programming, information management, database
management systems, or systems requirements analjj
3.1.4.3 Experience: Minimum of three years
systems management or programming including
software used for data management and gener
3.1.5 Program Analyst
3.1.5.1 Responsible for the installa
of software and programs; generating
control procedures on analytical dat,
3.1.5.2 Education: Minimum of Bac
intermediate courses in programming, in:
systems, or systems requirements analysis.
and maintenance
ferforming quality
.ted deliverables.
with four or more
management, information
3.1.5.3 Experience: Minimum of two years experiei^ce i^ systems or
applications programming inclmding~-ORe__£ear of experifen^e with software
used for data management and^ gemsr_at ion of~~35iivexables.
3.1.6 Inductively Coupled PlaSma\ICP) Spea€ro~
3.1.6.1 Responsible for the operation, i/nterpretation, and maintenance
of the ICP spectrometer(s) to meet a^.1 terms and conditions of the
contract.
3.1.6.2 Educati
scientific/engineer
spectroscopy.
3.1.6.3 Exp/ri
ICP analysis
gree in chemistry or any
ized training in ICP
rs of applied experience with
3.1.7
ICP
requiremi
maintaining
operation and maintenance of the ICP
.all teriJis/and conditions of the contract.
of Bachelor's degree in chemistry or any
.pline.
of one year of applied experience with
samples; or in lieu of educational
zfoal years of experience operating and
Station.
December, 1991
Page A-8
-------
Exhibit A
Metal Analysis of Ambient Air
3.1.8 ICP-MS Spectroscopist (Required if ICP-MS is
3.1.8.1 Responsible for the operation, interpret,
of the ICP-MS spectrometer(s) to meet all terms
contract.
e used.)
and maintenance
Conditions of the
3.1.8.2 Education: Minimum of Bachelor's degr
scientific/engineering discipline and specializ
ICP-MS spectroscopy.
3.1.8.3 Experience: Minimum of one year of applied experience wit
ICP-MS analysis of environmental sample/ ana a minimum of two years of
applied experience with ICP analysis of environmental/samples.
3.1.9 ICP-MS Operator (Required if
t
3.1.9.1 Responsible for the operati
spectrometer(s) to meet all terms and
3.1.9.2 Education: Minimum of Bachelor's degree^
scientific/engineering discit
fenance of the ICP-MS
the contract.
istry or any
3.1.9.3 Experience: Mini
ICP and ICP-MS analysis of env}
educational requirement, three a*
and maintaining ICP instrumentatic
3.1.10 Graphite Furnac
3.1.10.1 Response
spectrometer(s) t;
3.1.10.2 Educ
scientific/e^
:xperience with
'in lieu of
of experience operating
ng ICP-MS techniques.
(GFAA) Operator
intenance of the GFAA
ons of the contract.
degree in chemistry or any
3.1.10.3 Experi
analysis of enviro
requirement_three
3.1.11
3.1.
scienti
3.1.11.3
including at least
Exper
of one year of applied experience with AA
les; or in lieu of educational
ars of experience operating and
;tioi\ Laboratory Supervisor
1 technical efforts of sample preparations
ions of the EPA contract.
of Bachelor's degree in chemistry or any
/discipline.
inimum of three years of laboratory experience,
/year of supervisory experience.
December, 1991
Page A-9
-------
Exhibit A
Metal Analysis of Ambient Air
*
3.1.12 Sample Preparation Specialist
3.1.12.1 Responsible for all aspects of sample
terms and conditions of the EPA contract.
3.1.12.2 Education: Minimum of high school
course in general chemistry or equivalent.
3.1.12.3 Experience: Minimum of six monti
analytical laboratory.
3.1.13 Technical Staff Redundancy
3.1.13.1 In order to ensure continu
required work as specified by the co:
minimum of one chemist available at all
person with the following qualifications.
3.1.13.2 Education: Minimum of Bachelor's
scientific/engineering discin/ini
to meet all
ge level
applied experiencexin/an
o accomplish the
shall have a
back-up technical
istry or any
3.1.13.3 Experience: Minimum^of\pne~~yeaxL of experience in each of the
following areas: ICP and ICP-MS o^rationf anffTnaiateriance; AA operation
and maintenance; classical chemis£ry\ana^ytical procedures; and sample
preparation for metals analysis. \ \/ /
3.2
FACILITIES
The adequacy of the
technical staff for accc
contract.
faci
ies
np1ish ing\ the
equipm«
uired
it £$ as important as the
?rK/as specified by the EPA
3.2.1 Sample Keced.pt Area/
Adequate, ">5
-------
Exhibit A
Metal Analysis of Ambient Air
3.2.3.1 Benches with chemical resistant tops.
3.2.3.2 Exhaust hoods.
3.2.3.3 Glove box or isolated area in which
materials.
3.2.3.4 Source of distilled or demineraliz(ed/organic-i
3.2.3.5 Analytical balance(s) located away/from draft and rapic
in temperature.
3.3 INSTRUMENTATION
At a mini"""", the Contractor shall
operative at the time of the Preaward Sit?
full duration of the contract.
3.3.1 100 Samples/Month Capacity Requirement
inge
ng instruments
id committed for the
Fraction
No/ of
Instrument^
ICP Metals
ICIf EnlissionSpectrometer with MS
\p^ctefctor (if appropriate)
GFAA Metals
Atomic Absorption Spectrometer with
^Graphite Furnace Atomizer
NOTE: The Contractor jghallNjav*
(operational) at aT.1 /times
Quantify
ie following instruments available
system:
Inst
its
3FAA
These instruments miist/be included in the bidder's inventory of
equipment. In additiohxthe'Sontractor shall have an in-house stock of
instrument .parts—and circuit boards to ensure continuous operation to
meet con£^act-specifie< holding^an
-------
Exhibit A
Metal Analysis of Ambient Air
3.3.2 200 Samples/Month Capacity Requirements / /
Fraction
ICP Metals
GFAA Metals
No. of
Instrument (s)
1
1
/ Tyije of
/ Instrument
ICP Emission Speirtromefefer with MS
Dectectror /if appropriate }\.
Atomi/c Absorption Spectrometer wtfth
Graimite Furnace Atomizer ^/
NOTE: The Secondary Instrument Requirement/for
Capacity is one GFAA.
These instruments must be inclui
equipment. In addition, the Contractor
instrument parts and circuit boards to ensu
meet contract-specified holding and turnaround
3.3.3 Instrument Specificat
Further information on inXtrument--specifications
ancillary equipment may be found\inNj;xhibit/D
Contract.
les/Month
r's inventory of
an in-house stock of
lous operation to
3.4 DATA HANDLING AND PACKAGING
The Contractor shall
specified in Exhibit B.
required to:
• Provide spa
requirements
4
• Designate
submission.
to submiKreports and data packages as
jlete, this tasV, the Contractor shall be
3.5 LABORATORY
The Co
responsibil
sufficient/re
operatic'
personnel t
Function* inc
3.5.1
.d required
Exhibits in this
ill
s to meet the contract
msible for report preparations and
nave an organization with well-defined
for eacfiNjidividual in the management system to ensure
ources for EPA\contract(s) and to maintain a successful
o establish this\capability, the Contractor shall designate
carry out the following responsibilities for the EPA contract.
Je, but are not/limited to, the following:
Staff
Responsibtexfor all/technical efforts for the EPA contract such as
sample preparationT^anmie analysis, sample validation, and trouble-
shooting of all instruments.
December, 1991
Page A-12
-------
Exhibit A
Metal Analysis of Ambient Air
3.5.2
Project Manager
Responsible for overall aspects of EPA contra
receipt through data delivery) and shall be the
Headquarters APO and Regional Technical Project 0
3.6.3 Sample Custodian
Responsible for receiving the EPA samp
storage).
3.6.4 Quality Assurance Officer
Responsible for overseeing the q
and reporting directly to upper mana
(from sample
contact for EPA
. (TPO).
3.6.5
Document Control Officer
Responsible for ensuring that all document
the Complete SDG File for inventory and are
EPA Region or other receiver a.
aspects of the data
are placed in
.e appropriate
December, 1991
Page A-13
-------
EXHIBIT B
December, 1991
-------
EXHIBIT B
REPORTING AND DELIVERABLES REQUIREMENT!
TABLE OF CONTENTS
SECTION 1 CONTRACT REPORTS/DELIVERABLES DISTRIBUTION ......... B-l
B-3
SECTION 2 REPORTING DESCRIPTIONS AND ORDER/OF /DATA DELIVERABLES
2.1 Updated Standard Operating Procedure
2.2 Sample Traffic Reports
2.3 Sample Data Package ........... •x\- -^N • • • • B'7
2.4 Results of Intercompar
Performance Evaluation
2.5 Complete Case File (CSF)
2.6 Verification of Instrument
2.7 Quality AssurangePlan
SECTION 3 FORM INSTRUCTIONS GUID!
SECTION 4 DATA RE
B-12
B-12
B-12
B-12
B-14
B-49
December, 1991
-------
Exhibit B
Metal Analysis of Ambient Air
SECTION 1
CONTRACT REPORTS/DELIVERABLES DISTRI
The following table summarizes the contract r
requirements specified in the Contract Schedule an
of each deliverable. NOTE: Specific recipient
to change during the term of the contract. The EPA^A
Contractor in writing of such changes when they/occur.
;eliverables
ribution
ub j ect
,the
Item
No. of
Copies
Scheiland Detfvefcy
Distribution
CD
(2)
(3)
Updated Standard
Operating Procedures
(SOPs)
*Sample Traffic Reports
***3 days after
tsample in S
**Sample Data Package
including the Performance
Evaluation Sample (PES)
ocNdays a^tereCeipi of
last .sample in SDG
Results of
Intercomparison ..
Study/Preaward f
Performance Evaluation/ >
(PPE) Sample / /
35
r receipt of
in SDG
X
Complete SDG File /
recei
after data
f last sample
in SDG.
X
Verification of
Parameters
15th day of January ,
April , July , and
October .
Plan
\7aubmit copy within 7
days by written request
by APO.
As Directed
Distrib
(1) Sampl
(2) Environme"
(3) USEPA Region
ystems Laboratory-Las Vegas
December, 1991
Page B-l
-------
Exhibit B
Metal Analysis of Ambient Air
* Also required in each Sample Data Package.
** Concurrent delivery of these items to all recipients
*** An SDG is a group of samples within a Case, r
seven days or less and not exceeding 20 samp
in the SDG are due concurrently. (See Exhibt
description).
**** See Exhibit E for description.
NOTE: As specified in the Contract Schedul
Supplies and Materials), unless otherwise
shall dispose of unused sample volume and'
earlier than 60 days following submission of
Address
(1) USEPA Contract Laboratory Program""
Sample Management Office
P.O. Box 818
Alexandria, VA 22313
For overnight delivery service, use\st
300 North Lee Street
Alexandria, VA 2231
ivernment Furnished
;0, the Contractor
ties/containers no
data.
(2) USEPA Environment,
P.O. Box 93478
Las Vegas, NV
ATTN: Data Audit
For overnight
944 E. Harmon
Las Vegas
ATTN:
<3) USEP,
ory
e, use street address:
| EPA APO, will provide the Contractor with
10 EPA Regions. SMO will provide the
jfonal name/address lists as necessary
contract and identify other client
se basis.
December, 1991
Page B-2
-------
Exhibit B
Metal Analysis of Ambient Air
SECTION 2
REPORT DESCRIPTIONS AND ORDER OF DATA
The Contractor shall provide reports and other deli;
the schedule specified in Section F of the IFB, "S
required content and form of each deliverable is
All reports and documentation shall be:
• Legible;
• Clearly labeled and completed in acpord^nce witK instructions in this
Exhibit;
• Arranged in the order specified in thi
• Paginated; and
• Single-sided.
If submitted documentation doe
Contractor will be required to resub:
deficiency(ies) corrected, at no additional co^t
Whenever the Contractor is required t
result of an on-site laboratP*y^-evaluation
data shall be clearly marked as "ADDITIONAL
three contractual data rftcinietTt* (SlfO, EMSL
shall be included that vdescrribes wiii
Case(s) the data pertain,/and who /requested
criteria,
/with
the Government.
the
or resubmit data as a
augh an APO/TPO action, the
v.and shall be sent to all
Region). A cover letter
fng delivered, to which EPA
data.
Section 3 of tt
properly completing'vall
required documentation^
format.
libit contains instructions to the Contractor for
jor/cing forms to provide the EPA with the
3 the required data forms in EPA-specified
Description
Contract Peri
INFORMATION1
concurrent!
each deliverable item cited in the
.iveryxSchedute^^see Section F of the IFB "SCHEDULE
re specified as^follows in this Section. Items submitted
it be arranged in\the order listed. Additionally, the
component^ of/each item must be arranged in the order presented herein.
2.1 UPD2
DARD OPERATINC
DCEDDRES
2.1.1 The^Gmitrac^or sh«fl.l/submit updated copies of all required Standard
Operating-Procedures c&QPs)/that were submitted with the Prebid Performance
Evaluation (PPE) s^mpJLe resdlts. The updated SOPs must address any and all
December, 1991
Page B-3
-------
Exhibit B
Metal Analysis of Ambient Air
issues of laboratory performance and operation identi
in the review of the PPE sample data and the evalua$
Documentation.
2.1.2 The Contractor must supply SOPs for the
2.1.2.1 Evidentiary SOPs.
2.1.2.2 Sample receipt and logging.
2.1.2.3 Sample and extract storage area.
2.1.2.4 Preventing sample contamir
2.1.2.5 Security for laboratory and si
2.1.2.6 Traceabxlity/equivalency of
2.1.2.7 Maintaining instrument~"?ece*ds_ and bound
2.1.2.8 Glassware cleaning.
by the Contractor
Bidder-Supplied
2.1.2.9 Technical and mana
data package preparation.
laboratory operation and
2.1.2.10 Internal
individual data
pac
2.1.2.11 Sample
2.1.2.12 Chain.
preparation.
2.1.2.13 Sample
• Data flow
Proc
Ev,
\ /
contractu^llyxjrequired QA/QC data for each
data reporting.
itrol, including case file
ition/self-inspection system, including:
for data review;
ton and accuracy;
identifying systematic errors;
jhardcopy data are complete and compliant
libit B;
inspection procedure (demonstrated by
personal notebooks, internal PE samples,
etc
December, 1991
Page B-4
-------
Exhibit B
Metal Analysis of Ambient Air
Frequency and type of internal audits (e.g., ram
checks, perceived trouble areas);
Demonstration of problem identification, corrective
resumption of analytical processing result!
(i.e., QA feedback); and
quarterly, spot
jtions, and
il audit
external) ,
• Documentation of audit reports (internal/
corrective action, etc.
2.1.2.14 Data Handling.
2.1.2.14.1 Data Management procedures defined asf written procedures
that are clearly defined for all databases and files used to generate
or re-submit deliverables specifying the^aQquis^tion or entry,
update, correction, deletion, storage>>and security of computer
readable data and files. Key areas of concern include: system
organization including personnel and security>^demoh^tration,
operations, traceability, and quality control.
2.1.2.14.2 Data manual1
quality control procedures
2.1.2.14.3 The record of cha
updates to data originally genei
must be documented to allow traced
must include the fol
Justificatio
Initials
changes
must be subjected to
form of corrections and
mitted, and/or resubmitted
of updates. Documentation
ipr each change:
hanges or changes. Data
rating the deliverables;
Changed'
of the ori
t be retained according to the schedule
rable;
t be reinspected as a part of the
ion process prior to submission. The
st the changes must be reinspected;
igfcr must approve changes to originally
; and
changes may be requested by laboratory
December, 1991
Page B-5
-------
Exhibit B
Metal Analysis of Ambient Air
2.1.2.14.4 Life Cycle Management procedures must 1/e applied to
computer systems used to generate and edit contract^ deliverables.
Such systems must be thoroughly tested and dooUmenteM^prior to
utilization. **
2.1.2.14.5 A software test and acceptance p^an includir
requirements, test results, and acceptam
developed, followed, and available in wijittj^n form.
iteria must be
2.1.2.14.6 System changes shall not/
systems generating deliverables.
development system and tested prioi
2.1.2.14.7 Each version of the pi
identification number, date of installation^
and archived.
2.1.2.14.8 System and operations
and maintained for each sys
manual and an operations
2.1.2.14.9 Individual(s) re
shall be identified:
System operation and maintenar
training; and
owing functions
luding documentation and
tly to production
.de first to a
on.
fern will be given an
of last operation,
e developed
lude a user's
Database int
2.1.2.14.10
2.2 SAMPLE TRAFFIC
2.2.1 The origina^
shall be submitted to
original Contrac
2.2.2
SDG shal
data updating and QC.
backup, and archiving.
page marked "Lab Copy for Return to SMO"
ry receipt information and signed in
each sample in the SDG.
in^&QGsets (i.e., TRs for all samples in an
with an SDG Cover Sheet attached.
11 contain the following items:
ull sample price from contract;
December, 1991
Page B-6
-------
Exhibit B
Metal Analysis of Ambient Air
Case number; and
List of EPA sample numbers of all samples in the/SDG/ identifying the
first and last samples received, and their dai.es of ret
.
NOTE: When more than one sample is received in /the/first
shipment, the "first" sample received would be i^he/lowest s
(considering both alpha and numeric designations^, and the
received would be the highest sample number /considering both alpha
numeric designations). /
2.2.4 Each TR shall be clearly marked with/the SDG/Nurater and the EPA
sample number of the first sample in the/ SD;G. This/information shall be
entered below the laboratory receipt da4:e 60 the TR. /The TR for the last
sample received in the SDG shall be clearly ma^Jceti "/DC - FINAL SAMPLE."
2.2.5 If samples are received at the laboratory wifch^multi-sample TRs,
all the samples on one multi-sample TR may not nebe^sariiv be in the same
SDG. In this instance, the laboratory shall make the^^aoprobriate number of
photocopies of the TR, and submi/f~onS~T5«p5L-With each SDG^ejtfver sheet.
2.3 SAMPLE DATA PACKAGE
2.3.1 The sample data package sha}
and shall include data for analysis ol
samples include analytical and field ss
5te, consecutively paginated,
samples in an SDG. These
sample reanalyses, blanks,
spikes, duplicates, and
2.3.2 The sample
• Cover page;
• Sample data (
• Quality control
• Raw data;
• Prepar.
Cover Page
nt shall
tory control samples.
e is divided ^nto^ix units as follows:
shall co
Number;
ex;learly labeled "Cover Page." The Cover Page
ory name; laboratory code; contract number; Case
lumber (appears on cover page of SAS); EPA
December, 1991
Page B-7
-------
Exhibit B
Metal Analysis of Ambient Air
sample numbers in alphanumeric order, showing EPA Cample number cross-
referenced with laboratory ID numbers; and comments, Describing in
detail any problems encountered in processing th« samples in the data
package.
The Cover Page shall contain the follow!
"I certify that this data package is in
conditions of the contract, both technic
other than the conditions detailed abov
in this hardcopy data package has bee
Manager or the Manager's designee, as/ve
signature."
This statement shall be directly
Laboratory Manager or his designee with a t
the signer's name and title, and the date of
Lance with the terms
'and for completeness, for
the data contained
Che Laboratory
following
In the event that the Labrato
reported for each sample,
the problems associated with ce
2.3.2.2 Sample Data
he signature of the
below it containing
amp
te all data
t provide~^a~de£ailed description of
on the Cov^t Page.
Sample data shall be submitted with\FORM/I - Analysis Data Sheet, for
all samples in the SD^<—aH^nged in in^rea^ing alphanumeric EPA sample
number order.
2.3.2.3 Quality iCont
The quality control summar# shii.ll
the following forms:
NOTE: If morexthan
arranged in chror
• Initial and Contint
CRQL
iP/nd ICP-MS Interference Check Sample [FORM V - AAIN];
DRM VI - AAIN];
bcsratonNControl Sai
arm/is necessary, duplicate forms must be
tder.
vibration Verification [FORM II - AAIN];
idards (Quarterly) [FORM III - AAIN];
e [FORM VIII - AAIN];
itions [FORM IX - AAIN];
December, 1991
Page B-8
-------
Exhibit B
Metal Analysis of Ambient Air
AAIN];
1) (FORM XII
ICP and ICP-MS Serial Dilutions [FORM X - AAIN]
Method Quantitation Limits (Quarterly) [FORM
ICP and ICP-MS Interelement Correction Fact
AAIN];
ICP-MS Tuning and Response Factor Criteria [70RM XI
ICP-MS Internal Standards Summary [FORM^HJ/- AAIN];
Preparation Log [FORM XV - AAIN];
Analysis Run Log [FORM XVI - AAIN]
Standard Solutions Source [FORM
2.3.2.4 Raw Data
2.3.2.4.1 For each reported value,^fche Contractor shall include all
raw data from the instrument used to obtkin theSsanple values (except
for raw data for quarterly verifications or^lqstrumint parameters).
Raw data shall contain all instrument readouts u^ed fox. the sample
results, including those readeuts^_that may fall beiow the Method
Quantitation Limit (MQL) . .All ICPT"rt^-MS^__and GFAA instruments must
provide legible hard copy o:C tn^iirectreal-t535~-iBatrument readout
(i.e., stripcharts, printer CapeV etcTT? A~ph2tpcopy of the direct
sequential instrument readout
2.3.2.4.2 The order of raw data
ICP-MS, and GFAA. All raw data
ICP and ICP-MS (if Appropriate) and at
units for GFAA.
/data package shall be: ICP,
:lude concentration units for
aencies or concentration
2.3.2.4.3 Me
appropriate cos
following:
• Calibration^
• Initial and contir
oust be^tabeledvwith EPA sample number and
:o identify unequivocally the
.eluding source and preparation date;
bration blanks and preparation blanks;
.braeion verification standards,
les, CKQL standard, and linear range
iples (by EPA sample number) and all
olumes used to obtain the reported values.
and dilutions are consistent for all
a general statement outlining these
nt;
• Duplicates;
December, 1991
Page B-9
-------
Exhibit B
Metal Analysis of Ambient Air
Spikes (indicating standard solutions used, firial/spike
concentrations, volumes involved). If spike information (source,
concentration, volume) is consistent for a gjtven SD€L^ a general
statement outlying these parameters is sufi
Instrument used, any instrument adjustmei
other apparent anomalies on the measure;
data voided or data not used to obtain/
written explanation;
Data and EPA sample number for ICP
clearly and sequentially identifi
All calculations for sample and
percent recovery, coefficient of var~
linear fit;
data, including
and y-intercept of
Sample wei
Sufficient
(i.e., laborato
each batch prepare
• Time and date of each analysis. Instrument ruhxlpgs^an be
submitted if they contain/€Kis~~i»£Qrnjation. If tttesj^istrument does
not automatically provide^ timeof analySts-^-theise must be manually
entered on all raw data for iMti33r-and continuing?calibration
verification and blanks, as\weri as incerfe?enee^check samples and
linear range analysis standa
• Integration times for GFAA analsis.
2.3.2.5 Preparatl
These logs mus
• Date;
identify unequivocally which QC samples
sample, preparation blank) correspond to
arati
2.3.2
ant sample changes or reactions
TRs and SDG Cover Sheet shall be submitted
is Exhibit for all of the samples in the
;ed in increasing EPA sample number order,
md/numeric designations.
December, 1991
Page B-10
-------
Exhibit B
Metal Analysis of Ambient Air
TABLE B-l
Codes for Labelling Metal Data
/so
^\^/
for blank standard
SlO, etc.
Sample ...................... /. ./. . >x XJBSJXX
Duplicate
Sample Spike
Instrument Calibration Standards:
ICP and ICP-MS ............. Sor
Atomic Absorption
Initial Calibration Verification
Initial Calibration Blank ...... ......... ICB
Continuing Calibration Verification . / . x. ../../ ..... CCV
Continuing Calibration Blank ..... S^. . 7x / . / ..... CCB
Interference Check Samples:
Solution A ................. >x- ->Xr • • • ICSA
Solution AB .................. -^X' ^X. ' ICSAB
CRQL Standard for AA ............... -^X ' 7 ' ' CRA
CRQL Standard for ICP and ICP-MS /Tr^T— r-^^... . . . ?Ns/ . . CRI
Laboratory Control Samples . . . ( . .- •^~^~~~^^~-j ..... LCS
Preparation Blank ........
Linear Range Analysis Standard . . . . . ./. /~7~~r~~. — . . . . LRS
NOTES:
V
When an MSA is performed-ensamples
"1", "2" or "3" suffixes musKbe the 1
Number. For instaXicey'ailStSA\pike of a
"XXXXXXDO".
other\than field samples, the "0",
be added to the EPA Sample
cate must be formatted
2.
3.
The numeric suffia
indicates the/ti
'that follow
value
concen
fix for the standards
ion of the standard in
ICP and ICP-MS c
analytes at differed
follow the I
in the
ICP-
4.
Eon /Standards usually consist of several
.concentrations. Therefore, no numeric suffix can
calibration standards unless all the analytes
.at the same concentrations.
considered to be a calibration standard if
^LibXation curve, thus it must be formatted like
format must be used if the CRQL standard
ish the calibration curve.
December, 1991
Page B-ll
-------
Exhibit B
Metal Analysis of Ambient Air
2.4 RESULTS OF INTERCOMPARISON/PERFOEMANCE EVALUATION
The reporting of analytical results for Intercompa:
Performance Evaluation (PPE) sample analyses include,
specified in part 2.3 for reporting of sample data.,
carried through the exact same process as an anal
2.5 COMPLETE CASE FILE PURGE
2.5.1 The Complete SDG File package includes7 all lal
received or generated for a specific Ca.se/that have
submitted to EPA as a deliverable. These itfems sha}
as a deliverable. These items shall be/sulipitted
Inventory Sheet FORM AADC-2 (see Exhib
numbering and inventory procedure).
limited to, sample tags, custody records, s
analysts' logbook pages, bench sheets, instrumenb^readoi
ANALYSES
idy/Pre award
atory records
een previously
submitted to EPA
with their Document
tion of document
but are not
ing records,
records, computer
printouts, raw data summaries, instrument logbook pa|
instrument conditions), correspo/n~aen©«^_and the document
Luding
tentory.
2.5.2 Shipment of the Complet
overnight courier, priority mail 6r e^quivale^t
seals, which are provided by EPA, sbaLKbe ypL
and a document inventory and transmictal
is not required to maintain any docume
by
class mail,
'able. Custody
ed on shipping containers
included. The Contractor
a sample Case after
submission of the Complete_JIPG File packageKhowever, the Contractor should
maintain a copy of the/documentxinventoryXandxtransinittal letter.
2.6 VERIFICATION OF INS
The Contractor si
methods specified ii
instrument used und^r
methods, the Contract*
ferform and i?6p3r-t quarterly verification of MQLs by
ibit D and s. for eafc&OTpe and model number of
tfirs^conttracyt. For ICP and ICP-MS instrumentations and
shari/als/D report annual interelement correction
ination), wavelengths used, and integration
lent Parameters forms for the current
dafca package. using appropriate forms.
factors (including methoffvqf de
times. Annual Verification o£^Ins
year shall be sudSSIttea^HLn each
Submission of/Qitarj-Ai-jy VixrfJi^ai-ii^ of Ang<-yniiK.T»»- Parameters shall include
the raw dat? usj&o. to detferjnine\those values reported.
2.7
3SURANCE PLAN
TfifexContractor shall prepare a written Quality Assurance Plan (QAP)
which afe^cribe^the procedures/ that are implemented to achieve the
following?\mainta4^i data/integrity, validity, and useability; ensure that
analytical measuremehtssystams are maintained in an acceptable state of
stability and repr«kducibil;n:y; detect problems through data assessment and
established correctivfexacxion procedures which keep the analytical process
December, 1991
Page B-12
-------
Exhibit B
Metal Analysis of Ambient Air
reliable; and document all aspects of the measurement
provide data which are technically sound and legally
2.7.2 The QAP must present, in specific terms,
organization, objectives, functional guidelines,
activities designed to achieve the data quality
contract. Where applicable, SOPs pertaining to<
included or referenced as part of the QAP.
during on-site laboratory evaluation and upoi
ss in order to
ible.
December, 1991
Page B-13
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
all
FORM II - AAIN]
FORM III - AAIN]
• ICP and ICP-MS
AAIN]
[S7 Internal-Standards
• ICP-MS/In
lysfis Run Log [FORMKVI\- AAIN]
ard^Solutions Sources
SECTION 3
FORM INSTRUCTIONS GUIDE
This section contains specific instructions
required Data Reporting Forms for analysis of metal
air. This section is organized into the following
• General Information and Header Informations
• Cover Page - [COVER PAGE - AAIN]
• Analysis Data Sheet [FORM I - AAIN]
• Initial and Continuing Calibration
• CRQL Standards/Linear Range Standards
• Blanks [FORM IV - AAIN]
• ICP Interference Check S
• Spike Sample Recovery [FORM V!
• Duplicates [FORM VII - AAIN]
• Laboratory Control Sample^J FORM VII
• Method of Standar/Addlriqns VFORM
• ICP Serial Oil
• Method Quant
AAIN]
>RM XI - AAIN]
Correction Factors (Annual) [FORM XII -
Criteria [FORM XIII - AAIN]
Summary [FORM XIV - AAIN]
AAIN]
- AAI1
[FORM XVII - AAIN]
SampleSLog-InxSheet [PORM/AADC-IN-1]
Document Inv«ntory\shee/ [FORM AADC-IN-2]
December, 1991
Page B-14
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.1 GENERAL INFORMATION AND HEADER INFORMATION
3.1.1 Values must be reported on the hardcopy fo
individual form instructions in this Section. Eac
be filled out completely for all analytes. Multiple
submitted in place of one form if the information/o
submitted on one form. /
cording to the
submitted must
cannot be
bras can be
appr;
3.1.2 For rounding off numbers to the
observe the following common rules. If the
retained is less than 5, drop it (round d
than 5 , drop it and increase the last dig
up) . If the figure following the last
there are no digits to the right of the
the 5 equals zero, then round up if the^ d
round down if that digit is even.
3.1.3 All characters which appear on
presented in the contract must be reproduced b}
submitting data, and the format of the forms
to that shown in the contract. /*te— information may be^^sdderf, deleted, or
moved from its specified position withouC~TM?4Qr ^written approval of the
EPA APO. The names of the variousX^ields^and analyses— £i . e . , "Lab Code",
"Aluminum") on the forms must apfcear\as theV do— oujthe/Eorms , except that
the use of uppercase and lowercase\ letters As/optional".
3.1.4 All alphabetic entries made \nto tbfe forms by the Contractor
must be in ALL UPPERCASE letters (i.e.\"LoV', not "Low" or "low").
by 1 (round
ned equals 5 and
to the right of
tained is odd, or
forms
ractor when
be identical
3.1.5 Six pieces of information are common
each data reporting /forpu TOase \arjeu Lab
No., SAS No., and SDG Ho. This information
and must match 01
;o the header sections of
Contract, Lab Code, Case
(st be entered on every form
3.1.5.1 Th«
identify the Is
'Lab
3.1.5.2
hyphens,
The "Contrae
the
sde*
name chosen by the Contractor to
''may not exceed 25 characters.
number of the EPA contract, including
Q.ysesvwjere performed.
is an alphabetic abbreviation of up to 6
ttih EPA, to identify the laboratory and aid in
messing. This lab
5ntract is awarded,
:ept at the direction
laboratory, the
\ode shall be assigned by the EPA at the time
be modified by the Contractor,
PA. If a change of name or ownership occurs
will remain the same until the
ie EPA to use another lab code assigned by
December, 1991
Page B-15
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.1.5.4 The "Case No." is the EPA-assigned Case number (up to 5
characters) associated with the sample and recorde^ oi/the TR.
3.1.5.5 The "SAS No." is the EPA-assigned number forXanalyses
performed under Special Analytical Services (SAS) ./^IfsanipJ^s are to be
analyzed under SAS only and reported on these/forms, tttenente^ SAS No.
and leave Case No. blank. If samples are an^.yzed accordiitg.to
Contract and have additional SAS requiremen€sO-/then list bottOSase
and SAS No. on all forms. If the analyses/haye no SAS requirement
leave "SAS No." blank.
NOTE: Some samples in an SDG may have
3.1.5.6 The "SDG No." is the Samp.
number is the EPA sample number of t
When several samples are received togetl
the SDG number must be the lowest sample
and numeric designations) in the first group o
the SDG.
?e others may not.
number. The SDG
received in the SDG.
first SDG shipment,
idering both alpha
received under
3.1.6 The EPA sample number^is ±he uniqueTdeRtifying number given in
the TR that accompanied that satole^~T^ris--n/umber isas^igned by the EPA
and it must be used exactly as assii
3.1.6.1 The "EPA SAMPLE No." mus>t be/entered on several of the forms.
This number appears either in the upper right hand corner of the form,
or as the left column of—actable summarizing data from a number of
samples. When the "£PA SAMPLE No." is\nteXed into the triple-spaced
box in the upper r^ght/hand corner of a formXit must be centered on the
middle line of thp three liraes |£hSt*>qpmpriVe/the box.
3.1.6.2 All
field samples
addition, tt
listed in Table
appropriate.
samples7 and^qua^lty control samples associated with
be identified with an-BPA sample number. In
guffix and quality control sample abbreviations
:ion 2 of this Exhibit must be used as
ansctibed to FORMs II-XV in the raw data
of decimal/places that are described in Exhibit
o be rounded only when the number of figures
the maximum number of figures specified
form. If there are not enough figures in
the specified space for that result, then
places to the specified number of
suit for a specific form. The following
December, 1991
Page B-16
-------
.Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
Raw Data Result
5.9
5.99653
95.99653
995.99653
9995.996
99995.9
999995.9
Specified Format
6.3 (to three decimal places)
6.3 (to three decimal places)
6.3 (to three decimal places /
6.3 (to three decimal plac^|%y
6.3 (to three decimal plaices/)
6.3 (to three decimal places)
6.3 (to three decima^; peaces)
Cojzrec^c Entry on Form
/ / 5.900
^\5-997
/ ^\95?9>^
996^ \^
9996.0 ^xy
/\ 99996.0
/ / invalid
NOTE: 6.3 stands for a maximum of six si;
decimal places.
/es and up to three
3.1.8 Before evaluating a number for being irtscontfbl or out of
control in relationship to a certain limit, the number evaluated must be
rounded using EPA rounding rul(is~~To-*ae__significance re^y-ted for that
limit. For instance, the control limitfo?~an-KS^is ± 10 percent of the
true value. A percent recovery. vaKie~~o€-LlP. 4 wouloES' considered in
control while a value of 110.6 woulo\be consid€?&d-ouj/of control. In
addition, a calculated value of 110.561 would/be in control while a
calculated value of 110.55 would be\out\dr control.
3.2 COVER PAGE [Cover
IN]
3.2.1 This form
an SDG, and to pro'
comments. It is
Manager to autho/ize/and
with the SDG.
.so/the document
p list all bitiabt* samples analyzed within
tion and general
signed by the Laboratory
id deliverables associated
3.2.2 Under
sample number (inclui
analysis within the SDG?
dupl icates^tf""15!)
digestion/distillation^
must be/1
Extended
MAB123A is the lowest (cc
sample mimber within the
number fie4d. Samples lis
, MAB125/ '
enter up to seven characters for the EPA
spfkes and duplicates) for each required
spikes must contain an "S" suffix and
spikes (analytical, post
t haVe ait "A" suffix. These sample numbers
in ascending alphanumeric order using the
Interchange Code convention. Thus, if
iering both alpha and numeric characters) EPA
it would be entered in the first EPA sample
below it would be in ascending sequence -
(C111A, MA1111A, MA1111AD, etc.
3.2.3 All^EPA sampj^e/nuafoers must be listed in ascending alphanumeric
order, continuingxjzo the/following Cover Page if applicable.
December, 1991
Page B-17
-------
Exhibit B: Form Instructions Guide
Metal Ana
ivsis
of Ambient Air
3.2.4 Under "Lab Sample ID," a laboratory sample
ten characters) may be entered for each associated
a laboratory sample ID is entered, it must be ent
each EPA Sample No.) on all associated data.
:ification (up to
/sample number. If
(for
3.2.5 Enter "Y" or "N" for "YES" or "NO," ryspe
each of the two questions concerning ICP and ^CP;
question must be explicitly answered with & f^ or
question must be answered with a "Y" or "Ny if/the answer to the se
question is "Y." It should be left blank/If /the answer to the second
question is "N."
3.2.6 Under "Comments," enter any problems encountered, both technical
and administrative, the corrective ac/cionM^aken,/and/resolution performed
for all of the samples in the SDG.
3.2.7 Each Cover Page must be signed, in ^r^ginalbKby the Laboratory
Manager or the Manager's designee, and dated toauthorrse the release and
verify the contents of all data and deliverables associate)! with an SDG.
3.3 ANALYSIS DATA SHEET [FORM
3.3.1 This form is used to
for target analytes (Exhibit C) .
3.3.2 Complete the header information according to the header
instructions and as fo]
3.3.3 For "Lab S
for the sample, as,
3.3.4 For "D,
sample was rec
Validated Time
3.3.5 For "Air Vof
(to two decimaJL_i>laces)
e analysis results
;ory sample identification
3.3.8 Under tf
result is grei
result is lower
(formatted MM/DD/YY) the
ecorded on the TR [i.e., the
ed, Std. m3," enter the air volume sampled
d on the TR.
;d," enb«r/the date (formatted MM/DD/YY) the
laboratory.
r the chemical abstract services register
licable. If a case number doesn't exist,
'ded.
ibeled "CONCENTRATION," if the analytical
4qual to the MQL, report the result. If the
[L, report the CRQL value.
December, 1991
Page B-18
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
NOTE: Analytical results must be reported to two si
the result value is less than ten, and to three sign},
the result value is greater than or equal to ten.
NOTE: The requirement for reporting results to two or
figures applies to FORM 1-AAIN only. Follow the,' spefc"
for reporting all other results on required foijms &s des
Exhibit. / /
iant figures if
figures if
significant
ructions
this
3.3.8.1 Under "/ig/L," enter the value obtained (to two signifi
figures if the result value is less than/ten/ and to three significant
figures if the result value is greater ithai/or equalxfo ten) for the
analyte.
3.3.8.2 Under "jig/m3," enter the
figures if the result value is less
figures if the result value is greater
following equation:
Analyte Cone.
air, usr/m3
9 x
3.3.9 Under the columns labelec
qualifiers as identified in the
qualifiers are used, their explicit11
Cover Page in the Comments section.
3.3.10 FORM I-AAIN
These qualifiers mu
two significant
three significant
ten) from the
Eq. B-l
:er result
airgraphs. If additional
ns must be included on the
types of result qualifiers.
Interference-Corrected
air volume^**/
td. m3
3.3.10.1 C
was obtained
or equal to
a reading tha
3.3.10.2
meanings
Enter "B" if the reported value
the CRQL but greater than
orted value was obtained from
the MQL.
qualifier: Specified entries and their
because of the presence of
of the interference correction(s) is
result concentration;
Lon/exposure precision not met;
Recovery not within control limits;
December, 1991
Page B-19
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
• S - The reported value was determined by the/
Additions (MSA);
* - Duplicate analysis not within contro]
• + - Correlation coefficient for the MSA/ is/less""
NOTE: Entering "S," or "+" is mutually
these qualifiers can appear in the same
3.3.10.3 M (Method) qualifier: Enter/
. npn for Icp.
• "PM" for ICP-MS;
"A" for Flame Atomic Absorption;
• "F" for Graphite Furnace Atomic AbsorptionT
od of Standard
No
for an analyte.
NR if the analyte is not
3.3.11 Under "Comments," ente
the analyte results and note an-
sample analysis (e.g., MSA determ:
and administrative, the corrective
for the sample in the SDG.
3.4 INITIAL AND CONTINOT
3.4.1 This form
calibrations solut
3.4.2 Comple
instructions a:
ents concerning
at occurred during
both technical
taken, and resolution performed
.TION [FORM II - AAIN]
coveries from analyses of
ording to the header
-Cine
3.4.3 Enter the
maximum) and the "Cont
maximum).
EMSL-
additio:
Contra
identj
in t:
sol^itio:
3.4.4
sources we
Source" (twelve characters
n. Source" (twelve characters
* to indicate EPA EMSL-Las Vegas or
source of EPA standards. When
ire prepared in the future, the
supplied with those solutions for
frees were used, enter sufficient information
to identify the manufacturer and the
of FORM II-AAIN if more calibration
3.4.5 Under "WOMl^," ei/ter the number of the wavelength or mass number
for which the results^of each analyte are reported on the form. The
wavelength number is a number assigned to each wavelength used when more
December, 1991
Page fi-20
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
than one wavelength is used to obtain data for ana
wavelength number of "1" is assigned to the longest
the analyte in the SDG. A wavelength number of "2
second longest wavelength and so on. A mass numb
trhe greatest mass used for the analyte in the SD1
assigned to the second greatest mass and so on.
blank if a single wavelength or mass is used
analyte in the SDG.
lyt
3.4.6 Under "INITIAL CALIBRATION True,'
(in fig/L, to three decimal places) of eacl:
Calibration Verification Solution.
3.4.7 Under "INITIAL CALIBRATION Foi
concentration (in /*g/L, to three deci
measured in the Initial Calibration
3.4.8 Under "INITIAL CALIBRATION ZR,1
whole number) of the percent recovery computed
equation:
the SDG. A
ength used for
is/assigned to the
1" is assigned to
number "2" is
t be left
%* -
NUIHe-CALI
to
Verification So
lyte in the Initial
most recent found
each analyte
ution.
lue (to the nearest
to the following
Eq. B-2
Where True (ICV) is the true con
Calibration Verification solution
concentration of the analyte in the
Solution.
3.4.9 Under "CO:
concentration (in
Continuing Calibr
3.4.10 Under
concentration
in the Continuing"
f the analyte in the Initial
(ICV) is the found
Calibration Verification
ter the true
of each analyte in the
£NUING CALIBRATION Fo^mf." enter the found
to/three decimal places) of each analyte measured
ilibr^cioi/Verification Solution.
The
NOTE: The form_£pntainsxtwo "CONTINUING CALIBRATION Found" columns.
column to the^iefF^tost contain vaha.es for the first Continuing
Calibration Ve£4£lcatiohsand thV^oliumn to the right must contain values
for the/second Contihtiing Calibration Verification. The column to the
right ^should be left blank r^ no second Continuing Calibration
Verification was performe
Ifxmore than one F0RM/II-AAIN is required to report multiple
Contintting Calibration Verifications, then the column to the left on the
second formvmustsxpntain'values for the third Continuing Calibration
Verification/^the ceJiu^m t/o the right must contain values for the fourth
Continuing Calibration Verification, and so on.
December, 1991
Page B-21
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.4.12 Under "CONTINUING CALIBRATION %R," enter the/VaLue (to the
nearest whole number) of the percent recovery computedAccording to the
following equation:
Eq. B-3
True (CCV)
Where True (CCV) is the true concentration
(CCV) is the found concentration of the anaiyt<
Calibration Verification Solution.
NOTE: The form contains two "CONTINUING' CAtlBRATI
Entries to these columns must follow tne sequence /He
entries to the "Continuing Calibration Foynd" co
3.4.13 Under "M," enter the method use
3.4.14 If more than one wavelength or mass is^used Sb^analyze an
analyte, then submit additional copies of FORM li^AAJN asxappropriate.
3.4.15 The order of reporting/ICVs afli
the chronological order in whXch Xjke^gtandards
first FORM II-AAIN and moving
the following FORM II-AAIN as
for all analytes must be reported
where three CCVs were analyzed, the
left CCV column on the first FORM II
reported in the right ooltnnrKpf the s
reported in the left/CCV col
second FORM II-AAIN/ t
empty in this example In
analyte was needeti, JChe ICV
II-AAIN and the/CCV/ follow
ach analyte, aYid^ Fou
in the Continuing
columns.
iled above for
bropkiate./
theVirst CC
of the s«
.column ,
for each analyte must follow
starting with the
, continuing to
ice, the first ICV
t FORM II-AAIN. In a run
must be reported in the
the second CCV must be
The third CCV must be
FORM II-AAIN. On the
t CCV column must be left
if a second run for an
be reported on a third FORM
ion as explained before.
3.5
3.4.16 In theSsase whctre iboxV than one wavelength or mass is used for an
analyte in the SDG^^allrcV And CCV results of the longest wavelength
from all runs must beN^portfedbefore proce.eding to report the results of
the second wag&LsQgth orma_ss us>s{l and so on.
3.4.17 Uhder^€eimnents>!: entef>sny/ICV and CCV specific comments
concerning/the analyte results, any significant problems encountered
during'the ICV and CCV analysis (i.e., percent recovery outside the
control .limits, interferences), both technical and administrative, the
cor?4ct4ve action taken, ^nd (resolution performed for the ICV and CCV.
CONTRACT REQUIRED QUANT/TA^ION LIMIT STANDARDS/LINEAR RANGE STANDARDS
(QuartefcJV) fPQRM III / AAIN]
3.5.1 Contrac^fcxRequired/Quantitation Limit Standards (CRQL)
3.5.1.1 This fofmxis used to report analyte recoveries from analyses
of the CRQL Standards.
December, 1991
Page B-22
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.5.1.2 Complete the header information according
instructions and as follows.
3.5.1.3 Under "CRQL," enter the sources of th
"ICP Source," "ICP-MS Source," and "GFAA Source
respective fields (twelve characters maximum
3.4.3.
3.5.1.4 Under "WOMN," enter the wavele
explained in part 3.4.5.
3.5.1.5 Under "True," enter the true/coi
decimal places) of each analyte in
that was analyzed for analytical s
he header
Standards for
is in their
uLned in part
3.5.1.6 Under "INITIAL Found." en
Mg/L, to three decimal places) of each
Standard Solution analyzed at the beginning
3.5.1.7 Under "INITIAL ZR," enter the value
number) of the percent recov<
equation:
(in /Jg/L, to three
ource Solution
the SDG.
oncentration (in
'asured in the CRQL
run.
rest whole
following
Eq. B-4
3.5.1.8 Under "FINAL Found,
to three decimal places^—ofeach
Solution analyzed aj/the end^of each
3.5.1.9 Under
number) of the
equation:
found concentration (in /ig/L,
asured in the CRQL Standard
(to the nearest whole
according to the following
x 100
Eq. B-5
NOTE: For ey^rvinitiabxsolu^ion reported there must be a final one.
However ,xtneoppos±te is no'e^trueX If a CRQL Standard was required to
be analyzed^in-ihe mido^e of assur/(to avoid exceeding the 8-hour
limity, it must bereporc^d in the "FINAL Found" section of this form.
3.5/1.10 If more CRQL Standards analyses were required or analyses
we/e performed using more tnan one wavelength or mass per analyte,
submit additional copies/of/FORM III-AAIN in the appropriate order.
3.5.1.llN^The"twyler of'reporting CRQL standards for each analyte must
follow the chronoibgi/al/order in which the standards were run starting
with the firstTPQRM IIIy&AIN and continuing to the following FORM III-
AAIN as appropriate^x^men multiple wavelengths and masses are used for
December, 1991
Page B-23
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
one analyte, all the results of one wavelength
proceeding to the next wavelength or mass.
must
spe
3.5.1.12 Under "Comments," enter any CRQL-
the analyte results, any significant problems
CRQL standard analysis (e.g., percent recove
limits), both technical and administrative,
and resolution performed for the standard.
3.5.2 Linear Range Standards (LRS) (Quar
3.5.2.1 FORM III-AAIN is also used
the quarterly analyses of the Linear
3.5.2.2 Complete the header info
instructions and as follows.
3.5.2.3 Under "LRS," enter the source of
"ICP-MS Source", and "GFAA Source" analyses in the
(12 characters maximum each) ,/~£s~
eported before
concerning
the
taken,
lyjte recoveries from
(LRSs).
g to the header
ICP Source",
ctive fields
3.5.2.4 Under "INITIAL Tru]
to three decimal places) of eac
was analyzed for the analytical
\ V /
3.5.2.5 Under "INITIAL Found," enter
Mg/L, to three decimal^places) of eact
Solution analyzed at/the beginning of e^ach^
.true concentration (in
?ource Solution that
ss«fciated with the SDG.
found concentration (in
yte measured in the LRS
3.5.2.6 Under /INITIAL %
number) of the p^ercerit reco
equation:
the
ry compu
/> -
'.S initial Foun
(to the nearest whole
according to the following
LRS True
X 100
Eq. B-6
3.5.2.7 Under" FINAL^-EoundT^enter the found concentration (in pg/L,
to threey/de"cimal~plAqes) orxe^ach analyte measured in the LRS Solution
analyze
id oi
?ach
3.5.^.8 / Under "FINAL %R\" enter the value (to the nearest whole
numbery of the percent recovery computed according to the following
ecj nation:
Final Found
LRS True
x 100
Eq. B-7
3.5.2.9 If mc^e LRS Analyses were required or analyses were performed
using more than onex^ajfelength per analyte, submit additional copies of
FORM III-AAIN in the appropriate order.
December, 1991
Page B-24
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.5.2.10 The order of reporting the IRS for each
the chronological order in which the standards wer
the first FORM III-AAIN and continuing to the followi
appropriate. If multiple wavelengths or masses atre
analyte, all the results of one wavelength or mass
before proceeding to the next wavelength or ma^s..
rte must follow
starting with
ig FORM III-AAIN as
sed for one
be reported
>ec£f ic comme
encountered
control Iimits7>
action taken, and
^rning
3.5.2.11 Under "Comments," enter any LRS -
the analytes results, any significant prob!
LRS analysis (e.g., percent recovery outsiae
technical and administrative, the correc;Civ<
resolution performed for the standard.
3.6 BLANKS [FORM IV - AAIN]
3.6.1 This form is used to report "^tQalyte^-confcen^rations found in the
Initial Calibration Blank (ICB), the Continuing Calibration Blanks (CCB),
and the Preparation Blank (PB).
3.6.2 Complete the header information according
instructions and as follows.
the^beader
3.6.3 Under "WOMN," enter
results of each analyte are rep
number is a number assigned to
than one wavelength or mass is used\to
SDG. A wavelength number of "1" is
used for the analyte intheSDG. A wangle
to the second longest/wavelength and so
assigned to the greasests-m&$s uied for th
number of "2" is assigned to^the/sseend greN
field must be left: blank if a/ single wa
data for an analyte An the
.or mass n
or
er for which the
wavelength or mass
mass used when more
taifn data for an analyte in the
d to the longest wavelength
th number of "2" is assigned
mass number of "1" is
yte in the SDG. A mass
mass and so on. The
.length or mass is used to obtain
3.6.4 Under
Mg/L, to three defc
Calibration Blank
CA^IB/BLANK (ICB)," enter the concentration (in
il {Jiace/) of each analyte in the most recent Initial
3.6.5 Fpr^all banks,
(pos itiver or^negatj-ve )
of the
.asurec
pncentration of each analyte
the MQL or below the negative value
3.6.6/ /'Under the "C" qufcliiier field, for any analyte enter "B" if the
absolut^ value of the analyte] concentration is less than the CRQL but
gre4±er than or equal to nhe MQL. Enter "Un if the absolute value of the
analyfee\in the^blank is Ifess/than the MQL.
3.6.7 Unde^x^ONtSl^NG/CALIBRATION BLANK 1," enter the concentration
(in /Jg/L, to thrfe«Ldecimal places) of each analyte detected for the first
CCB analyzed after the^ ^CB. Enter any appropriate qualifier, as
December, 1991
Page B-25
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
explained for the "Initial Calibration Blank," in the/"C/ qualifier
column immediately following the "CONTINUING CALIBRATION BLANK (CCB)"
column.
lumfis^labeled
lyz*
3.6.8 If only one CCB was analyzed, then leave
"Cone. 2" and "Cone. 3" blank. If up to three yCCBs' were
complete the columns labeled "Cone. 2" and "Coftc./S," in accteyJance^ith
the instructions for the "CONTINUING CALIBRATTO^BLANK (CCB)"
more than three CCBs were analyzed, then conpleyce additional copies^
FORM IV-AAIN as appropriate.
3.6.9 Under "PREPARATION BLANK (PB),
jug/L, to three decimal places) of each
appropriate qualifier, as explained f<
column immediately following the "PRE1
'enter the concentration (in
analfyte in ttoe /PB. Enter any
th^ICB, /n jrhe "C" qualifier
column.
3.6.10 Under "M," enter the method used, as
3.7
in part 3.3.10.3.
3.6.11 If more than one wavelength or mass is used l^analyze an
analyte, submit additional copiesoT~-f!9RM__IV-AAIN as appropriate.
3.6.12 The order of reporting
the chronological order in which
first FORM IV-AAIN and moving from
following FORM IV-AAIN as explained
wavelengths or mass are used for the
results of one wavelength—ex^jnass
the next wavelength ojr mass.
3.6.13 Under "Co:
concerning the
during the ICB,
limits), both t
and resolution
must
[FORM V - AAIN]
fibr aaen—iCP and>or
Complete the hea.de
: irons and as follows
lalyte must follow
arting with the
n\lef\ to/ri^ht and continuing to the
»d Rrevious/ly. When multiple
s of one analyte, all the
orted before proceeding to
and iJCB1 specific comments
.cant problems encountered
.anks outside the control
the corrective action taken,
!CP Interference Check Sample (ICS)
truments used in SDG analyses.
information according to the header
3.7S3L Fbr-'ICP ID No., "/enter an identifier that uniquely identifies
the spe^^^ficlnstrument within the Contractor laboratory. No two ICP
instrumentsxwithtnva laboratory may have the same ICP ID Number. If ICP-
MS is used,
3.7.4 For "ICP-Ms^iC^o. ," enter an identifier that uniquely
identifies the specific instrument within the Contractor laboratory. No
December, 1991
Page B-26
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
two ICP-MS instruments within a laboratory may have
Number. If ICP is used leave blank.
fcune ICP-MS ID
3.7.5 For "ICS Source," enter the ICS source (twelve characters
maximum each), as previously explained in part 3/4.3. rk*r EPA solutions,
include the name and number identifying it (e.g/, EPAxLV8/}v^ The
laboratory must use the identification supplie/i by the
3.7.6 Under "WOMN," enter the wavelength /fitOfiass number for which the
results of each analyte are reported on thes form. The wavelength iHjmb4r
is a number assigned to each wavelength used /when more than one
wavelength is used to obtain data for an/ana4yte in /Che SDG. A
wavelength number of "1" is assigned to/th«! longest/ wavelength used for
the analyte in the SDG. A wavelength Aimper of "2" i/s assigned to the
second longest wavelength and so on. /A mass number/of "1" is assigned to
the greatest mass used for the analytfe-^in the^SDG./A mass number of "2"
is assigned to the second greatest mass and so on/ The field must be
left blank if a single wavelength or mass is^-nsed ts^ obtain data for an
analyte in the SDG.
3.7.7 Under "TRUE Sol. A, "
three decimal places) of eacha
concentration (in /Jg/L, to
rte presenE~^ft-Siilution A.
3.7.8 Under "TRUE Sol. AB," «
three decimal places) of each ana
ter\ the tj
ae/coiTCentration (in
in Solution AB.
3.7.9 Under "INITIAL FOUND Sol. A> ent^4r the found concentration (in
Mg/L to three decimal DLaces) of each snal^te measured in the initial
analysis of Solution/A as required in Exhibit; E.
3.7.10 Under "INI
/ig/L to three decimal places^ of each a;
analysis of Solurioji AB as
entektfhe found concentration (in
te measured in the initial
Exhibit E.
3.7.11 Under
number) of the pei
equation:
ant
JCOVX
enter the value (to the nearest whole
sry computed according to the following
found values
zer'b-i of each
or rt»r/-MS
Solution AB
rrUBvSp.Zut.zoji AB
X 100
Eq. B-8
3.7.12' TMder "FINAL FOtJND,\ enter the found concentration (in /zg/L, to
three decimal places) of >eacl^ analyte measured in the final analysis as
req/iren in Exhibit E.
enter the concentration (positive,
.nalyte at each wavelength or mass used for
3.7.
negative,
analysis by
December, 1991
Page B-27
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.7.14 Under "FINAL FOUND %R," enter the value (to
number) of the percent recovery computed according
equation:
%# = Final Found Solution AB
True Solution AB
learest whole
following
NOTE: For every initial solution reported
However, the opposite is not true. If an ICS
in the middle of a run (to avoid exceedingth<
reported in the "FINAL FOUND" section of/thi
Eq. B-9
8-hour limit), it must be
form.
3.7.15 If more ICS analyses were requ^rec
FORM V-AAIN as appropriate.
submit/additional copies of
3.7.16 The order of reporting ICSs for ea^sh analyse must follow the
temporal order in which the standards were ruTtKstarfcing with the first
FORM V-AAIN and continuing to the following FORM^S^AAItT^s appropriate.
When multiple wavelengths or masses are used for oneNanalyfce, all the
results of one wavelength must/be~~reT">tte4^before proceeding to the next
wavelength in the same manner\
3.7.17 Under "Comments," enter a«y "SCS spe6i£i
-------
.Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
assigned to the greatest mass used for the analyte in/the^ SDG. A mass
number of "2" is assigned to the second greatest mass ana so on. The
field must be left blank if a single wavelength or jnas? is used to obtain
data for an analyte in the SDG.
3.8.5 Under "CONTROL LIMIT %R," enter "75-12
value was greater than or equal to one-fourth
If not, leave the field empty.
added
value.
3.8.6 Under "SPIKED SAMPLE RESULT (SSR)J erfcer
Mg/L, to three decimal places) of each analytis in the spike sample.
Enter any appropriate qualifier in the "G"' qnalifier/^so^lumn immediately
following the Spiked Sample Result (SSR/ co/umn.
3.8.7 Under "SAMPLE RESULT (SR),n ^ntefxthe concentration (in pg/L, to
three decimal places) of each analyte neasure^dLJm the sample (reported in
the EPA sample number box) on which the matrix spike was performed.
Enter any appropriate qualifier in the "C" quaj^ifierxcjolumn immediately
following the Sample Result (SR) column.
3.8.8 Under "SPIKE ADDED (S.
three decimal places) of each
added concentration is specifi
reported must be that specific c
3.8.9 Under "ZR," enter the val
percent recovery computed according
NOTE: ZR must be
value of zero mu;
than the MQL.
3.8.10 Under "Q,"
control limits (75-
one - fourth of _the_sample
3.8.12 Us
required spike"
concentratreorf (in /jg/L, to
le. If the spike
lue added and
nearest whole number) of the
following equation:
Eq. B-10
;ative, positive or zero. A
the analyte value is less
Lf the spike recovery (ZR) is out of the
spiked added is greater than or equal to
ed or enter "NR" if the analyte is
s were used for spike sample analysis of
mal copies of FORM VI-AAIN must be submitted
s of FORM VI-AAIN for each sample on which a
sis was performed.
December, 1991
Page B-29
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.8.13 Under "Comments," enter any spike sample spec4fid comments
concerning the analyte results, any significant probflemfe encountered
during the spike sample analysis (e.g , percent recovery outside the
control limits), both technical and administrative, the^uprrective action
taken, and resolution performed for the sample.
3.9 DUPLICATES [FORM VII - AAIN]
3.9.1 This form is used to report results
determining the precision of the method.
3.9.2 Complete the header information
instructions and as follows.
3.9.3 In the "EPA SAMPLE No." box.
characters maximum) of the sample from
this form were obtained. The number must be
3.9.4 Under "WOMN," enter the wavelength or mass
results of each analyte are re/p/ort:e'?i-sn__£h.e form.
number is a number assigned
than one wavelength or mass
SDG. A wavelength number of "l"\is 'assign
luplicate analyses
header
ss
data for
used for the analyte in the SDG. w
to the second longest wavelength aiwl so\0n.
assigned to the greatest mass used f o\ the
number of "2" is assigne^-tQthe secon
field must be left blank if a^ingle wav
for an analyte in th4 S
ample number (7
.plicate results on
in the box.
>r which the
felength or mass
used when more
in analyte in the
igest wavelength
.gjrh number of "2" is assigned
A mass number of "1" is
lalyte in the SDG. A mass
test mass and so on. The
»th is used to obtain data
3.9.5 Under "CONTROL LIMIT, 1 enter the^-CRQL" (in appropriate units,
Mg/L) for the analyse if the/sampleb-r duplicate values were less than
five times CRQI/andCereater/thah or equ^i-~to the CRQL. If the sample and
duplicate values^wereXltess/than the CRQL or greater than or equal to five
times CRQL, leavethe field i^mpty.
3.9.6 UnderJISAMPLE (S)>^ente^the concentration (in the required
concentration units~T^
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
in either the sample or the duplicate, computed accor
following equation:
to the
Eq. B-ll
3.9.9 A value of zero must be substituted f c
concentration is less than the MQL in either/bis^. If the
concentration is less than the MQL in both/S arid D, leave the RPD
empty.
3.9.10 Under "Q," enter "*" if the dup
out of the control limits. If both s
greater than or equal to five times C.
or equal to 20 percent to be in contra
values are less than five times CRQL, the
between the two values must be less than or
control. If both values are below the CRQL,
applicable.
3.9.11 Under "M," enter the
3.9.12 If different samples were\us
different analytes, then additiona
submitted for each sample as approp
for the analyte is
te values are
must be less than
e or duplicate
lute difference
:he CRQL to be in
:rol limit is
3.9.13 Use additional
required duplicate s
3.9.14 Under "Coi
concerning the a:
during the dupli
control limits}
taken, and res
3.10 LABORATORY CONTROL
3.10.1 ThM^formi^afted to
Sample
of FORM v\I-AXlN for each sample on which a
le analsis was performed.
ica~Ce—s&mple analysis of
FORM VII-AAIN must be
jlicaos/sample specific comments
Leant problems encountered
/percent recovery outside the
^trative, the corrective action
for the sample.
VIII-AAIN]
esults for the Laboratory Control
3.10.2/ Complete the header Information according to the header
instructions and as follows.
3.1tK3 Fo*x"LCS USED," en/ter/the appropriate source solution identifier
(12 cha^Kactersxmaximum) prov/ded by the EPA for the LCS solution that was
analyzed bVxthe methods/In Exhibit D.
3.10.4 If no analyse was
was not required to
'analyzed by a certain method or if the analyte
ilyzed, then leave the appropriate spaces empty.
December, 1991
Page B-31
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.10.5 Under "WOMN," enter the wavelength or mass numbe/ for which the
results of each analyte are reported on the form.
number is a number assigned to each wavelength or
than one wavelength or mass is used to obtain da
SDG. A wavelength number of "1" is assigned to
used for the analyte in the SDG. A wavelength
to the second longest wavelength and so on. % m
assigned to the greatest mass used for the a
number of "2" is assigned to the second
field must be left blank if a single wave]
data for an analyte in the SDG.
3.10.6 Under "M," enter the method us«
,e Wavelength or mass
,ssoused when more
for Ss^ analyte in the
avelength
er of"<2" ^xassigned
numberbf"l"N
e in the SDG/XA mas*
mass and so on. ffte
or mass is used to obtain
3.10.7 Under "LIMITS," enter the low^imitSvCoXicetration value (to the
nearest whole number) in the left column^xand the Dipper limit
concentration value (to the nearest whole number) ^h^the right column for
each analyte in the LCS according to the ± 20
3.10.8 Under "TRUE," enter
places) of each analyte in th LCS.
iCentration (to^tijiTee decimal
o three decimal
3.10.9 Under "FOUND," enter theXfoutKl conc/nt^at
places) of each analyte measured in tr
3.10.10 Under "C," enter "B" or "U"\r lefve empty to describe the found
value of the LCS.
3.10.11 Under "%R,
percent recovery c
lue (to ^he nearest whole number) of the
the Sol/lowing equation:
Eq. B-12
3.10.12 If the a
zero must be substitu
3.10.13
more tha;
FORM VI
analy
tration is less than the MQL, a value of
he LCS Found.
FORM VIII-A£IN as appropriate, if
ddition, submit additional copies of
one wavelength was used to determine an
en^er any LCS specific comments concerning the
.nt problems encountered during the LCS
•ery outside the control limits), both
the corrective action taken, and resolution
December, 1991
Page B-32
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.11 METHOD OF STANDARD ADDITIONS [FORM IX - AAIN]
3.11.1 This form is used to report the results of ^^mp/es analyzed using
the Method of Standard Additions (MSA) for GFAA an/
3.11.2 Complete the header information accordir
instructions and as follows.
3.11.3 Under "EPA SAMPLE No.," enter the ER
characters maximum) of the sample from whicj
results on this form were obtained.
NOTE: Only field samples and duplicate
thus the EPA sample number usually has
3.11.4 A maximum of 32 samples can be^ntere^iorf tWis form. If
additional samples required MSA, submit aad^ional/FORMs IX-AAIN.
Samples are listed in alphanumeric order per^aoalytfes^ Submit additional
FORMs IX-AAIN as appropriate.
3.11.6.1 UndeisJ'ZERJ
decimal places)
first addition to t
3.11.5 Under "An," enter the
for each parameter for which
The parameters must be in alp:
NOTE: Results for different sampt
sequentially, with the analytes or<
listing of their chemical symbols. Fi
(Aluminum) in samples BBJilSA. BBB121,
sequence, followed by/the resu
3.11.6 Under "ADDI
observed value in
analyte before
rs maximum)
sample listed.
ical symbols.
parameter must be reported
ding to the alphabetic
ance, results for Al
122 would be reported in
ium) in BBB120 etc.
>
RST," "SECOND," "THIRD,"
cimal places) of the
enter the concentration in /*g/L (to three
irte (excluding sample contribution) after
by MSA.
3.11.6.2 Bffder "FlRSO^, AddeUxFouM," enter the concentration in
(to three de«i»aLDlace^) of tba^aftalyte added in the left column and
the fqund/value in)ig/L C^o three decimal places) of the analyte
(exclAtdiiig sample contfcibu\ion) after the first addition to the sample
/ / \ \ *
analyze^ by MSA in the right column.
3.44.6. 3XInder "SECOND, Addeld, Found," enter the concentration in
(to three dermal place/) of the analyte added in the left column and
the foundxj/alue^^n ng/L (to three decimal places) of the analyte
(excluding sample csQcribution) after second addition to the sample
analyzed by MSA^Sji the iright column.
December, 1991
Page B-33
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.11.6.4 Under "THIRD, Added, Found," enter the concentration in /ig/L
(to three decimal places) of the analyte added in/the/left column and
the found value in Mg/L (to three decimal places/ of A:he analyte
(excluding sample contribution) after third addition tbxthe sample
analyzed by MSA in the right column.
NOTE: The "ZERO, Found," "FIRST, Found,
Found" must have the same dilution factor.
3.11.7 Under "Final Cone.," enter the fi
Mg/L to two decimal places) in the sampl
according to the following formula:
Final Cone. = (-l)x/x-
, Found/
lyte concentration (in
by MSA computed
Eq. B-13
NOTE: The final concentration of a param
value for that parameter which is reported o
sample.
not have to equal the
IN for that
3.11.8 Under "r," enter the cx^EPA^SAlfi>LE/No." box, enter the EPA sample number (seven
characters maxinuJmi of the sample from which the serial dilution analysis
results on this fornhvere obtained. The number must be centered in the
box.
December, 1991
Page B-34
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.12.4 Under "WOMN," enter the wavelength number f or jWiifeh the results
of each analyte are reported on the form. The wavelengtji number is a
number assigned to each wavelength used when more th4n >one wavelength is
used to obtain data for an analyte in the SDG. A Wavelength number of
"1" is assigned to the longest wavelength used for the analyte in the
SDG. A wavelength number of "2" is assigned to X:he/s«eona''4f \sacTT~MWLlyte in the~~9lluted sample
(reported in the EPA sample number b>ox) onyZhL£n~~a-serAal dilution
analysis was performed. Enter anysapproprlatfe qualifier in the "C"
qualifier column immediately following\jfe /'Serial Dilution Result (S)1
column.
NOTE: The Serial Dilution Res^t (S) isNobtkined by multiplying by five
the instrument measured .etmcentiiation value (f» /*g/L) of the serial
diluted sample and/that: the "vC" Qualifier for /the serial dilution must be
established based/on .the serial dilutiohxresult before correcting it for
the dilution regardless of th4 yXlue^xeporte'd on the form.
3.12.7 Under
place) of the per&ejit di
between the original
dilution) according to tl
ffereac
ter the absolute value (to one decimal
erehce in concentration of required analytes,
le and the diluted sample (adjusted for
follbxing equation:
x 100
Eq. B-15
used to calculate % Difference in the
reported on this form. A value of zero
:he analyte concentration is less that the
'ation in (I) is less than the MQL
"%ybifference" field empty.
3.12.8 Under "Q^^enter 7E" if the percent difference is greater than 10
percent and the orig"inal/sample concentration (reported on FORM I-AAIN)
is greater than 50x the MQL reported on FORM XII-AAIN.
December, 1991
Page B-35
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Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.12.9 Under "M," enter the method used.
3.13 METHOD QUANTITATION LIMITS [FORM XI - AAIN]
3.13.1 This form documents the Method Quantitat,
instrument that the laboratory used to obtain
instrument and wavelengths or masses used to gen
must be included.
for each
Only the
ng to the header
on which the MQL
3.13.2 Complete the header information
instructions and as follows.
3.13.3 For "Date," enter the date (fo
values were determined (or became effi
3.13.4 Enter the instrument ID numbers fbx^the"fields "ICP ID No.,"
"ICP-MS ID No.," and "GFAA ID No." (twelve chsracters^maximum each).
These ID Numbers are used to uniquely identify ekch instilment that the
laboratory uses for CLP analyses.
on
to\bt
3.13.5 Under "WOMN," enter th% wavelength or
results of each analyte are re
number is a number assigned to e
wavelengths or masses are used
A wavelength number of "1" is assi
the analyte in the SDG. A wavelength'
second longest wavelengpb—and so on. Ax
the greatest mass useia for theXana
is assigned to the s,econd~"gseat
left blank if a si
analyte in the SD<
for
numbe
;le/waveleagtfc
ilyte
st mass arts
1SS
iber for which the
form. The^fravelength or mass
m two or more
an analyte in the SDG.
longest wavelength used for
of "2" is assigned to the
number of "1" is assigned to
SDG. A mass number of "2"
The field must be
to obtain data for an
/AVE
3.13.6 Under "1
two decimal pi;
established and
is used for an analyt<
to report the
GTH (nm),/ enter
(to
eaz
use
ther
•avelength in nanometers
lyte for which an MDL has been
MQL column. If more than one wavelength
copies of FORM XI-AAIN as appropriate
3.13.7 Under^atfa&s^" enTser the"ma^s/to charge ratio (m/z, to four
decimal/places) for each analyte for which an MDL has been established
and is/lifted in the MDhvcolumn. If more than one wavelength is used for
an analyse, use other copies\>f FORM XI-AAIN as appropriate to report the
MDL,
3.13. BXUndef^^INTEG. Tl
two decima"iLplacessJ usec
/enter the integration time (in seconds, to
fo/ each measurement taken from each instrument.
3.13.9 Under "BACKGROUND/" enter the type of background correction used
to obtain GFAA data">x|nrer "BS" for Smith Hieftje, "BD" for Deuterium
Arc, or "BZ" for Zeeman background correction.
December, 1991
Page B-36
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.13.10 The Contract Required Quantitation Limits (i
must appear in the column headed "CRQL".
3.13.11 Under "MQL," enter the MQL (in jtg/L to th
determined by the laboratory for each analyte ai
for which the ID Number is reported on this fo
to two significant figures if the MQL value is
significant figures for values above or equal
3.13.12 Under "M," enter the method used t
wavelength or mass used.
3.13.13 Use additional copies of FORM
wavelengths are used. Note that the
the analysis dates in the SDG data pa;
three months.
3.13.14 Under "Comments," enter alternative"
the conditions under which they are used, any
encountered during the MQL analysis, the corrective^
resolution performed for the ss
3.14 ICP AND ICP-MS INTER KT.KMENT
AAIN]
L) in Exhibit C
iecimal places) as
the instrument
reported
three
3.14.1 This form documents the ICP
Factors for each ICP and/or ICP-MS
to obtain data for the jpG-r-^JDnly the
masses used to genera^
3.14.2 The correc
months). A copy
factors must be
ns t rument s and
must not exceed
them by more than
s or masses and
problems
t i on> taken, and
1) [FORM XII -
Interelement Correction
ts that the laboratory used
ient and wavelengths or
be included.
> '
.nnually (every twelve
interelement correction
ackage on FORM XII-AAIN.
3.14.3 Complet
instructions and a
3.14.4 For
correction
the ICP and/.
must notf pr
ormation according to the header
3.14.6 For "It>J>-MS
characters maxi
(formatted as MM/DD/YY) on which these
r use. This date must not exceed
in the SDG data package. Also, it
e than twelve calendar months.
the instrument ID number (twelve
oduce the data for the SDG. If more than
mit additional FORMs XII-AAIN as
enter the instrument ID number (twelve
to produce the data for the SDG. If more than
December, 1991
Page B-37
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
one ICP-MS instrument is used, submit additional FORMs Xdl-AAIN as
appropriate.
3.14.7 Under "WOMN," list the wavelength in nanometers ^60 two decimal
places) for ICP or the mass to charge ratio (m/z/, to reur decimal places)
for ICP-MS used for each analyte. If more than one wavel^ngthor^ mass
is used, submit additional copies of FORM XII-'AA.pN as appropriate.
3.14.8 In the "INTERELEMENT CORRECTION FAC
FOR:" column, enter
correction factor (negative, positive or zero/ to seven decimal places,
10 characters maximum) for each corrected/ analyte analyzed by ICP and/or
ICP-MS. If an analyte was not corrected^for an anaiyt/ that is listed in
the header of a column, a zero must be/enljered to /Ind/cate that the
correction was determined to be zero.,
3.14.9 Use additional copies of FORM XII^kAJN as 4ppropriate if
correction factors for more than six analytes^w^re
3.14.10 Columns of correction
interelement correction must
XII-AAIN according to the alp!
starting on the first FORM XII-
XII-AAIN as appropriate.
3.14.11 Under "Comments," enter
the conditions under which they are
encountered during the
and administrative, tXe correc
for the sample.
3.15 ICP-MS TUNING
3.15.1 This fo
calibration res'
3.15.2 Complete the he^wjer £
instructions .and—as^ folio1
for analytes ffequirirtig
to right s^m'ting on FORM
igmical symbols
e following FORM
wavelengths or masses and
significant problems
analysis, both technical
and resolution performed
[FORM XIII - AAIN]
tuning ariQ^response factor, and mass
-P-MS used to obtain data for the SDG.
rmation according to the header
3.15.3 E6r JJifetRodv!' enfe&r the m&t&bd code (two characters maximum)
accordiiig to 3.3.10.3>v If inore instruments or analyte masses are used,
submit/additional FORMS XjIlXAAIN as appropriate.
3.15/4 $or "Date," enter
initial tinting solution we
exceed th^ ICP^HS analys:
ite (formatted as MM/DD/YY) on which the
re Determined for use. This date must not
ites in the SDG data package.
3.15.5 For "ItR^MS iDvyNo./" enter the instrument ID number (twelve
characters maximunf)xused/to produce the data for the SDG. If more than
one ICP-MS instrument^-is/used, submit additional FORMs XIII-AAIN as
appropriate.
December, 1991
Page B-38
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.15.6 For "Run No.," enter the run number (two characters maximum)
which is the number that applies to a continuous analytical sequence
consisting of prepared samples and all associated quality assurance
measurements as required by the contract. /
3.15.7 Under "Analysis Time," enter the initial' ai
to the following:
me according
3.15.7.1 For "Initial Time," enter the tim/~N£^h military fo
at which each initial tuning solution analysis was performed.
3.15.7.2 For "Final Time," enter the t^me/('in military format - HH:MM)
at which each final tuning solution analysis was performed.
3.15.8 For "% Relative Abundance," eXiterxtzhe initial and final percent
relative abundance according to the
3.15.8.1 Under "Initial," enter the percenb-sjrelatztvce abundance (to two
decimal places) calculated from the intensities-sjneasuTsed, for each of
the isotopes listed, as a result of analyzing the^iOO ppb tuning
solution at the beginning of/eaclr~i€£iUSrun. The isb^jzfpes are listed
in the first column from thef lef£_JLn theTuStnfr-Section of the Form.
3.15.8.2 Under "Final," enter "bhe ^Rercentz'relaErTe-^afeundance (to two
decimal places) calculated from\he\Lnte!nsi/t;Les measured, for each of
the isotopes listed, as a result of analyzing the 100 ppb tuning
solution at the end of each ICP-MS \un. /The isotopes are listed in the
first column from the^leit in the Tuning^Section of the Form.
3.15.9 For "RF100
relative abundance/according
enter tree initial and final percent
3.15.9.1 Under/"!
per second, to ti
at the at thexbegi
ratio listed in
Section of the Form?
tial," e&itar" tnexmeasvnfed response factor (in counts
nearest: whole numbers/in the 100 ppb tuning solution
f each ICP-MS run, for each mass to charge
'olumn from the left in the Response Factor
theNneasured response factor (in counts
st whoie^iumber) in the 100 ppb tuning solution
ICP-MS run, for each mass to charge ratio
from the left in the Response Factor Section
" enter the observed mass (to four decimal
solution at the beginning of each ICP-MS
ratio listed in the first column from the
Section of the Form.
December, 1991
Page B-39
-------
Exhibit B: Form Instructions Guide
Metal
Analvs:
sis of Ambient Air
NOTE: The values measured and reported in the Tuning', Response Factor,
and Mass Calibration Sections of the Form must be wifthi/n the control
limits listed in the second column from the left in each of the Sections.
NOTE: For every initial solution reported there/mu/t^be a f"inal one.
However, the opposite is not true. If a tuninfg aolutiori^as required to
be analyzed in the middle of a run (to avoid exceeding the S^feour rimjlt),
it must be reported in the "Final" section orchis form.
3.16 ICP-MS INTERNAL STANDARDS SUMMARY [FOE
-AAIN]
3.16.1 This form is used to report the
levels for ICP-MS. The relative inten,
standards in all analyses performed
the FORM XIV-AAIN.
Internal sta
ityof each/of,
eac
ICP-1
ds intensity
the internal
.st be reported on
NOTE: A run is defined as the continuous to6a^lty
by an instrument throughout the sequence initiate^by,
initial and the final tuning solution, the first reql
standard and terminated by, ana. incTtRli»g^_the CCV and
the last required analytical aamp^e^Fpr examp
all quality control analyses (rncluding~~tttning solutio
analyses performed
including, the
alibration
ink following
field samples and
calibration
standards, ICVs, CCVs, ICBs, CCBsv MtS, CRIs, ACSsT-tRSs, LCSs, PBs,
duplicates, and matrix spikes) assVeia^ed/witth. the SDG must be reported
on FORM XIV-AAIN. The run must be contitmoufe and inclusive of all
analyses performed on the particular instrument during the run.
3.16.3 Submit one FO]
including instrumen
analyses per run w
XIV-AAIN as appropti
of FORM XIV-AAIN
3.16.4 Completex^he
instructions and a,
3.16.5 For
according
submit
3.16.7
characters maxi
one ICP-MS instr
appropriate
XIV-AA^N per run\f nb more than 32 analyses
ion were perfarme^. If more than 32
d,Ufh~e"n\submic\atiditional copies of FORM
new run mttfctbe started on the first line
ormation according to the header
thod code (two characters maximum)
instruments or analyte masses are used,
appropriate.
the run number (two characters maximum)
es to a continuous analytical sequence
and all associated quality assurance
e contract.
enter the instrument ID number (twelve
produce the data for the SDG. If more than
sed, submit additional FORMs XIV-AAIN as
December, 1991
Page B-40
-------
.Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.16.8 For "Start Date," enter the start date (forma
which the analyses was started. This date must not
analysis dates in the SDG data package.
3.16.9 For "End Date," enter the end date (form
which the analyses run was ended. This date mu
analysis dates in the SDG data package.
3.16.10 Under "EPA SAMPLE No.," enter the
sample in the SDG and of all other prepara
spikes, LCSs, PBs, and repreparations (al
B-2 of this Exhibit). All EPA Sample
increasing temporal (date and time) ordj
next FORM XV-AAIN if applicable. The
analyses not associated with the SDG
the reported analytical run, must be
identified with the EPA SAMPLE NUMBER of
"ZZZZZZ" need not have intensities reported
3.16.11 Under "Time," enter the time (in military
which the analysis was performed!"
as MM/DD/YY) on
the ICP-MS
/DD/YY) on
ICP-MS
ample number ol
such as duplicate!
tted according to Table
isted in
s,/continuing to the
time of other
the instrument in
analyses must be
Samples identified as
1 standards.
NOTE: For any particular ICP-
sequence on FORM XIV-AAIN and
A sample number and time
rAAJiN musbe/~iaei«Jifl4l.
3.16.12 Under "Internal Standards ZD For : ,7 enter the chemical symbol of
the internal standard in the two spaces header field provide to indicate
the internal standard fpjs-which the percent\ differences in that column
were reported.
HH:MM) at
3.16.12.1 In th
whole number)
blank calibrat
standard in tl
form (exclud:
using the follow'
Breeds/difference (to the nearest
internal standard in the
tensity of the internal
sample analyze listed on the
e percent difference (XD) is calculated
Eq. B-16
x 100
3.16.13
or spike is g
five fold diluti
equal to 50%, then
of the internal standard in the blank
and\
|of I internal standard in the EPA sample number
'E" if the %D for a field sample, duplicate,
)X for the second time after being run at a
le percent relative intensity is less than or
the field empty.
December, 1991
Page B-41
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
NOTE: A comment on the appropriate FORMs I-AAIN, VI
explaining which analytes are affected by this flag
NOTE: Columns of internal standard %D must be en
starting with the internal standards of the lowe
XIV-AAIN and proceeding to the following FORM
3.17 Preparation Log [FORM XV - AAIN]
3.17.1 This form is used to report the s
ICP-MS analyses only. In addition, the
must have been prepared in the same ma
dilution or concentration steps. The
the samples listed on this form for e
multiplying each analyte's concentratr
the dilution factor (DF) listed on the
or VII-AAIN
be included.
to right
first FORM
iate.
3.17.2 All field samples and all quality contro
duplicates, spikes, LCS's, PB's and reprepared
the SDG must be reported on FO!
associated with the SDG may be( submitted on
analysis log for ICP and
on this form
-preparation
t'ted'on FORM I-AAIN for
be obtained by
the instrument by
.tions (including
ciated with
tions
3.17.3 Submit one FORM XV-AAIN p^r Method iff ijSTimMse-jfoan 32
preparations including quality con\ror\preparations were performed.
more than 32 preparations per methoa\were/P^f°rmed, then submit
additional copies of FORM XV-AAIN as \pprotrriate.
In
3.17.4 Complete the he'ader ir
instructions and as -foil
jrmation
3.17.5 For "Analwfce,/ enter the name ol
Target Analyte Lj&t /in Exhibi/t C>
ing to the header
analyte as identified in the
3.17.6 For "Ruk^No. T^Ventei: ttfe run number (two characters maximum)
which is the numbelsvthatxappll.es to a continuous analytical sequence
consisting of prepareoS^samplee and all associated quality assurance
measurements as requiredoy the>sontract.
3.17.7 Eo'r "J«s€mment"TbD No. ^^ntfer the instrument ID number (12
characters .maximum) which is the identifier that distinguishes each
instnuaent/used for anaWsis\in the SDG. If more than one instrument is
used./sujnnit additional copies of FORM XV-AAIN as appropriate.
3.1^8 Fo^E^Start Date," /ent^r the date (formatted MM/DD/YY) on which
the ana'lysisisun was star/ced;
3.17.9 For
analysis run
en^er the date (formatted MM/DD/YY) on which the
December, 1991
Page B-42
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.17.10 Under "EPA SAMPLE No.," enter the EPA sample/number of each
sample in the SDG and of all other preparations, such a/ duplicates,
spikes, LCSs, PBs, and repreparations (all formatted according to Table
B-2 of this Exhibit). All EPA sample numbers musf' beO-isted in ascending
alphanumeric order, continuing to the next FORM XV-AAIN>f applicable.
If a sample was reprepared, list the same EPA s;ampl/ex'Bumberxiji the order
of increasing preparation date. ' /
3.17.11 Under "PREP. DATE," enter the date/ffxvrmatted MM/DD/Y^Kpn wh^ch
each sample was prepared for analysis by tjrfe method indicated in
header section of the form.
3.17.12 Under "Final Volume," enter •
nearest whole number) of the preparat
analysis by the method indicated in
field must have a value for each samp
3.17.13 Under "Time," enter the time
which each analysis was performed.
3.17.14 Under "DF," enter th
which the final product of
analysis performed.
NOTE: A DF of "1" must be entere
analyzed without adding any further
solutions to the sample or an aliquo
preparation.
NOTE: For EPA supp,
be entered if the
that specified b
reported in sue!
values on the
supplied with
true value of 250
solution is prepared
on FORM XIV^AAISUand the
true value^of 1250)?
value of^SOdrO-regardle-
ICV must be correctedxfor
following/ formula:
Found vaJ
on FORM
mL, to the
prepared for
the form. This
- HH:MM) at
imal places) by
iluted for each
preparation product was
e/of dilutant or any other
of tfhat sample taken for
such as^ICVs), ICSs, and LCSs, a DF must
used^at a dilution different from
7with the solution. The DF
rould make the reported true
ition equal those that were
'the EPA. For instance, if the ICV has a
aluminum at a 20 fold dilution,- and if the
dilution, a DF of "2" must be entered
instrument reading is compared to a
Iri^Khis example, FORM III-AAIN will have a true
of tnex^ilution used. The found value for the
die dilution listed on FORM XV-AAIN using the
\ue \ = Instrument readout
in
„ nB,
x DF
Eq. B-17
3.17.15 Uhder ">CRx" eiufer/fche percent recovery (to two decimal places)
for each analy^cal spike/analyzed. Leave the field blank if the
analysis reporteoN^s not/an analytical spike.
December, 1991
Page B-43
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.18 Analysis Run Log [FORM XVI - AAIN]
3.18.1 This form is used to report the sample ana/ysi^run log for each
instrument used for analyses in the SDG. This ineludes^any analysis run
where conditions for reporting on FORM XV-AAIN \i/ere/nOt met>\ FORM XV-
AAIN is analyte and method specific.
3.18.2 A run is defined as the totality of
instrument throughout the sequence initiate
required calibration standard and terminated,
continuing calibration verification and plat;
required field sample.
Lyses performed
and including,
5y, and including, the
analys^&s^following the last
3.18.3 All field samples and all quaiity^^ontroj
tuning solutions, calibration standardTs>. IC\
CRIs, ICSs, LRSs, LCSs, PBs, duplicates/>ce^-dige:
spikes, and spike addition analyzed by the
must be reported on FORM XVI-AAIN. The run must^
iparations (including
ICBs, CCBs, MTSs,
(tion spikes, analytical
iiated with the SDG
sinuous and
inclusive of all analyses performed on the particulai
the run.
3.18.4 Submit one FORM XVI-AA
including instrument calibration'
32 analyses were performed in the
XVI-AAIN as appropriate.
3.18.5 Complete the
instructions and as
3.18.6 For "Run N
which is the num1
consisting of p
measurements a,
3.18.7 For "Start
the analysis run was
3.18.8
nent during
32 analyses
'run. If more than
additional copies of FORM
rding to the header
er
characters maximum)
LUOUS analytical sequence
iated quality assurance
er the date (formatted MM/DD/YY) on which
>d code (two characters maximum).
the date (formatted MM/DD/YY) on which the
3.
numl
distin
one instr
appropriate.
3.18.11 Under "EPA
.," enter the instrument identification
maximum) which is the identifier that
used for analysis in the SDG. If more than
submit additional copies of FORM XVI-AAIN as
No.," enter the EPA sample number, including
the QC suffix of each sample (formatted according to Table B-2 of this
December, 1991
Page B-44
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
Exhibit). All EPA sample numbers must be listed in i:
(date and time) order of analysis, continuing to the
for the instrument run if applicable. The analysis/da
other analyses not associated with the SDG but ai
in the reported analytical run must be reported.
identified with the EPA Sample No. of "ZZZZZ
3.18.12 Under "PREP. DATE," enter the date (f<
each sample was prepared for analysis by the
header section of the form.
3.18.13 Under "VOLUME," enter the final
whole number) of the preparation for
the method indicated in the header sec
have a value for each field listed.
3.18.14 Under "TIME," enter the time ( inlailitary^f ormat - HH:MM) at
which each analysis was performed. If an autb*ample"*vis used with equal
analysis time and intervals between analyses, th&HvOnly^the start time of
the run (the time of analysis of the first calibration standard) and end
time of the run (the time of atfalysls--ef-^he final CCV os/CCB, whichever
is later) needs to be reportec
ising temporal
FORM XV-AAIN
and time of
the instrument
ilyses must be
ich
to the nearest
fed for analysis by
This field must
3.18.15 Under "DF," enter the di^uti^n fac/or/(to
by which the final product of the
distillate) can be analyzed within
does not include the dilution inherent^ in
the preparation procedures—in Exhibit D
e decimal places)
procedure (digestate or
tent standard range. The DF
.e preparation as specified by
NOTE: A "1" must be
without adding any
the "Volume" or
that sample.
prepare
lutart
the
NOTE: For EPA
be entered if the
that specified by
reported in
values on the
supplied
true va}/ue fit 2500.0
solution \£ prepared at
on FORM X'tV-AAIN and the
true/value of 1250 Mg/L.
.0 regardless;
rected for/the
product was analyzed
r any other solutions to
listed on FORM XV-AAIN for
by
ICO]
ICV must
following
ns such as ICVs, ICSs, and LCSs, a DF must
ution was used at a dilution different from
ions provided with the solution. The DF
t which would make the reported true
solution equal those that were
For instance, if the ICV has a
aluminum at a 20 fold dilution, and if the
old dilution, a DF of "2" must be entered
rected instrument reading is compared to a
|his example, FORM II-AAIN will have a true
the dilution used. The found value for the
dilution listed on FORM XV-AAIN using the
ELoundValiie _ Instrument readout „ nE,
II-/AAIN ~ in mg/L x DF
Eq. B-18
December, 1991
Page B-45
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.18.16 Under "ANALYZES," enter "X" in the column of/the/designated
analyte to indicate that the analyte value was used /fronf the reported
analysis to report data on any of the forms in the .fiDG.^Leave the column
empty for each analyte if the analysis was not useti to re|xy:t the
particular analyte.
3.19 STANDARD SOLUTIONS SOURCES [FORM XVII - AAIt
3.19.1 This form is used to report the sou:
on an analyte-by-analyte basis for ICVs, 0
LCSs standards used for QC analyses in th
3.19.2 For EPA supplied solutions, ent
EPA solutions must be identified usin;
solutions identification.
3.19.3 For non-EPA supplied solutions, enter
the available twelve spaces to unequivocally
and the solution used.
3.19.4 Complete the header in:
as follows:
3.19.7 Under "
quantitation li:
which the CRI
3.19.8 Under "LRS Stan)
source (twelvj
were repor
3.19.9
standa:
ICS re'su
:e tit each standard solvrt
/CRQLs, LRSs, ICSs, and
.ot sufficient.
upplied with the
t information in
inufacturer
e instructions and
iden
3.19.5 Under "ICV Standard Source,
(twelve spaces maximum) for each ana
reported on FORM II-AAIN.
3.19.6 Under "CCV St
source (twelve space
were reported on
the!' initial calibration source
or/which the ICV results were
continuing calibration
teNfor which the CCV results
3.19
standar
results wer
IB contract required
cimum) for each analyte for
jfrted on FORM III-AAIN.
enter the linear range standard
analyte for which the LRS results
ource," enter the interference check sample
maximum) for each analyte for which the
IRM V-AAIN.
'urce," enter the laboratory control sample
maximum) for each analyte for which ICS
VIII-AAIN.
December, 1991
Page B-46
-------
Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
3.20 SAMPLE LOG-IN SHEET [FORM AADC - IN - 1]
3.20.1 This form is used to document the receipt
shipping containers and samples. One original
for each shipping container.
FOE
spection of
JC-IN-1 is required
3.20.2 If the samples in a single shipping cop
more than one SDG, then the original FORM AADC
the deliverables for the SDG of the lowest
of FORM AADC-IN-1 must be placed with the
SDG(s). The copies should be identified a's "/opy(ies),'
of the original should be noted on the cc
3.20.3 Sign and date the airbill (if
container and record the presence/ab
condition (i.e., intact, broken) in
custody seal numbers in item 2.
,ne the shipping
and their
(RMAADC-IN-l. Record the
3.20.4 Open the shipping container, remove the e
FOJ
documentation, and record on
presence/absence of chain-of-
Packing Lists), and airbills
airbill or an airbill sticker
Record the airbill or sticker
3.20.5 Remove the samples from the
samples and the sample tag (if
sample bottles (i.e., intaet-^broken,
absence of sample tags in item:
3.20.6 Review the/s
information. C
samples, and ci
(i.e., TRs,
ify if there is an
'AADC-iN-i.
container(s), examine the
record the condition of the
and the presence or
AADC-IN-1.
d complete the header
d on all the documents and
item 9 on FORM AADC-IN-1.
3.20.7 If thefexare nbxpr/folems observed during receipt, sign and date
(include time) FOMSAADC^IN-/, the chain-of-custody record, the TR, and
write the sample numbebcon F©I£M AADC-IN-1. For each sample number
entered, entej^-sbe^corresp^ndingN^r volume sampled in standard cubic
meters (std\ m3) in tteappropx^ate^olumn. Record the appropriate
sample tags atIo7"a"s»imedN^borato~*3j/numbers if applicable. The log-in
date shoulclbe recorded atVhe top of FORM AADC-IN-1, and the date and
time of syunple receipt at: tnte laboratory should be recorded in items 10
and YL. /Cross out unused\col\imns and spaces.
3.2t)v8 If^fchere are problfems/observed during receipt (e.g., data on air
volume samplecNj^ missing; for one or more samples) or if an answer marked
with an asterisk ei^e.,/• absent*") was circled, then contact SMO and
document the rfesolutiW of/the problem on a CLP Communication Log.
Following resolutban^, sign and date the forms as specified in the
December, 1991
Page B-47
-------
.Exhibit B: Form Instructions Guide
Metal Analysis of Ambient Air
preceding paragraph and note, where appropriate, the
problem.
solution of the
3.20.9 For "Sample Transfer," enter the fraction designation (if
appropriate) and the specific area designation (e/g. , relFs^gerator
number) in the Sample Transfer block located in /the/b^b^om Ie-£t corner of
FORM AADC-1N-1. Sign and date the sample tran9ter/block>
3.21 DOCUMENT INVENTORY SHEET [FORM AADC - IN
3.21.1 This form is used to record the i
Delivery Group Case file (CSF) documents
3.21.2 Organize all EPA-CSF documents/as
Assemble the documents in the order s
Exhibit B, and stamp each page with tlv
number the DC-IN-2 form). Inventory the
numbers and recording page number ranges in
AADC-IN-2. If there are no documents for a spec
"NA" in the empty space.
of the Complete Sample
to the Region.
Exhibit B.
AADC-IN-2 and
(Do not
the document
provided on FORM
:nt type, enter
3.21.3 Certain laboratory sp<
fit into a clearly defined cate
2 to determine if it is most app
26, 27, or 28. Item 28 should be
These types of documents should be
under each appropriate item.'
to
the CSF may not
»uld review DC-IN-
under items 25,
e is no appropriate item.
or listed in the blanks
December, 1991
Page B-48
-------
Data Reporting Forms
SOW No. XXX - Ambient Air
SECTION 4
DATA REPORTING FORMS
//\\
PAGE NO.
/v ^\
Cover Page - [COVER PAGE - AAIN] /. J . . . X\ . B7-50
Analysis Data Sheet [FORM I - AAIN] .././... ^ B-51
Initial and Continuing Calibration Verification [fORM/II - AAIN] . . B-52
CRQL Standards/Linear Range Standardi^QuartfirlV) LFORM III - AAIN] B-53
Blanks [FORM IV - AAIN] :X • . X B-54
ICP Interference Check Sample [FORM V - AAIN] -^X: • ^X B-55
Spike Sample Recovery [FORM V/ - AAIN] r~r-^-^. . . /7 B-56
Duplicates [FORM VII - AAIN] /
Laboratory Control Sample [FORM
Method of Standard Additions [FORM IXV AAIN]
ICP Serial Dilution;.
- AAIN]
:ors (Annual)
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
Method Quantitat
n
^"*
lits (Quarterly)
ICP and ICP-MS
[FORM XII-
tnt ere lenient/ Correction^
ponse factor Criteria [FORM XIII - AAIN]
ards "s^mmar^vtFORM XIV - AAIN] B-64
XVN AAIN] ^ B-65
AAIN] B-66
Source^ [fORM XVII - AAIN] B-67
[F0»! AADC-IN-1] B-68
Document Inventory Sheet/[FORM AADC-IN-2]
B-69
December, 1991
Page B-49
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
COVER PAGE
Lab Name
Lab Code:
Case No.:
Comments
Y* for Yes or an 'N" for No
If yes,
application o:
x \
I certify that this data package is in compliance with the terms and
conditions of the contract, both technically and for completeness, excluding
> conditions detanedabove. Release of the data contained in this
r data package and in the computer-readable data submitted on floppy
i authorized by the Laboratory Manager or the Manager's
1 by the following signature.
Name:
Title:
Revision MAA01.0
COVER PAGE - AAIN
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM/X EPA SAMPLE NO.
Metals in Ambient Air
ANALYSIS DATA SHEET
Lab Name:
Lab Code:
Case No.:
SAS No.:
SDG No.:
Contract:
Lab Sample ID:
Date Received:
Air Volume Sam,
Date Analyzed/
/ /^x. X^
/ / ^\ ^x
/6V "\ "\
pled/Std. m 3: ^\ /
/
CAS No.
7429-90-5
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-70-2
7440-47-3
7440-48-4
7440-50-8
7439-89-6
7439-92-1
7439-95-4
7439-96-5 7
7439-97-6 C
7440-02-0
7440-09-7
7882-49^2
7440^22-4
7440-23^
^440/28-0
74^6-31-5
7440-62-2
7440^66^6
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copped
Iron7 /• X
Mad/
^lagrfesium
M^iganese /
Molybdenum/
>«
Vanadium j
Zinc /
COr^lCENTRATIOrf /
Mg/L ^~
/ — — ~^-~-
(
\ \ ^~
\ \
\ \,
\ "
\
X \
\
) ^"^
/ ^
/ ^\.
/
X.
^^v^
^ 7
\y
I
L ^J>/
X^^/tg/m/
^\ "
\
~-^~~~^_^_
~~~7 _
/ / — -
r /
/
\
r \
\ >
V
r-7
L/
C
x^
X
x,/
/
j
Q
M
Comments:
Revision MAA01.0
FORM I - AAIN
12/91
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
INITIAL AND CONTINUING CALIBRATION
Lab Name:_
LabCode:_
SAS No.:
SDG No.:
Concentration Units: pg/L
[CATION
nSdurce:
tion Source:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
/"*.. !•!! T..— ,.
\ ^3Ci mi 11 In
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium /-
Silver /
Sodium/' /
Thallium /
Tin/ /
VJanadiuiH^
Zinc\ "\
W
O
M
N
/
*s
r*~ —
,^— ~-
s^
INITIAL CALIBRATION
(ICV)
True
s
/
/ /
/ /
/ /
L .
^^ ^^~
\.
"x
~^-^
^x
•— — ^
^v
Found
/
\
- — -\
\
r ^\
)
/
/ /
/ /
" /
^ ^x
\^
"X,
\
\
\ \
\
/ /
%R
\~
S N
s
\
1^-
/* •
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11 \s
\ /
"
C \pON71NyiNG CALIBRATION (CCV)
CGVNo.:^ /
True^-
—
^7
\ /
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\ /
\ \
\
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m
xfbuncN
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\
x^
~-7
/
CCV No.:
True
>
y
Found
%fi
.
M
Comments:
Revision MAA01.0
FORM 0 - AAIN
-------
Lab Name:
Lab Code:
Case No.:
CRQL:
ICP Source:
ICP-MS Source:
GFAA Source:
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
CRQL STANDARDS/LINEAR RANGE ST
Contract:
/
SAS No.: /
SDG No.:/ /
Concentration
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
^
Potassium
Selenium /
Silver /
Sodium / /
Thallium / /
Tin C ^
Vanadium ^\^
Zinc
W
O
M
N
x"
/
v
x^
CRQL STANDARDS\x.
INITIAL
True
/
/
/
/ ^
^\
." ^
X.
x^^
Found
/"
/ s—
/
/
f
\
X^
x^
x^
. X
X
\
/
/
%R
y
/
\
"X^
**x.
\
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7'
<^
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^X
^
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)
/
FINAL
Found
-~ — >_
^v~ —
\ \
\ S
\
\
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/ \
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s
xy
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—> — .
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s^^
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—
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/
/
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J
^TJNEAR RANGE STANDARDS (LRS)
X^
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^ INITIAL
Found
X /
^*^
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J
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FINAL
Found
*R
• ' :
••
• ••.:••••:
:•'.',
" . : . ."
. .."..
M
rVtmnuMitc- ^X. ^/ /
Revision MAAO1.0
FORM III - AAIN
-------
Lab Name:
Lab Code:
Case No.:
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
BLANKS
Contract:
SAS No.:
SDG No.,
Concentration Units:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Ohroini^TP
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium /
Thallium / /
Tin / /
Vanadium/ /
Zinc x^ ^X.
W
O
M
N
f^-
s*
s
I,
INITIAL CALIB.
BLANK
(ICB)
Cone.
^
/ ,
/ /
/ /
/ /
C \
"V^ "S
\
i --^
1 _^ X
\
N
C
--,
— ^
/
/
J L
4.
"X
\.
\
s N
\
/ /
CONTINUING C/OJBRATIOfTBLANK
/ ftCB] / /
Cone. 1
r —
-------
Lab Name:
Lab Code:
Case No.:
ICP ID No.:
Concentration Units: pgfL
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM/x
Metals in Ambient Air / /
ICP INTERFERENCE CHECK SAMPLE /
Contract: / x^
SAS No.:
SDG No
ICS
ICP
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium /
Silver / /
Sodium / /
Thallium / /
Tin 4 X,
Vanadium ^x^
Zinc ^\
W
0
M
N
i
»— —
x^
TRUE
Sol.
A
/
/ /
/ /
/ /
X
X^
"X
— ~^
"-X,
^\
x^
Sol.
AB
<
^ -^
^ -n.
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/
/
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^ /
s
^x/
x ^V/
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-.
^--7 ^
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J /
/
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\ \
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/
"^^
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\x
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Sol.
A
x^
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X /
7
j
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AB
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.'. ' ,
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. ' ' . :": ':- ."
••• •• • . ' -.
f
" . -,'.""'
M
Comments:
Revision MAA01.0
FORM V - AAIN
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM EPA SAMPLE NO.
Metals in Ambient Air
SPIKE SAMPLE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Concentration Units: /tg/L
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium /
Tin /
Vanadium / /
Zinc \
W
O
M
N
/
/
/
\
CONTROL
UMJT
O6.D
TOT\
/
/
/ /
<. ^
\
,--
^ ^
SPIKED SAMPLE
RESULT
(SSR)
Cone.
r
^
\
X" ~^x
/ /— -^ \
7 ^ l
/ )
/ /
\ / /
V ^ /
"\ \
•^ ^"^
^v \
X \
\ \
} }
1
C
—
v
*\
\
*
^^*~
f*f~~'
\
SAMPL^
/Cotfa.
^ \
"\
^x
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1 ^_
v ^~7 )
\ / /
v V /
\ (
\ \
\ \
\ \/
^ ^— r
\^_/
.
J>
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
DUPLICATES
Contract:
SAS No.:
SDG No.:
Concentration Units: /tg/L
Comments:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
f!«dmiiiTfl
Calcium
CTnmrniiiTn
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver /-"""
Sodium / ^
ThalliuBi /
Tin/ /
Va^adiuln
Zmc^ ^\
W
O
M
N
f
/
X,
•^.
CONTROL
LIMIT
/^~
/ / —
/ /
' /
/ ,, ,
"x^.'-y
^ -
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fc^,- _ •
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X ••->
\
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(S) / /
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X
/^^-.
(^
\ \
\ \
\ N
\
^\
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\ ^- \
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/
/
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AP)/
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f
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\
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7
c
">
y
RPD
Q
M
xy /
Revision MAA01.0
FORM VR - AAIN
12/91
-------
Lab Name:
Lab Code:
Case No.:
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
LABORATORY CONTROL SAMP]
Contract:
GFAA Source:
ICP-MS Source:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
fadmiitm
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver /
Sodium /
Thallium7
/
Vanadium
LCS
USED
\
LOWER UPPEfr-
/
\
\
\
\
V /
\ \
\
\
FOUND
%R
M
Comments:
Revision MAA01.0
FORM VIII - AAIN
12/
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
STANDARD ADDITION RESULTS
Lab Name: Contract:
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
Lab Code:
Case No.:
Concentration Units: /ig/L
/
/
/ /
/ /
4 \
x^
~x
S"
/
^
x
*-
*
x
\
SAS No.:
SDG No.:
/
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
ICP and ICMrtS SERIAL DILUTIO]
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
Contract: __
SAS No.: /
SDG
Concentration Units: /ig/L
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum /
Nickel
Potassium
Selenium
Silver
Sodium/
Thalljam /
Tin/ /
Initial
Sample
Result
(D
\
/ /
X
\
\ \
\
\
\ \
\ \
\
Comments:
JJ_
^Difference
7
M
/
Revision MAA01.0
FORM X - AAIN
-------
Lab Name:
Lab Code:
Case No.:
Date:
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGI
Metals in Ambient Air
METHOD QUANTTTATION
Contract:
SAS No.:
SDGNc
GFAA ID No.:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Vrflomiv^y*
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Tin /
Vanadium /
Zinc /
W
O
M
N
/
/
/ t
^
"X
/ •
/
/ S
/
/
V
WAVE-
LENGTH
(nm)
<
^ ^
/
' /^ ^\
/
/ /
\ / /
^ ^ /
>V ^
^\
"\
\ \
X \
\ \
,
MASS/
(m/z)\
/ " •— .
^
\ \
\ \
\\
\
N
\
^ ^x
/- — \
/
•^
^\
\ /
^>*y
'J£j
\
\
^^_^_
^--7 J
/ /
//
/
. \
\ \
\ }
V
"-7
^J
^BACK-
GJM>UND
k
. \.
\.
\
/
""— '
CRQL
Otg^-)
226
92
> 92
/ 11
7
18
381
44
55
37
126
118
89
15
33
52
758
- 577
229
592
562
155
26
444
MQL
G*g/L)
M
.
Comments:
Revision MAA01.0
FORM XI - AAIN
12/91
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
ICP AND ICP-MS
Lab Name:
Lab Code:
Case No.:
ICP ID No.:
Metals in Ambient Air /^y
CORRECTION ^ACTORS (ANNUAL)
Contract: / <^
SASNo.: /
SDG No.:_
Date:
Comments:
~
ICP-MS ro NO/
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
farimiiim
Calcium
Chromium
Cobalt
Copper ,
Iron /
Lead / /
Magnesium / /
Manganese / /
Molybdenum ^ ^v^
Nickel • ~\
Potassium
Selenium ^ ^
Silver/' „ ^
Sodjum / ^\
Tpallium
*m/
VanaSrum
Zufe^ ""\
W
O
M
N
r
<
\
<*• — \
^_^ ^
' >
1
/ /
/ /
^ /
•\ ^^
"\^
\ ^
\
\ \
\ \
) )
/ /
INT^IUPLEMENT/^RECTION FACTORS FOR:
~?
\
-— _
,.
\ ^
\ \
\ V
\
\
N
s — \
\
\^
\^
. /
^"^
^/,
^ ' /
^\
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— ^.
^7 _^__
/ /
/
(
\
V \
\/
r
/
/
\
•N. ^s
\y
"-^^
/
~~**"^S
•
Revision MAA01.0
FORM XH - AAIN
I2f
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PR(
Metals in Ambient Air
ICP-MS TUNING AND RESPONSE FA<
RESPONSE FACTOR (raont«W second)
(RFO);
X kASS CALIBRATION
'"
In
"•
•n
6.9)60 -/7. 1160)
(5fcg332^-
59.0332)
- 115.0040)
(204.8744 - 205.0744)
Observed Mass
Revision MAA01.0
FORM
- AAIN
12/91
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
ICIHMS INTERNAL STANDARDS SUMMARY
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
Lab Name:
Lab Code:
Case No.:
Run No.:
Start Date:
End Date:
EPA
SAMPLE
NUMBER
/
/
/ /
-' /
/ X,
^\
^
Time
/
/
/ ,
/ 4
.x,
s' ~^-
^
/
x^
\ "\
x^ ^
\^
Contract:
SAS No.:
SDG No.:/
Method:/
ICP-M^ID^
• /7
/ /
/ c
/ ^x ^"x
r
\^ \^
\7
Internal Standards/%!^ For
s*
/
/
/
/
X^ /
\
^ x
x^
\ \
N
\
/
\
/ /
x/ /
/
x^y
Q
/
\
s^
s
s^
)
/
I
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X
""X
\
1
J
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~ — —
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\ \
\ \
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x^^
X /
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\
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s/
^
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X
/
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x/
x^
x^
.— »™» — l
7 r-~^
{ /
/
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4
/
/
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^
- — ,
^ 1 _
/
x^
\ ">
x/
• — ,
/
Q
Q
Revision MAA01.0
FORM XTV -AAIN
12
-------
Lab Name:
Lab Code:
Case No.:
Rim No.:
Start Date:
End Date:
1
2
3
4
5
6
7
8
9
10
11
12
13
14
IS
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
U. S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
PREPARATION LOG
Contract:
SAS No.:
SDG No.j_
Analyte:
Instrument ID
EPA
SAMPLE
No.
PREP.
DATE
S
/ /
T -±_
\
X. \.
Final
Volume
\ \
\ \
\
\
Z
\
\ \
\
/
%R
Revision MAA01.0
FORM XV - AAIN
I2t9
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air
ANALYSIS RUN LOG /N
Lab Name:
Lab Code:
Case No.:
Start Date:
End Date:
Contract:
SDG No.:
SAS No.:
Run No.:
Method: <
/ /
/ /
/ ^\
/ />X\ ^\
x / ^\ \.
Instrument ID No.: • / / ^s\ /
EPA
SAMPLE
No.
PREP.
DATE
j---
s
/ s
/ /
/ /
/ c
V \
\^
\
VOLUME
(mL)
/
/
/
/ /
/ /
c ^
\
..
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16
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20
21
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23
24
25
26
27
28
29
30
31
32
Revision MAA01.0
FORM XVI - AAIN
12/91
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CONTRACT LABORATORY PROGRAM
Metals in Ambient Air /\
STANDARD SOLUTIONS SOURCES /
Lab Name:
Lab Code.:
Case No.: •
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
fadminm
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
M'MlgaiHn'W
Molybdenum
Nickel
Potassium
Selenium
Silver
Thallium
Tin
Vanadium
Zinc
Comment /
/ /
/ /
C ^
ICY
Standard
Source
/
/
/ /
/ /
/ /
c x.
x^
^
_
' ^x
^ "*
\
ccv
Standard
Source
r
<
\
~^^^^--,
^\
/ — x \
) l
I
/ /
/ /
x/ /
s^ X^
x^ ^>
X x
\ \
\ \
) )
Contract:
SDG No.:
SAS No.:
CRQL
Standard/
Source/
/
/ /
/ ^
X^
X
h
T^- .
\ ^—
V \ /
\ \/
\ v /
\ V
\
\
x^
- — -^ ^SN^
X^y
x^
^
/
/ .
/ /'
^/
Standard
/Source
f /
/
/ /
^Xy /
s^ X^
X^ ^
x^
f~ " —
/
\
\
V
7
/
^^
x^ ^x^
\^
ICS
Standard
Source
y
f
^
"x
x^/
7
f
\^
Source
Revision MAA01.0
FORM XVU - AAIN
12/91
-------
Lab Name:
SAMPLE LOG-IN SHEET
Page:.
of.
Received By (Print Name):
Received by (Signature):
, . _/\
Log-in Dater.
Case Number:
Sample Delivery
Group No.:
SAS Number
CIRCLE THE APPROPRIATE
RESPONSE:
1. Custody Seal(s)
Present/Absent*
Intact/Broken
Present/Absent*
Present/Absent*
Aiibfll/Stkkcr
Present/Absent*
2. Custody Seel Nos.:
3. Chain-of-Custody
Records
4. Traffic Reports or
Packing List
5. Aiibfll
6. Airbill No.:
7. Sample Tags
Sample Tag
N ambers
8. Sample Condition:
9. Does information on custody
tfaffic leports, an sample tags
agree. Yes/No*
10. Date Received at Lab:
11. Time Received:
EPA
SAMPLE
#
\ \
SAMPLE7 ASSIGNED
TA(
vC^/ LAR
77
Z
\\
V
LAB
#
/ 7
/r
*If Citclcdy cootftct SMO uid attach racora of rcsoiutioo
Reviewed by: ^^
Date:
Logbook No.: _
Logbook Page No.:
AIR
xSuPMENT
ETC.
REMARKS:
CONDITION
Revision MAA01.0
FORM AADC-IN-1
12191
-------
METAL IN AMBIENT AIR ANAL
COMPLETE SDG FILE (CSF)
INVENTORY SHEET
Lab Name:
Case No.:
SAS No.:
SDG No.:
Contract No.:
SDG Nos. to FolW:
City/Staie:/
All documents delivered in the complete SDG Hie musrbe/original documents where possible.
(Reference Exhibit B, Section 3) / / /x
/ / PafeeNbs. (Please Check:)
Lab
1. Inventory Sheet (AADC-2) (Do not number)
2. Cover Page
3. Inorganic Analysis Data Sheet (FORM I-AAIN)
4. Initial & Continuing Calibration
Verification (FORM H-AAIN)
5. CRQL Standards/Linear Range Sfc
(Quarterly) (FORM IH-AAIN)
6. Blanks (FORM IV-AAIN)
7. ICP and ICP-MS Interference Check Sample
8. Spike Sample Recovery (FORM VI-AAIN)
9. Duplicates (FORM
10. Laboratory Control Sample/
11. Method of Standard ,
12. ICP and ICP-MS 1
13. Method Detection L
14. ICP and ICP-MS i
(Annual) (FORM:
IS. ICP-MS Tuning and.]
(FORM xm-/
16. ICP-MS Internal Standards i
17.
Log (B) (FORM
Revision MAA01.0
FORM AADC-IN-2 (Page 1 of 2)
12/91
-------
METAL IN AMBIENT AIR ANALYTES
COMPLETE SDG FILE (CSF)
INVENTORY SHEET
23. EPA Shipping/Receiving Documents
Airbill (No. of Shipments )
Chain-of-custody Records
Sample Tags
Sample Log-In Sheet (Lab & HDC-1)
SDG Cover Sheet
24. Misc. Shipping/Receiving Records
(list all individual records)
Telephone Logs
25.
26.
27.
Internal Lab Sample Transfer Records &
Tracking Sheets (describe or list)
Internal Ohginial Sample Preparation
(describe or list)
Preparation Records
Analysis Records
Description
Other Records (describe or
Telephone Communicai
28. Comments:
(Print Name & Title)
(Print Name & Title)
(Date)
(Date)
Revision MAA01.0
FORM AADC-IN-2 (Page 2 of 2)
12/91
-------
-------
Exhibit C
Metal Analysis of Ambient Air
TABLE 1
METALS IN AMBIENT AIR
TARGET ANALYTE LIST (TAL) AND
CONTRACT REQUIRED QUANTITATION LIMITS
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Tin
Vanadium
Zinc
ct Required
Limit1-2-3
CAS RN
7429
7440
7440
7440
7440
7440
7440
7440
7440
7440
7439
7439
7439
7439
7439
1313
7440
7782
7440
(1) The analytica^ methods specified in Exhibit D, Sections 3 and 5 must be
utilized and the achieved instrument detection limits must meet the Contract
Required Quantitacion Limits (CRQJL) requirements. Higher detection levels may
only be used in the followihgvCircbostance:
concStMyration^excee^s two times the detection limit of the
tod itv. use, Che^yvalue may be reported even though the
detection limit may not equal the contract
red/ quantitation\lim£t. The method detection limit must be
ibits D.
If the s
instrument
inst:
requ
doc
(2)
blank pre
tnced as described \n
se CRDL's are the method
rations that must be
Jtection limits obtained from actual method
using the procedure in Exhibits D.
ir Hi-Vol filter and 40 mL final extract volume.
id 5.11.2 for calculations.
December, 1991
Page C-l
-------
Exhibit C
Metal Analysis of Ambient Air
TABLE 2
METALS IN AMBIENT AIR
TARGET ANALTTE LIST (TAL)
CONTRACT REQUIRED QDANTITATION
FOR ICP-MS ANALYSES
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Cobalt
Copper
Iron
Lead
Manganese
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
CAS RN
7429
7440
7440
7440
7440
7440
7440
7440
7440
7439
7439
7439
1313
7782
^440
Contract Required/
Quantitation Limit1*2
itg/L
226
92
92
11
7
18
44
55
37
126
118
15
52
577
229
562
26
444
(1) The ICP-MS method/specif iifa rfi Exhibit if, Section 4 may be utilized
provided the documented^raethod/defection Krafts meet the Contract Required
Quantitation Limit CSJL)it*gu*reoents.
(2) The CRQL is the methoU^detefeC^on limits obtained in pure water that must
be met using the opaoadure in Exb4£itDv.The method detection limits for samples
may be considerably higherxdepend£ngoiifche sample matrix.
(3) Ass
See Exhibi
r Hi-Vol filter and 40 mL final extract volume.
or \calculations.
December, 1991
Page C-2
-------
Exhibit C
Metal Analysis of Ambient Air
Interference
C O1UDOT1GD t
Al
Ca
Fe
Mg
Na
P
K
S
C
Cl
Mo
Ti
As
Cd
Cr
Co
Cu
Mr.
Ni
Se
Ag
V
Zn
TABLE 3
INTERFERENCE CHECK SAMPLE COMPONENTS/
CONCENTRATIONS FOR ICP AND ICP-1
Solution A
Concentration (mg/L)
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
,000.0
,600.0
10.0
1
100
0.050
0.100
200
0.100
0.100
200
100
0.100
0.200
0.100
December, 1991
Page C-3
-------
Exhibit C
Metal Analysis of Ambient Air
TABLE 4
INITIAL AND CONTINUING CALIBRATION
CRQL STANDARD CONTROL LIMITS, AND LCS STANDARD CO!
FOR INORGANIC ANALYSES
INITIAL AND CONTINUING CALIBRATION
CATION LIMITS
Analytical Method
Inorganic
Species
e Value CEPA Set)
imit High Limit
ICP
ICP-MS
GFAA
Metals
Metals
Metals
110
110
110
CRQL STANDARD
Analytical Method
ITS
X of True Value (EPA Set)
Low Limit High Limit
ICP
ICP-MS
GFAA
85
85
85
115
115
115
The LCS
limits
ARD CONTROL LIMITS
/dard Control Limits apre the same for all inorganics species. The
L20 percent.
December, 1991
Page C-4
-------
EXHIBIT D
ANALYTICAL METHODS FOR
OF METAL COMPOUNDS
HI-VOL FILTERS AND ANAL'
INDUCTIVELY COUPLED PLASMA (ICP)
EMISSION SPECTROMETRY, INDUCTIVELY COUPLED
SPECTROMETRY (ICP-MS^TORr-GRAPJITE FURNACE
ABSORPTI01
-------
EXHIBIT D
ANALYTICAL METHODS FOR THE DETERMINAT]
COMPOUNDS COLLECTED ON HI-VOL FILTERS
INDUCTIVELY COUPLED PLASMA (ICP) ATOMIC
INDUCTIVELY COUPLED PLASMA MASS SPECTRbMEtfRY (ICP-MS) OR
GRAPHITE FURNACE ATOMIC ABSORPTION OGFA/6 SPECTROMETRY
PAGE NO.
SECTION 1 INTRODUCTION >x, . /\ D-1
SECTION 2 SAMPLE PREPARATION AND
RELATED HANDLING PRO
SECTION 3 SAMPLE ANALYSIS BY ICP . \ . \ .././. D-ll
SECTION 4 SAMPLE ANALYSIS BY ICP-MS
D-3
SECTION 5 SAMPLE ANALYSIS B'
SECTION 6 BIBLIO
SECTION 7 TABLES
D-38
D-66
D-89
D-91
SECTION 8 FIGURES . . . >w . . >x. " D-104
December, 1991
-------
Exhibit D
Metal Analysis of Ambient Air
SECTION 1
ANALYTICAL METHODS FOR THE DETERMINATION
COMPOUNDS COLLECTED ON HI-VOL FILTERS AND
INDUCTIVELY COUPLED PLASMA (ICP) ATOMIC EMISS,
INDUCTIVELY COUPLED PLASMA MASS SPECTROME!
GRAPHITE FURNACE ATOMIC ABSORPTION (GFA^)
1. INTRODUCTION
1.1 SCOPE AND APPLICATION
1.1.1 The methods specified in Exhibit'D rfiust be risedf and the
documented instrument or method detection/limits must/meet the Contract
Required Quantitation Limits (CRQL) m the undiluted and diluted
proof that dilution was
ed and undiluted sample
All sample dilutions
,y acidified to maintain
1.1.3 The Cont/ac
compendium of requ:
performance of ^analyst
assurance/quality
performed in associat
Exhibit E.
is reminded and^cautifoned that Exhibit D is a
ed and permitted analytical methods to be used in the
contract. The quality
(QAyQC) procedures or measurements to be
witnvthese methods or analyses are specified in
cautioned that the collection and
may not be referred to within the individual
;he^Quality Assurance Protocol of Exhibit E. The
ireWnts are specified in Exhibit B. Raw data
sociation with the performance of analyses
shall Conform to the appropriate provisions of
1.1.5 Laboratory gias^wa/e to be used in metals analysis must be acid
cleaned according^© EPA'yS manual "Methods for Chemical Analysis of Water
December, 1991
Page D-l
-------
Exhibit D
Metal Analysis of Ambient Air
and Wastes" or an equivalent procedure (see part 2.1/6.3$. Samples must
be opened and digested in a hood. Stock solutions tto be used for
preparing instrument or method calibration standards ra^y be purchased or
prepared as described in parts 3.6 and 4.6. All yother sections to be
used for QA/QC measurements shall conform to the/spe'&ific requirements of
Exhibit E.
1.1.6 Background corrections are required
Each GFAA analysis requires a minimum of tw/d
during full Method of Standard Additions
measurements shall require a minimum of
Appropriate hardcopy raw data for each
included in the data package in accorc
of each set of exposures/injections si
sample analysis, and reporting as speci
must be reported in the raw data in concei
11 GFAA measur
infections (burns)
). All ICP and ICP-MS
ixposures.
:on shall be
ib/t B. The average
standardization,
it D. All exposures
its.
December, 1991
Page D-2
-------
Exhibit D
Metal Analysis of Ambient Air
SECTION 2
SAMPLE PREPARATION
2.1 MICROWAVE EXTRACTION AND RELATED HANDLING PROG
2.1.1 Introduc t ion
2.1.1.1 This Section describes a microw,
extract the metals from the particulate
Following microwave extraction, target a
ICP-MS, or GFAA.
2.1.2 Sample Preservation
2.1.2.1 Ambient air glass-fiber
half lengthwise with the particulate
protective envelopes. These protective
to 30°C until analysis.
2.1.2.2 The maximum sampl
days. To be compliant with
samples within 180 days even
data submission times allowed
2.1.3 Summary of Method
2.1.3.1 A 1" x 8"
in the Federal Reference Met!
11). The metals a/e eaffrltsted'
acid/nitric acid vsoluxion usVn,
After cooling, ^ne ^igestate/ is
material.
lass-fiber
ces are analyzed by ICP,
e received folded in
'ard and enclosed in
be stored at 15
under this^bo&tract is 180
actor must analyze
in the maximum
x 10" filter as described
Figure D-l and Reference
strip by a hydrochloric
microwave digestion system.
ed to remove any insoluble
2.1.3.2 Mi6spwaves>extr4cti:on is used to prepare samples for ICP
analysis. ThisnteJ^iodcusLng nitric acid only) or an alternate hot
extraction technique^sajy be^s^sed to prepare samples for ICP-MS and GFAA
analysis.
rials
ve system and capping station: With
up to 600 watts (see Figure D-2).
Ni
the
corrosion"
protected ag
home-use microwave shall NOT be used for
er this contract. The oven cavity must be
well ventilated. All electronics must be
osixm for safe operation.
December, 1991
Page D-3
-------
Exhibit D
Metal Analysis of Ambient Air
2.1.4.2 PFA Teflon digestion vessels: Capable
pressures of up to 100 psi. Pressure venting ves
controlled pressure relief at pressures exceedin;
mL capacity).
istanding
/capable of
psi. (60- to 120-
2.1.4.3 Teflon PFA overflow vessel:
capacity).
Doub
2.1.4.4
oven.
Rotating table: For uniform
2.1.4.5 Volumetric glassware: 50-
borosilicate).
2.1.4.6 Bottles: Linear polyethy
caps, for storing samples; Teflon bottf
standards (500-mL, 125-mL, and 30-mL).
2.1.4.7 Centrifuge tubes: polypropylene tube
polypropylene, 50-mL (Nalgenc
acity (Class A
ipylene with leakproof
multielement
:w tops of
acy of setting of
''Automatic
2.1.4.8 Pipette: Automati
0.1 mL or better and repeatability
Dispensing Pipette, Model ADP-SO^ o\ equivalent).
2.1.4.9 Rack: Wire (Fisher 14-79$-!) /r polypropylene (Fisher 14-
8090), for holding
2.1.4.10 Particle
handling glass-fiJ
tubes during, shaking.
No\ 8500) : 1?o beNworn while cutting and
•er /filters
2.1.4.11 Centri
(Internationa]
Eug«s: Capable
Equipment
speeds of 2000 rpm
Model>wK or equivalent) .
2.1.4.12 Template
Federal Register 19"
2.1.4.13
To"vktd £n sectioning the glass-fiber filter.
,43 (Oc^. 5), 46258-46261. (See Figure D-l).
ThitVxwheelN>(< 1 mm) .
Eberbach Corporation Model 6460 or
2.1.5.2 Nitrl
eqivalent), for pr€
: American Chemical Society (ACS) reagent
(or equivalent), for preparing samples.
Redistilled spectrographic grade (16M) (or
ng samples.
December, 1991
Page D-4
-------
Exhibit D
Metal Analysis of Ambient Air
2.1.5.3 ASTM Type II water (ASTM D1193).
2.1.6 Microwave Extraction Procedure
2.1.6.1 Microwave Calibration Procedure
2.1.6.1.1 Calibration of the microwave unit: is/a critical s"bep prior
to its use. In order that absolute power Settings may be^interbhanged
from one microwave unit to another, the a/fbual delivered powe^must
determined.
2.1.6.1.2 Calibration of a laborato
depends on the type of electronic sy
the unit has a precise and accurate/li:
output power and the scale used in/confer^llin
then the calibration can be a single^poin
power. If the unit is not accurate or
controlling scale, then a multiple-point
the unit power calibration needs multiple-
point where the linearity begins must be i
calibration at 100, 99, 98,
power settings can be appl
portion of the calibration (Jurvev can~~bie—excluded
Each percent is equivalent
(see Figure D-2)
manufacturer. If
iorfship between the
microwave unit.,
ation at maximum
some portion of the
>n is necessary. If
calibration, then the
example, a
60,^knrif 50 percent
The nonlinear
estricted in use.
5 W and becomes
the smallest unit of power that\can\be/coEftrolled. If 20 - 40 W are
contained from 99 - 100 percent .^thab/poirion of the microwave
calibration is not controllable byXthre/ to seven times that of the
linear portion of the^-e«n^rol scale\nd\rill prevent duplication of
precise power conditions specified in^hatyportion of the power scale.
2.1.6.1.3 The
available for
measuring the
electromagne
are made onS*eighe
room temperatur
(Teflon) vessels.
through the
are r
stirr
use
owingXp'aragraph evaluate the power
ivity. This is accomplished by
water exposed to
riod of time. Measurements
(five replicates) of 1 kg samples of
water in thick-walled microwave transparent
iners must be 'circulated continuously
minutes at full power. The vessels
the contents are stirred. After
e of^the/water is measured and recorded for
wit:
Irradia
90, 80, 707
container must?
ial temperature of the water, (T4) , to
temperature should be between 22 and 26°C.
r sit full power, 100 percent (99, 98, 97, 95,
rcent power setting) for 120 seconds. The
lated through the cavity at a rate of at least
December, 1991
Page D-5
-------
Exhibit D
Metal Analysis of Ambient Air
one revolution every 30 seconds during the irrs
final temperature of the water, after stirring,
while stirring the water (an electronic stirrer,
works best) within 30 seconds of the end of
maximum reading. Repeat for a new sample, i
replicates per microwave setting, of distilled room-
using a new, clean container. Calculate tt
to the formula:
Power =
Measure the
0.1CC,
bar
ding
34.87 =
where:
Power
K =
CP
M
T
t
2.1.6.2.2 Deri
range and det
setting seal
appropriate
microwave unit
actual power
2.1.6.3
The apparent
joule-sec'2) ^
The conversions
to W (equal to
The heat capacity^
- 1.0
The ma**—of the samp}
in
Eq. D/IN-2
Eq. D/IN-3
sample in watts (W -
ical calories-sec"1
capacity, or specific heat
ter);
grams;
inear portion of the calibration
va. watts of the arbitrary
?atts to determine the
microwave unit being used. Each
ts own setting that corresponds to the
ne samples.
Vessels
use, new vessels must be annealed before they
sntYcleaning procedure must be followed. This
the vessels for 96 hours to 200°C. The
bbled during annealing and the sealing surfaces
ir the rim) must not be used to support the
2.1.6.3.2 "'Rinse v>i£& distilled water. Immerse in a cleaning bath of
1:1 HC1 for a minimum of three hours after the bath temperature has
reached a temperature/just below boiling. Rinse with distilled water.
Immerse in a cleaning bath of 1:1 HN03 for a minimum of three hours
December, 1991
Page D-6
-------
Exhibit D
Metal Analysis of Ambient Air
after the bath temperature has reached a temperature^ jUst below
boiling. The vessels are then rinsed with copious/ampunts of
deionized, distilled water prior to use for any analyses under this
contract. Between sample digestions, the PFA ve'sse^s should be
detergent washed and 1:1 HN03 rinsed followed by a detonized, distilled
water rinse.
2.1.6.4 Digestion Procedure for Microwave
2.1.6.4.1 Prepare extracting acid (2M H
analysis. In a 1-L volumetric flask, c
500 mL of deionized, distilled water
redistilled spectrographic-grade nit
reagent-grade concentrated hydrochl
to 1 L with deionized, distilled w,
NOTE: Nitric and hydrochloric acid
we11-ventilated fume hood. Mixing
Stir slowly.
2.1.6.4.2 Prepare nitric aoid
analyses. In a 1-L volumetric
500 mL of deionized distilled, wa
acid. Slowly dilute to 1 L.
in order and mix well
icentrated (16M)
.5 mL of ACS
Cool and dilute
Lask combine
Prepare in a
.o thermic reaction.
P-MS and GFAA
der and mix well,
ter
)2 mL of concentrated nitric
2.1.6.4.3 Cut a 1" x 8" strip frfcm i:he folded particulate bearing
filter using a template and a pizzaVcutrer as described in the Federal
Reference Method forLead^Osee Figurk D-\ and Reference 11). Using
vinyl gloves or plastic forbeps, accor^lon\fold or tightly roll the
filter strip and plac/rTtxon ^ts edge in\a centrifuge tube.
cask an<
NOTE: A breathing
personnel handling dry gl
prevents the Anh
material. ^
also prevent co:
glo
Lation
NOTE: It is
extracte
analysis.
zested
ensui
are required for safety of
The breathing mask
minute glas's—shards and particulate
te/t the skin from the same materials and
of the sample by skin secretions.
mor-e^than one strip from a filter be
samjJS»e volume for sample and QC sample
*6.4/4 Add 10.0 mL o
xtracting acid for ICP analysis or 10 mL of
nicric acid for GFAl^ oi ICP-MS analysis , using a preset calibrated
au'tometic dispensing pipette or Class A regular pipette. (The acid
ld c«ver the strip comp/letely) . The sequence of adding the filter
stripxand ate4.d to the orentrifuge tube may be reversed, if more
convenietu^, wrfcbout affecting the results. Place the centrifuge tube
in a TeflonNKFA ve^*§£l containing 31 mL of deionized water.
December, 1991
Page D-7
-------
Exhibit D
Metal Analysis of Ambient Air
2.1.6.4.5 The caps with the pressure release valves ^re placed on the
vessels hand-tight, and then tightened using constant torque to 12
ft./lbs. Connect the sample vessel to the overflow/vessel using the
Teflon PFA connecting tube. Weigh the two vessel assembly to the
nearest 0.01 g. Place the vessels in the mic/owave^carobsel. Connect
the overflow vessels to the center well of the dven (s^e Figure D-2).
2.1.6.4.6 Place the 12 vessels on the turfrtkble of the micrbwave
Any vessels containing 10 mL of acid soli/tion for analytical bis
purposes are counted as sample vessels./ Irradiate the sample vessels
at 486 W for 23 minutes. (Based on th/ cauibratiotwof the microwave
as previously described).
2.1.6.4.7 At the end of the program, Remove ttfe tzurntable containing
the microwave vessels and cool it rn^tap water far 10 minutes. Open
the microwave vessels and discard the waiter tha/ they contain.
the centrifuge*
)ecant the
2.1.6.4.8 Add 10 mL of deionized distilled
tube, using the preset calibrated automatic disp
using a Class A regular pip<
mechanically shake for five( mir
and operate for 25 minutes
from the centrifuge tube into^n \reighec
polypropylene bottle (bearing sajnpl^ ID/1<
disturb the solids in the bottom
contents. The matrix is 0.45M nitfejlc ac,
for ICP analysis or l^Slt^nitric aci
deionized, distille
-------
Exhibit D
Metal Analysis of Ambient Air
2.2.3.3 Centrifuge: Capable of maintaining speed^ oE 2000 rpm
(International Equipment Company Model UV or equivalen/).
2.2.3.4 Centrifuge tubes: Polypropylene tubes/an<( screw tops, 100-
mL.
2.2.3.5 Pipette: Automatic dispensing wit;
better and repeatability of 20 pL, (Grumman
Model ADP-30 DT or equivalent).
2.2.3.6 Particle, mask: To be worn
fiber filters.
2.2.3.7 Template: To aid in sect
Federal Register 1978, 43 (Oct. 5),
2.2.3.8 Pizza cutter: Thin wheel (<"
2.2.4 Reagents
2.2.4.1 Nitric Acid (HN03)/ CJoT
spectrographic grade.
utting and handling glass -
-fiber filter.
fee Figure D-l.
illed
2.2.4.1.1 Nitric Acid, 3M: Pr>par« by aidiifgTSS-wtf of concentrated
nitric acid (2.2.4.1) to distilled, \eianized water and slowly diluting
to 1 L. \ V /
NOTE: Nitric acid fume*—ate toxic, ^repa^re in a well-ventilated fume
hood. Stir slowly.
2.2.4.2 ASTM
2.2.5 Sample
2.2.5.1 Ex]
particulate mate
stored at 15 to 30°
2.2.6
'ater must be monitored.
should be folded in half with
enclosed in protective envelopes, and
lysis.
2
Ai
with
corrosiohxprodui
*x^
analytes) ar
s£rip as described in the Federal Reference
D-l),
half twice, and place in a 150-mL beaker.
Letely cover the sample. Cover the beaker
Important to keep the sample covered so that
(formed/on fume hood surface which may contain target
in the extract.
December, 1991
Page D-9
-------
Exhibit D
Metal Analysis of Ambient Air
NOTE: It is suggested that more than one strip per
to ensure adequate volume for sample and QC analys
2.2.6.3 Gently boil the sample in a beaker o
fume hood for 30 minutes. Do not let the samp
NOTE: Nitric acid fumes are toxic.
2.2.6.4 After 30 minutes, remove the be
cool to near room temperature. Rinse watch
with distilled, deionized water.
2.2.6.5 Decant extract and rinsing;
Add distilled, deionized water to thj
watch glass and set aside for a mini
critical step and cannot be omitted
the filter to diffuse into the rinse water.
2.2.6.6 Decant the water from the filter into
rinse filter and beaker twice/wTtlr~dTrs£il.led,
the rinse to the volumetric rlaskjintil the
r be extracted
under a
.o dryness.
and sides of beaker
volumetric flask.
beaker, cover with
This is a
s the HN03 trapped in
deionize
2.2.6.7 Stopper flask and sha&e Irigorox
approximately five minutes or until
l/ ~atttt-s«'fc aside for
dissipated.
2.2.6.8 Bring solution to volume with distilled, deionized water, and
mix thoroughly. Allow^eeiu^ion to sec^le \or one hour before proceeding
with analysis.
NOTE: Do not fil
because of possible
final extract
any suspended
trie flask,
ater, and add
olume is 80 to 85 mL.
emove particulate matter
clue to filtration. The
for 30 minutes to remove
2.2.6.9 If s
to a polyethylene bo
solids.
2.2.6.1
HN03
2.2/6.Li Blank filter s
digestion blanks should
reaeentsNised.
e stored for subsequent analysis, transfer
careful not to disturb the settled
traction procedure are now in 0.45M
should be extracted and analyzed, and
to ensure low levels of metals in the
December, 1991
Page D-10
-------
Exhibit D
Metal Analysis of Ambient Air
SECTION 3
SAMPLE ANALYSIS
BY
INDUCTIVELY COUPLED PLASMA (ICP) ATOMIC EMIS;
3.1 INTRODUCTION
3.1.1 Metals for which this method is appli
Exhibit C, and are determined by ICP after
digestion. Appropriate steps must be taken/to/correct
interference effects.
3.1.2 Table D-l lists analytes along
typical estimated instrumental detect!
pneumatic nebulization. Actual worki
dependent and as the sample matrix varies^
vary. In time, other analytes may be added a
available.
3.1.3 Because of the differen
satisfactory instruments, no
can be provided. Instead, the
provided by the manufacturer of the
ive
ts are sample
may also
ormation becomes
arious
3.2 SUMMARY OF METHOD
3.2.1 The analyte conc^;
spectroscopic analysis/
nebulizer. The aero
plasma and the
and ionic line emi
are produced when/th
The spectra are
line radiation(
photomultiplier tul
tube will increase in
element in the sample wit'
The photocuprent is~~|JJ«
-------
Exhibit D
Metal Analysis of Ambient Air
ences are
.e type of
the
of the calibration
le analyses
optional use of
necessary.
interferences. Recommendations for correcting for int
briefly summarized below under headings that categori
interference that is being considered.
3.2.3.1 Recommended Corrections for Physical
The use of peristaltic pump to introduc*
nebulizer.
Frequent (20 percent or better) ana
stability standard.
Adequate rinsing (one minute or
using ten percent HN03 or ten px
humidified argon or a nebulize
3.2.3.2 Recommended Corrections for
Matrix matching between samples and all
diluting the sample dury
3.2.3.3 Recommended Correcti<
sample
ces
Use of calculated interele;
or first or second order equa
function (on-peak correction).
Optional use o
both sides of
Optionally,
waveleng
calibrat
performe'
3.2.4 Every solution?
method blanks, and
exposures
quantitat
times
MQL and
ons in the form of factors
describe the interference
:d shift on either side or
correction).
of the analyte element
imultaneously plotted with a
ion standard scan may be
refere;
3.2.6 If the*
any analyte is
reported value is to
calibration standards, calibration and
is, must be analyzed using two full
Is sufficient to meet the method
?r each^anadyte emission line. All exposure
LI analyses and all quarterly analyses (i.e.,
factor.)
round) and on-peak (interelement
tions) interference corrections made for
and reported with the analysis results.
.ues of the interference corrections) made on
the resulting analyte concentration, the
agged with an "I" on FORM I-AAIN.
December, 1991
Page D-12
-------
Exhibit D
Metal Analysis of Ambient Air
3.2.7 If the analyte requiring dilution interferes
the interference corrections) must reflect the ac
the interferent in the undiluted samples.
3.2.8 The specific spectral lines that are empl
3.2.9 All reported analyte data must have bee
linear range of the respective analyte emission
concentration results in the linear range of
exceeded, the sample must be diluted such tfcat
concentration falls within the linear ran
3.3 SAFETY
3.3.1 The toxicity or carcinogenici
method has not been precisely defined;
should be treated as a potential health
responsible for maintaining a current
regarding the safe handling of the chemicals spec
reference file of material handling data sheets
personnel involved in the chemicaT
.nother analyte,
icentration of
e reported.
t not below the CRQL.
awarene
3.4.2 Spe,
such as s,
to syst
are ma<
quant
corr<
exac
correct
overlap anoStjackg
the metals ca
performed on a
ca
electron/
within t
ant addit
used in this •
chemical compound
laboratory is
OSHA regulations
this method. A
ilable to all
3.4 INTERFERENCES
3.4.1 ICF emission spectroscopy
in practice are experienced in two
translation of the analytical curve a:
increase in background
continuum and/or scat
matrix and spectral
that is independent
of the analytical
sensitivity, is
performance pro
changes in the
metals. Both fo:
particular sample matr
Interelement effects, which
Interferences that cause a
ed by spectral line overlap or
al ion recombination
spectrometer. For a given
e interference is produced
Rotational interference
.ally as a change in
f variations in nebulizer
les of the sample solution and
'tions in the plasma caused by the matrix •
can operate .simultaneously for a
broa
rly resolved metal spectral lines,
itinuum spectral background, will lead
lytical results unless proper corrections
emission will lead to a deterioration of the
rease the difficulty of off-peak background
ing translational interference (other than
andards to the sample) include the on-peak
thod can be applied to both spectral line
ement, but it requires specific knowledge of
ference. On-peak correction can only be
basis if the interfering metals are included
December, 1991
Page D-13
-------
Exhibit D
Metal Analysis of Ambient Air
in the multi-metal analysis, although uncertainties
whether the correction coefficients employed match
particular sample matrix.
lose
:ill exist in
'required for the
3.4.3 Rotational calibration curve interference/
given matrix and spectral line as a change in ttj
calibration. This type of interference indue
transport effects, often called physical i
diffusion interferences; and chemical interfi!
vaporization interference and ionization interferences. Such
interferences can be reduced by matrix matching of thexstandards and
samples and by the method of standard additions, (aLChoygh standard
additions can become quite lengthy and impracticable far multi-metal
analyses) and by the use of internal standards. Matrix matching can
correct for any of these interferences B^t thVvCOTreyCtion is dependent on
the accuracy of the matching. Variations Jxi the matrix from sample to
sample will cause corresponding inaccuracies rn^the analyte results.
ourpose,
3.4.4 Listed in Table D-2 are some interference ef
recommended wavelengths given i
intended for use only as a rudi^nen^ajry^ guide
potential spectral interference
between concentration and intensify ftect the
can be assumed. The interference
Ames Laboratory (USOOE, Iowa State Urtivei
expressed as analyte concentration equiyalei
concentrations) arising ^ffeo-4pO mg/L ors.the'
the
The data itNiyble D-2 are
indication of
ar relations
the interferents
>n/ which was collected at the
Ames, Iowa 50011), is
'ts (i.e., false analyte
interferent element.
3.5 APPARATUS AND EQUII
3.5.1 Computer-
spectrometer sysl
»lled inductively
Lth:
plasma atomic emission
Polychromato^wit
the metals can
instrument that a3
for this me]
hardd
units or
concentratid'
3.5.2 Argon gas sup
ed dispersion and detector system such that
detfermijied simultaneously, or a sequential scanning
evement of the quality control requirements
3ling system;
ng both off-peak (background correction)
f first or second order regression
:ed interference) spectral interference
the software must be capable of creating a
ypes of corrections in either concentration
density data along with net calculated
Welding grade or better.
December, 1991
Page D-14
-------
Exhibit D
Metal Analysis of Ambient Air
3.5.3 Assorted laboratory volumetric glassware, pipe
id micropipets.
among various
operating
Ld follow the
Instrument.
Die
for
3.5.4 Operating conditions: Because of the differej
makes and models of satisfactory instruments, no del
instructions can be provided. Instead, the analyst
instructions provided by the manufacturer of the
Sensitivity, instrumental detection limit, precis
range, and interference effects must be investi
each individual analyte line on that particulaj"Mj
measurements must be within the instrument li/hear range where
factors are valid^It is the responsibility7of/the analyst to verify^ehat
the instrument configuration and operating/conditions used satisfy
analytical requirements and to maintain cmalircy controiMata confirming
instrument performance and analytical re,sul£s.
3.6 REAGENTS AND STANDARDS
3.6.1 In the determination of trace elements, containers can introduce
either positive or negative errors in the measubamentbf. trace elements by
contributing contaminants through leaching or surface description and
>tion.
analysis
depleting concentrations throuj
treatment of the samples prior/to
The following cleaning treatment^ se<|tie«ce_Jias been
adequate to minimize contaminate
borosilicate glass, linear polyettf
ASTM Type II water, 1:1 hydrochlori
acid, and ASTM Type I water.
Thus the>s
-------
Exhibit D
Metal Analysis of Ambient Air
be required
3.6.9 Calibration
resulting solution
according to the p
3.6.10 Initial calibration vi
verification solution
the calibration standards
respective calibration
same acid matrix-as the ca
one. HC1
cone. HN03
ater
nc. HN03
3.6.6 No more than five multi-metal stock standards
containing metals in the following concentrations:
Metal
Na, Al, Ca, As, Se
Ba, Co, Mn, Ni, Pb, Ag, Tl, V, K
Be, Cd, Cu, Cr, Zn, Sb, Sn, Mo, Fe, Mj
3.6.6.1 Using the appropriate metal sal
following standards have been found to b
Metals Mixes
Al, Ba, Be, Fe, Ni, Ag, Na, Tl
Ca, Cd, Co, Cu, Pb, Mg, Mn, Zn
Cr
V
3.6.7 A single metal stock st,
metal.
3.6.8 Calibration standards: Prepare caTrbfation standards by dilution
of stock or spiking standard solutions^ All/caiibfatritm standards must be
matrix matched with the extracting acidNsolution according to the
preparation procedure used in the analysiV. /Concentrated hydrochloric
acid can be used instead of HN03 if required/for stabilization of a
metal(s).
eded for each
lanks such that the
tracting acid solution
the analysis.
iffeation: "The initial calibration
e yfrom a different source than that used for
be approximately in the middle of the
•e. "SChis verification standard must be in the
standards.
:k sampi^y Prepare by dilution of the stock
ible from the EPA. If the solution is
be made using the concentrations in
e run at least five times and the mean
orted in the raw data.
NOTE:
known concent
magnitude of int
corrections.
corrected by the data
The
/solution(s) (ICS) is prepared to contain
Bering elements that will demonstrate the
id provide an adequate test of any
£ed to verify that the interference levels are
tern within quality control limits.
December, 1991
Page D-16
-------
Exhibit D
Metal Analysis of Ambient Air
3.7 QUALITY CONTROL
3.7.1 Instrument Calibration
3.7.1.1 Summary
Prior to the analysis of samples and re
shall be initially calibrated to determine
3.7.1.2 Frequency
Instruments shall be calibrated
each time the instrument is set up.
3.7.1.3 Procedure
pre
Calibration standards shall be
matrix and at the same concentration as
following sample preparation.
Calibrate according to
procedures using at least
Before beginning the sampI
calibration standard as if it
3.7.1.4 Calculations
% Rec,
3.7.1.5 Technica
Recovery
within ± fi
3.7 .1'. 6 Corrective
ry 24 hours and
the same type of
tion blank
mfacturer's recommended
blank.
'ighest mixed
on
probl
x 100
Eq. D-4
ation standard shall be
value (i.e., 95-105 percent).
's recommendations to correct the
'on is acceptable as long as it is
le or after the continuing calibration
; resloping is acceptable as long as it is
idiately followed by a CCV and a CCB.
The
raw data.
dized data and time shall be included in the
'centration should be in pg/L.
December, 1991
Page D-17
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.2 Initial Calibration Verification
3.7.2.1 Summary
Immediately after the ICP system has been/calfb£ated>^he accuracy
of the initial calibration shall be verified^ana docuJhentea^for every
analyte by the analysis of EPA Initial Calibration Verifrea^tion^
Solution(s) (ICV) at each wavelength used/Ba^analysis.
3.7.2.2 Frequency
Each time the instrument is calib/atea, the iCV^hall be run
immediately following the calibration,Before any ^samples are
analyzed.
3.7.2.3 Procedure
If the ICV solution(s) are not available ^ispm EP^tyor where a
certified solution of an analyte is not availabl&xfroni^ny source,
analyses shall be conducted/onatr-i»deEendent standarration> but
within the linear range. An\ iTwepenaent^standardia? defined as a
standard composed of the analy±es\from a difFetenfc-source than those
used in the standards for the ihastrumertt c
3.7.2.4 Calculations
100
3.7.2.5 Technica
Recovery
value (i.e.'
3.7.2.6 Corrective A
Eq. D-5
± 10 percent of the true
the^ICV ex&eed the technical acceptance
shallT>evjCerminated, the problem corrected, the
and the calibration reverified.
incentration (ftg/L), true concentration
ry on FORM II-AAIN.
December, 1991
Page D-18
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.3 Continuing Calibration Verification
3.7.3.1 Summary
To ensure calibration accuracy during an
continuing calibration verification solution/CC
reported for every wavelength used for the
and
e.
iroent or every two hours
>
sample in the
3.7.3.2 Frequency
The CCV is run at a frequency of
during an analysis run, whichever is
The CCV is also run after the 1
analysis run.
3.7.3.3 Procedure
The same CCV shall be used throughout theN^nalysis runs for a Case
of samples received. The analyte concentrations^!! thfe> continuing
calibration standard shall /6e"~an—EBA^_solution or a contractor prepared
standard solution and should he_ at ornea?~±-l£Lpercent of the mid-
range levels of the calibrat
ott
Each CCV analyzed shall refiec
of the associated analytical sample
samples or the preceding analyt
The duration of analysis^, rinses a:
affect the CCV measured result
greater extent tjwm jfche^xteNjit appliedN^o
samples. For instance, t,
and the blank >unmaiately /following
tions of analysis for all
preceding 10 analytical
les up to the previous CCV).
r related operations that may
shall \ot e applied to the CCV to a
e associated analytical
ime between a CCV analysis
as Veil as the difference in
time between/the/CCV and,
it shall not/exceed the
consecutivesanalyfcical /si
3.7.3.4 Calculatior
ne/anar)Mn.cal -sample immediately preceding
[lest difference in time between any two
Jles associated with the CCV.
Concentration
Ktue Concentration
x 100
Eq. D-6
3.7.3/.5 .Technical AcceotanVe Criteria
(Recovery for the CCW snail be within ± 10 percent of the true
90-110 peiceit).
December, 1991
Page D-19
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.3.6 Corrective Action
When recoveries of the CCV exceed the technical<(acceptance
criteria, the analysis shall be stopped, the p/roblemXprrected, the
instrument recalibrated, the calibration reverif£fe«L andx^he preceding
10 analytical samples reanalyzed (or all analytical samples^sjLnce the
last compliant CCV).
3.7.3.7 Documentation
Report the CCV found concentratior
(/ig/L), and percent recovery on FORM/
3.7.4 CRQL Standard
3.7.4.1 Summary
To verify linearity near the CRQL, the
ICP standard at two times the MQL or two times
greater. This standard
analysis.
3.7.4.2 Frequency
shall analyze an
chever is
'th used for
concentration
The CRQL standard shall be
sample analysis run, or a minimum
is more frequent.
3.7.4.3 Procedure
3.7.4.4 Calcul
Concen tra ti on
True Concentration
Corrective
beginning and end of each
'ce per eight hours, whichever
before the ICV solution.
x 100
Eq. D-7
analys
samples
^standard shall be within ± 15 percent of the
sngth used for analysis.
aes not fall within the control limit, the
ited, the problem corrected and the analytical
Compliant CRQL standard reanalyzed.
December, 1991
Page D-20
-------
Exhibit D
Metal Analysis of Ambient Air
L), true
-AAIN.
3.7.5.4 Calculatio
3.7.5.6 /Cor
alues above this linear
3.7.4.7 Documentation
Report the CRQL standard found concentration,
concentration (^g/L), and percent recovery on
3.7.5 Linear Range Analysis (Quarterly)
3.7.5.1 Summary
The concentration range over which
remains linear must be determined and
range shall be diluted and reanalyzed
3.7.5.2 Frequency
For all ICP analyses, a linear*1
shall be analyzed and reported quartei
each element on the target analyte list
standard shall be analyzed during a routine
under this contract. This, standard shall be
used for each analyte repor^ec
3.7.5.3 Procedure
The standard shall be analysed "as thoug"h it were a separate
analytical sample (i.e., each mea|u«*fei«fshall be followed by a rinse
and/or any other procedure normally performed between the analysis of
separate samples).
ion check standard
calendar months) for
nhibit C). The
run performed
wavelengths
x 100
Eq. D-8
3.7.5.5 Te
Recovery for ti
of the true value (i.
range standard shall be within ± 5 percent
percent).
thiei linear range standard does not meet the
iteVia, then the analysis shall be terminated
dilutions of the standard shall be reanalyzed until the
e concentration of this standard that meets
e/upper limit of the instrument linear range
t be reported under this contract without
ti«£al sample.
December, 1991
Page D-21
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.5.7 Documentation
Report the linear range standard found conce
true concentration (in /Jg/L) and percent reco\
FORM III-AAIN.
3.7.6 Initial Calibration Blank
3.7.6.1 Summary
To verify that the ICP system is
calibration blank (ICB) shall be ana
3.7.6.2 Frequency
The ICB shall be analyzed each tim*
immediately after the ICV.
3.7.6.3 Procedure
t:ion ( in
ach analyte on
is calibrated and
If the absolute value
result shall be reported.
3.7.6.4 Calculations
Not applicable.
3.7.6.5 Technical Acceptance
The absolute/va
3.7.6.6 Correctj
When the
criteria, term£
the calibration,
:han the MQL, the
1/ss than the CRQL.
ton does not meet the technical acceptance
Is, correct the problem, recalibrate, verify
the ICB.
To
run, conti
jig/L on FORM IV-AAIN.
Blanks
tern is not contaminated during the analysis
ion blanks (CCB) are analyzed.
December, 1991
Page D-22
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.7.2 Frequency
Analyze the CCB at a frequency of 10 percent
whichever is more frequent.
Analyze the CCB after every CCV.
3.7.7.3 Procedure
ivery two hours,
A CCB shall be run after the last G
absolute value of the CCB is greater ti
reported.
'the analysis run.
:xe MQL, the result shal be
3.7.7.4 Calculations
Not applicable.
3.7.7.5 Technical Acceptance Criteria
The absolute value of the CCB must be less t
3.7.7.6 Corrective Action
When the CCB concentratio
criteria, terminate analysis,
the calibration, and reanalyze
all analytical samples since the
3.7.7.7 Documentatio;
Report the O
3.7.8 Preparatii
3.7.8.1 Summa
To ensure agai
preparationblank (PB
3.7.8.2
leal acceptance
roblem, recalibrate, verify
10 analytical samples (or
'mpliant CCB).
-AAIN.
The
sample pre
nation during sample preparation, a
prepared and analyzed with every SDG or
digested, whichever is more frequent.
cons/st^f ASTM Type II water processed through each
lysis procedure step.
December, 1991
Page D-23
-------
Exhibit D
Metal Analysis of Ambient Air
The first batch of samples in a SDG shall be assigned to PB one,
the second batch of samples to PB two, etc.
3.7.8.4 Calculations
Not applicable.
3.7.8.5 Technical Acceptance Criteria
The absolute value of the PB must b;
3.7.8.6 Corrective Action
If the absolute value of the c
or equal to the CRQL, no correctiv
If any analyte concentration in the F
lowest concentration of the analyte in the
10 times the PB concentration. Otherwise, all s
the PB and with the analyt
concentration and above th^ CRQL_ shall
for that analyte. The samp
the PB value.
ss than the CRQL.
ted
/the PB is less than
auired.
the CRQL, the
samples must be
associated with
0 times the PB
and reanalyzed
be corrected for
If an analyte concentration
then all samples reported below 1C
shall be redigested a»d-E^analyzed.
3.7.8.7 Documentation
The values
3.7.9 ICP Inte
3.7.9.1 Summary
is below the negative CRQL,
CRQL associated with the PB
ded in /ig/L on FORM IV-AAIN.
To
Interf
3.7.9.
3.7.9.3
The ICS
Solution A consis
background correction factors, an ICP
analyzed.
beginning and end of each analysis run or a
hour working shift, whichever is more
ICV.
two solutions: Solution A and Solution AB.
the interferents, and Solution AB consists of
December, 1991
Page D-24
-------
Exhibit D
Metal Analysis of Ambient Air
the analytes mixed with the interferents. An ICS
analyzing both solutions consecutively (starting
all wavelengths used for each analyte reported
The ICP ICS shall be obtained from EPA (
analyzed according to the instructions supplied
If the ICP ICS is not available from E
shall be prepared with interferent and
levels specified in Table 3, Exhibit C
deviation shall be established by init
five times repetitively for each anal;
If true values for analytes con
ICP are not supplied with the ICS
initially analyzing the ICS at lea:
particular analytes. This mean dete
analytical run where the results for the
met all contract specifications.
initial mean determination is to be used as
lifetime of that solution (/7eTr-t»til the
3.7.9.4 Calculations
sis consists of
Solution A) for
available and
CS.
Additional
analyzing the ICS at least
and analyzed by
be determined by
epetitively for the
11 be made during an
supplied EPA ICS
suit of this
.ue for the
exhausted).
the
% Recovery
3.7.9.5 Technical Acce
Recovery for
value (i.e., 80
3.7.9.6 Correc
If the
criteria, term
instrument,
analytical^ ampj.es
3.7.9.7
Eq. D-9
\ncracion
CriteriaN
be within. ± iO percent of the true
verify
not meet the technical acceptance
lysis, correct the problem, recalibrate the
^ration, and reanalyze all of the
st compliant ICS was analyzed.
Concentration (pg/L), true concentration
lean and standard deviation on FORM V-AAIN.
iviation shall be reported in the raw data.
December, 1991
Page D-25
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.10 Spike Sample Analysis
3.7.10.1 Summary
To provide information about the effect o
the digestion, a known amount of analyte is
sample.
3.7.10.2 Frequency
At least one spike sample analysis
group of samples for each SDG. EPA
sample analysis upon special reques
the Contractor will be paid.
If two analytical methods are use
for the same analyte within a SDG (e.g.,
samples shall be run by each method used
3.7.10.3 Procedure
The spike is added befor
digestion) at concentration
indicated in Table D-3.
Samples identified as field
sample analysis. EPAjnay require tt
the spike sample
one spike sampleper/-SBG^and
contract criteri
method in the
3.7.10.4 Cal
prmed on each
lonal spike
Officer, for which
the reported values
then spike
'(i.e. , prior to
le solution as
lot be used for spiked
specific sample be used for
where there is more than
e recovery is not within
:he same matrix, level, and
Eq. D-10
x 100
per:
sampl
the dupl
percent recov
performed on the same sample that is
le analysis, spike calculations shall be
s of the sample designated as the "original
Duplicate Sample Analysis). The average of
be used for the purpose of determining
December, 1991
Page D-26
-------
•Exhibit D
Metal Analysis of Ambient Air
When the sample concentration is less than the
detection limit, use SR = 0 only for purposes of
recovery.
3.7.10.5 Technical Acceptance Criteria
Recovery for the spike should be within
amount (i.e., 75-125 percent).
3.7.10.6 Corrective Action
rument
.ulating percent
spiked
If the spike recovery is not withi/n the limit^of 75-125 percent,
the data of all samples received associated witbi that spike sample and
determined by the same analytical method shall/be/1'lagged with the
letter "N" on FORMs I-AAIN and VI^AAD
An exception to this rule is grantfedvin situations where the
sample concentration exceeds the spike cohcentra>64°n by a factor of
four or more. In such an event, the data sha"il be reported unflagged
even if the percent recovery_jdoes not meet the 75^.25 percent recovery
criteria.
Duplicatj
and analysi
analytical
3.7.11.2 Fre
3.7.10.7 Documentation
Report the spiked sample re
percent recovery for the spike
The units for
3.7.11 Duplicate Sample
3.7.11.1 Summa:
e results, spike added and
on FORM VI-AAIN.
results will be in
met"
carried through the preparation
rov/de information about the precision of the
as matrix effects.
ate
sample
analysis shall be performed on each
SDG. EPA may require additional duplicate
request by the Project Officer, for which
d.
ds are used to obtain the reported values
.n a SDG (e.g., ICP and GFAA), then duplicate
ach method used.
December, 1991
Page D-27
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.11.3 Procedure
Samples identified as field blanks cannot be/usfsd for duplicate
sample analysis.
EPA may require that a specific sample
sample analysis.
wit
In the instance where there is more
SDG and one duplicate result is not
the samples of the SDG.
Duplicate sample analyses are
relative percent difference.
3.7.11.4 Calculations
RPD
where:
RPD = Relative Perc
S = First Sample
D = Second Sample
on FORM 1-AAIN.
/contract criteria, flag all
ilations of
Eq. D-ll
Duplicates
3.7.11.5 Technical/ Ac
A control
and duplicat
(Exhibit C)
values less
If one result
below, use
cal
3.7.1
If the
flag' with an
with that duplic
shall be used for original
or equal to five times CRQL
shall be used for sample
five times CRQL level and the other is
than the MQL, the RPD is not
for each analyte will be added to FORM IX-
d on precision results.
sample results are outside the control limits,
'all the data for samples received associated
Sample.
December, 1991
Page D-28
-------
Exhibit D
Metal Analysis of Ambient Air
ses shall be
e entered in
group of samples
re frequent.
e same sample
s employed for the
e Concentration
e Criteria
3.7.11.7 Documentation
The results in pg/L of the duplicate sample
reported on FORM VIII-AAIN.
The absolute value of the control limit
the "CONTROL LIMIT" column on FORM VIII-AAI)
3.7.12 Laboratory Control Samples
3.7.12.1 Summary
A laboratory control sample (LCS)
ensure against analyte loss in the
3.7.12.2 Frequency
One LCS shall be prepared and analyzec
in a SDG, or for each batch of samples, whic
3.7.12.3 Procedure
A LCS shall be analyzed
preparations, analytical me
EPA samples received.
The LCS solution shall be obta
other EPA Quality Assurance Check
may be used.)
3.7.12.4 Calcula
om EPA. (If unavailable,
or other certified materials
x 100
Eq. D-12
3.7.12.5 Techni
Recove
value
3.7.12
within ± 20 percent of the true
the exception of Ag and Sb.
for the LCS falls outside the technical
analyses shall be terminated, the
samples associated with that LCS reprepared
am
December, 1991
Page D-29
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.12.7 Documentation
Report the LCS found concentration (jig/L) ,
, and percent recovery on FORM IX- AAIN .
concentration (in
3.7.13 Performance Evaluation Sample (PES)
3 . 7 . 13 . 1 Summary
The performance evaluation sample Q^ES)/ assists the Agency in
monitoring the laboratory performance
quantification .
3.7.13.2 Frequency
One PES shall be delivered, prepar
of samples in a SDG, or for each batch
frequent.
lyzed for every group
whichever is more
Recovery fa
of analyte.
3.7.13.6
identification and
3.7.13.3 Procedure
A PES shall be analyzed
preparations, analytical metft
EPA samples received.
The PES solution shall be obta
contractor must contact.^he Agency
3.7.13.4 Calculations
Not appli
3.7 .13.5 Tech:
;e same sample
employed for the
om EPA. (If unavailable, the
[0 for instructions.)
be within 75 percent of the true value
.ction
icy/may take, but\is i
Show Cause and/or Cur
Reduceion of the nnmb
for the PES falls below 75 percent, the
i.s \ot limited to the following actions:
Notice for unacceptable performance;
of samples shipped to the laboratory;
shipment;
December, 1991
Page D-30
-------
Exhibit D
Metal Analysis of Ambient Air
• A site visit;
A full data audit; or
Require the laboratory to analyze remedial
In addition to the above cited actions, ydheAabora^pry
provide the Technical and Administrative Project Officers^a
correction action report on every unacceptable (less than
PES score within seven days of written cyz verbal request by
personnel.
3.7.13.7 Documentation
Report the PES on Form I-AAIN 0.n
3.7.14 Method Quantitation Limits
3.7.14.1 Summary
also
3.7.14.3 Procedure,
MQLs (in
average of t.
nonconsecut
PB extracts
separate anal
a rinse and/or arr
analysis of separate
for eac
Prior to sample analysisTThe-msthpd quantitatibs^J/imit (MQL)
shall be determined for eaph instnoment^citat-Jtill be used.
3 . 7 . 14 . 2 Frequency
MQLs shall be determined within
contract and at least quarterly (every
the end of the contr
of the start of the
.ree calendar months) until
by Multiplying by three, the
obtained on three
analysis of seven different
must be performed as though it were a
(i.e., each measurement must be followed by
rocedure normally performed between the
MQLs shall be determined and reported
nalysis of the samples.
ned MQU for an instrument shall always be
instrument during that quarter. If the
iri\anyway that may affect the MQL, the MQL for
:edetermined and the results submitted for
for that instrument for the remainder of
tK
December, 1991
Page D-31
-------
Exhibit D
Metal Analysis of Ambient Air
3.7.14.4 Calculations
MQL = 3 x (oa_
3.7.14.5 Technical Acceptance Criteria
The MQLs shall be < the CRQLs in Exhib,
3.7.14.6 Corrective Action
If an instrument's MQL exceeds th
instrument cannot be used in this
concentration is greater than or e
3.7.14.7 Documentation
MQLs shall be submitted with each data pafc
FORM XI-AAIN for each instrument used. If multit
Eq. D-13
used for the analysis of an
the analyte shall be used
SDG.
3.7.15 ICP Serial Dilution
3 . 7 . 15 . 1 Summary
The serial dilu
of matrix inter fe
lyte, that
analyte
the reported MQL.
within an SDG,
ration
3.7.15.2 Frequen
One serial: dilution
3.7.15.3 Procedu1
reported on
tents are
ighest MQL for
values for that
to check for the presence
d for each SDG.
The serialdiluti^KshallNbe performed by diluting a prepared
sample aliquot~flvefolo>3s:4)?>XThe dilution must be performed on an
analyte bvanalyte ba^es. The^serial dilution is the dilution of the
sample, sir an aliquot of the sample, that contains a concentration
level.
-------
Exhibit D
Metal Analysis of Ambient Air
where:
I
S
Initial Sample Result; and
Serial Dilution Result.
3.7.15.5 Technical Acceptance Criteria
If the original sample concentration is/gre,
MQL, the %D should be within ± 10 percent
result.
3.7.15.6 Corrective Action
If the serial dilution results aye
flag all the data for the affected
associated with that serial dilutyi
FORM I-AA1N.
3.7.15.7 Documentation
The values for the serial dilution shall be
FORM XI-AAIN.
3.7.16 Interelement Correction
3.7.16.1 Summary
the
3.7.16.2 Freq-
Before an-/ f
interelemen
months prio
thereafter.
3.7.16.3 Procedure
Cptrec
Control limits,
samples received
on FORM XI-AAIN and
in jig/L on
To ensure against spectral int
factors are determim
reported by ICP.
.ces, interelement correction
.s used for each analyte
intere
the resul
under this contract, the ICP
determined within three
contract analyses and at least annually
for sjStec^ral interference due to Al, Ca, Fe, K,
rmined for all ICP instruments at all
analyte reported by ICP. Correction factors
due to analytes other than Al, Ca, Fe, K,
d if they were applied.
.djusted in any way that may affect the ICP
actors, the factors shall be redetermined and
use.
December, 1991
Page D-33
-------
•Exhibit D
Metal Analysis of Ambient Air
Follow the instrument manufacturer's recommem
interelement correction factors.
3.7.16.4 Calculations
Not applicable
3.7.16.5 Technical Acceptance Criteria
Not applicable
3.7.16.6 Corrective Action
Not applicable
3.7.16.7 Documentation
Results from interelement correction fact
be reported on FORM XI-AAIN for all ICP paramete
s for applying
ination shall
3.8 INSTRUMENT OPERATION
3.8.1 No detailed operating ins
plasma power, argon flows, torch
given. The analyst should follow thi
manufacturer of the particular instrum'
3.8.2 The sample int
use of a peristaltic
washer is a very us
flow system by pla
just before enter
to the nebulizer
connected to a tine
flow is observed,
flow and blown through^
and restarting the ori
3.8.3 C
characte,
is reco;
eduction
imization of the
guration, etc. will be
ions provided by the
3.8.
call
and s
of which i
All exposure t"
analyses (i.e.,
of a pneumatic type. The
tion is required. A tip
rted into the sample
'tee donnector"^x»Qrtie carrier argon flow line
:he nebula.zer^ "brae arm/of the "tee connector" runs
ther to/the/carriera*gon flow line and the third is
peristaltic pump. When a drop in the carrier
of water is pumped into the carrier argon
nebulizer orifice, dissolving the salt buildup
argon flow.
ier afg«n/flow may change the emission
£e. The use of a digital mass flow controller
carrier argon flow.
ruments, every solution, including
ration and method blanks, reference samples,
;ed/using two full exposures (peak scan), each
rne^t the MQL (at each analyte emission line).
the same for all analyses and all quarterly
md interelement correction factor). Each
December, 1991
Page D-34
-------
Exhibit D
Metal Analysis of Ambient Air
background spectral region shall have an exposure time
full exposure time for direct reading instruments.
equivalent to a
3.8.5 Selection of the appropriate background spectral region for each
analyte shall account for the major interferents wjtthin that region and
for the possibility of analyte line broadening at/higfiNconcehtrations.
One of the best ways to select the appropriate bAckgrounaNtpectral region
is to perform a wavelength scan around the anal^te/wavelengthsvin tl
presence of metals frequently encountered at M^m^levels in the samples
Alternately, if the instrument does not have/automatic scanning
capability, selection of the background spectral region will have to be
determined on the basis of manual scans an/a experience
3.8.6 A calibration blank rinse betweei( each sampj
sufficient to prevent carry-over between samples.
spiration should be
3.8.7 The determination of the linear range of"eacii analyte line,
interference effects, and any type of detectionsj-imrbvpr precision
measurement shall be established under the same cbraditiohs used for the
analysis of the samples, including the background cori?e.ctioi> scheme.
3.9 PROCEDURE
3.9.1 Calibration
3.9.1.1 Set up the instrument withVpri
instrument shall be allowed to become
analysis. This require$—»t^least 30 ml
plasma lit prior to
3.9.1.2 Initiate
computer.
Analysis Se
tionrblank (IGB), i
rerice check samcle.
ration values shalM
(.percent, while the
than 15 percent. /
L. Tfta, interference
iperating parameters. The
lly stable before beginning
of operation with the
ration of the instrument
3.9.1.3 Perfo
to align the e:
commonly called
3.9.2
ommended by the manufacturer
e entrance slit. These steps are
wavelength calibration procedure.
e analysis run, analyze the initial
itial calibration verifications (ICV),
i the CRQL standard (CRI). The ICV and LRS
: deviate from the actual values by more
shall not deviate from its actual values
calibration blank values shall not exceed
heck sample found values shall not deviate
true values. If these conditions are not
tinue the analysis and refer to Exhibits D
December, 1991
Page D-35
-------
Exhibit D
Metal Analysis of Ambient Air
(Quality Control - Initial and Continuing Calibratio,
additional information.
3.9.2.2 Upon successful analysis of the ICV, 1C,
all PB extract(s) prepared with the samples. I
values are not less than or equal to the CRQL,
the appropriate action.
3.9.2.3 If the PB and LCS values are wi
analyze the spike sample. If the recove
the acceptable ranges, see Exhibit E for/th<
Proceed to the analysis of samples if
after consulting Exhibits D and E.
anks) and E for
.nd ICS, analyze
lank(s)
E for
any analyte deviates from
appropriate action.
4coverie« a^e acceptable or
3.9.2.4 The continuing calibration verified
continuing calibration blank (CCB) shalT-fee ana
analytical sample analyses. The analyst shal
after the analysis of the previous sample, but
standard (ICV) and the
lyied after every 10
runv€£V and CCB samples
use of a tip
wash or other clean out device.
deviate from the actual value
the absolute values for the
conditions are not met at any
the analysis and see Exhibits D
CCV concentration
10 percent
3.9.2.5 At the end of the sample
and CCB. If the values for any of
required limits, see Exhibits D and E
3.9.3 Sample Analysed
hall not
n addition,
the CRQLs. If these
'sis, discontinue
ate action.
analyze the ICS, CRI,
les deviates from the
itional information;
3.9.3.1 All sample -Extracts/shall firsX^be analyzed without any
dilution. Dilutotng/sample extratets^is permissible if necessary,
provided that fine Dilution Aoep not proaaoe results below CRQL.
3.9.3.2 All concentrations/within the linear range of the analyte shall
be reported. All con&eritraCions reported shall be obtained within the
established linear rangeNEor that analysis run, and interference
based on^the actual concentration of the
interfer/ent a»d-*o_t theNapparentxcpTicentration obtained when the
interfereivt concentration^ above the linear range.
3.9.4
[eolations
3. fv4.1 ^^P obtain the arialyfce air concentration (in /*g/m3 ) , multiply
the itt&erf erfe«ce - corrected analyte values (in ^g/L) by nine times the
appropriate volulBe( in /iters) used in the extraction and divide by the
volume of airx(in s^anoar
-------
Exhibit D
Metal Analysis of Ambient Air
in2) of the Hi-Vol filter exposed to the air strea
exposed area (7 in2) in one l"x 8" strip.
Q Interference-Corrected
Analyte Cone. _ y x Analyte Value, \ig/L
air, pff/m3 ~ no. of
ided by the
£q. D-15
strips digested
3.9.5 Documentation
3.9.5.1 Report the air concentration valties,
interference-corrected analyte value in ^g/I/on FORM I-AAIN.
December, 1991
Page D-37
-------
Exhibit D
Metal Analysis of Ambient Air
SECTION 4
SAMPLE ANALYSIS
BY
INDUCTIVELY COUPLED PLASMA-MASS SPECTRO]
4.1 SCOPE AND APPLICATION
4.1.1 Metals for which this method is applLcabl
Exhibit C in are determined by 1CP-MS after/sample preparation by
microwave digestion (Section 2 of this
limits, sensitivities, and linear ranges
the matrices, instrumentation, and oper
method is restricted to spectroscopist
recognition and the correction of spect?
interferences in ICP-MS. The experience
commercially available ICP-MS.
4.2 SUMMARY OF METHOD
tent quantisation
.ts will vary with
Use of this
.geable in the
and physical
is one year on a
mi.
4.2.1 The method describes th
by ICP-MS. The method measures
inductively coupled plasma. Anal
nebulized and the resulting aerosol
plasma torch. The ions produced are
means of a water cooled interface, int
spectrometer, capable of^p*e«iding a
amu peak width at 10
interface consisting
leads into the high /racVum c
ion clusters produi
introduction of th& i^n beam
according to the
electron multipl^r. Inter:
applied or the d
standard technique is
enhancements caused by s<
-elemental
,by a radio;
>ecies/
lutJ
Ination of analytes
requency
in a liquid are
by argon gas into the
in the plasma gas and by
into a quadrupole mass
n better than or equal to 1
The water-cooled
rentially pumped and
pectrometer. The ions and
ormed during the
ctrometer, are sorted
quantified with a channel
rejices must be assessed and valid corrections
indicate problems. Use of the internal
:he peak height
rs, is
je mas!
[uire
-------
Exhibit D
Metal Analysis of Ambient Air
resolution at 10 percent of the peak height, and very
adjacent masses can contribute to ion signals at the
Table D-9 shows approximate concentrations at which
rise to a contribution of 10 pg/L to the analyte o
resolution of 1 amu at 10 percent peak height, if
quantitation. It should be noted that the info
D-9, was experimentally derived and the interfe
occur from several different sources. One interference is
resolution on adjacent peaks. This has a largfe^effect at 1
the interferant than at one amu greater than/th<
the trapezoidal peak shape associated with
Another interference which would be observed is
ion currents at
of interest.
ent masses give
interest at a
were chosen for
^described in Table
scribed
of
ion. These interferences only cause an
the interferant's mass. It should also,
interferences are not necessarily linei
to extrapolate the values to a particul
included for its informational content all
interferant's mass
drupole mass spectrometer.
the formation of a hydride
ference/at/i amu greater than
emembered tfhat these
attempts/should not be made
The table has been
4.3.2 Isobaric molecular and doubly charged iofi^-interJerences in ICP-MS
are caused by ions consisting of more than one atom or charge. Table D-
10, lists isobaric molecular - ioEf~late*fe£ences which coui4/affect the
analyte s. It should be noted tjnatjoaany oftKSse—interferences are
extremely rare, but adverse effe
individual constituents occurred
concentrations. When the interfere
another isotope with sufficient nat
must be applied. Corrections for mole*
be based upon the natural^.Lap^tope ratios
determination of the
interferant is preset
If a correction
to the extent of
previously dei
interferant.
ion corrections
isobaric interferences
identified in the literati
4.3.3 Ph;
nebuliza
efficienci
matrix'"'
marine
Inte
interfe
elements
matrix compone:
lighter atomic
occur if the
iently high
be avoided by the use of
e, corrections to the data
interferences may either
ie molecular ion or a
which occurs when the
correction may be normalized
late internal standard
1 of oxide as the
f correction has been reported for oxide
use on rare earth elements. Host
affect ICP-MS determinations have been
es afexe££ects associated with the sample
ocesses as well as ion-transmission
transport processes are those in which the
e in surface tension or viscosity in a
rds used in performing calibration.
ed to correct for these interferences. The
pressions and are seen by the lighter
elements. The effects are greater for
atomic mass than for matrix components with
es in matrix composition therefore can cause
December, 1991
Page D-39
-------
Exhibit D
Metal Analysis of Ambient Air
significant suppressions and enhancements. Dissolved*soL£d levels can
contribute deposits on the nebulizer tip of a pneumatic ;nebulizer and on
the interface skimmers (reducing the orifice size aiui tj^ie instrument
performance). Total solid levels below 0.2 percent (2,Ot)Qsopm) have been
recommended to minimize solid deposition. Internal s'feandardsxjnust be
affected to the same degree as the analyte to de
compensate for these interferences. A minimum
standards, listed in Table D-7, bracketing
When the intensity level of an internal sta
or greater than 125 pecent of the intensity/of/
during calibration, the sample must be reanalyzed aftes^performing a five
fold (1:4) dilution. The intensity levelfe at the internal standards for
the CCB and CCV solutions must agree within/± 20 pe/cerit of the intensity
level of the internal standard of the IcB solution/ If they do not agree,
terminate the analysis, correct the prok^em, re^adib/ate, and reanalyze
the previous 10 samples at no additional ct
4.3.4 Memory interferences are effects which are^dependant upon the
relative concentration differences between samples orxstano^rds which are
analyzed sequentially. Sample
-------
Exhibit D
Metal Analysis of Ambient Air
4.5 OPERATIONAL REQUIREMENTS
4.5.1 System configuration: Because of the differ
makes and models of satisfactory instruments, no detai
instruction can be provided. Instead, the analyst/shou
instructions provided by the manufacturer of the
Sensitivity, method quantitation limits (MQL's)
range and interference effects must be establi
particular instrument. All reported measure
instrumental linear ranges. The analyst mus
data confirming instrument performance and /analytical results.
between various
operating
follow the
strument.
dynamic
withfi'
lity contrail
IT IS THE RESPONSIBILITY OF THE ANALYST 70 VERIFY
CONFIGURATION AND OPERATING CONDITIONS USED/SATISFY/
REQUIREMENTS SET FORTH IN THIS DOCUMENT ANC. TO
DATA CONFIRMING INSTRUMENT PERFORMANC
INSTRUMENT
ANALYTICAL
QUALITY CONTROL
RESULTS.
The data must include hardcopies and computer^eadaoie storage media which
can be readily examined by an EPA audit team. The^data^aust demonstrate
defendable choices of instrument operating conditions-xwhicfe^mimimize
interferences such as oxides.
4.5.2 Precautions must be
multiplier from high ion currents^ Tiie chs
suffers from fatigue after being exposed t
-------
Exhibit D
Metal Analysis of Ambient Air
Many more molecular-ion interferences are observed on
hydrochloric and sulfuric acids are used, as demonst
Concentrations of antimony and silver above 300
(v/v) HC1 for stability.
4.6.2 Internal standards must be used to moni
that occur from differences between standards
information must be clearly reported in the
which internal standards correct, are primarily
Internal standards must be present in all
identical levels by mixing the internal
nebulized prior to the nebulizer. This
second channel of the peristaltic pump
uptake tube. If adding the solution t<
the internal standard must be added in
samples and standards to prevent the poss
internal standard levels. The double
analytes when
in Table D-10.
one percent
lity
spiking"
changes
rds and samples at
solution being
.ed by using a
1 standard to the
is not used then
uots to the
improperly spiking the
that misquantitation
accon
the
iptaki
tandards
jche appr
contaj
will not occur based upon a single internal sta;
spiking may occur either by adding a constant volume
concentrate to identical volume
by diluting the internal stan
the analyses . One typical ex
standards and samples into indivl
mg/L solution of the internal s
This adds identical amounts of the 1
analysis. The concentrations of the
not have to be corrected^fox^the diluti
dilution is canceled o>rt when oarrections
their dilution.
rd
to
Double
rnal standard
red samples, or
level for its use in
mL of all
.100 mL of a 10
to each of the containers.
to each solution for
levels in the standards do
ch occurs because the
samples are made for
sure out 1C
Standard
4.6.2.1 Bismuth
Dissolve 0.1115/g Bi2O3 in a,
cone. HN03 and/ailjjte to l.jOOO
4.6.2.2 Holmium Tsi^ernal/ st$
Dissolve 0..1757 g Hoz>fQp3)3«
HN03. After aissolutioriMs con
mL cone. BNOTandTlriute to
1 standard solut
with
"stock, 1 mL = 100 jig Bi:
>f dilute HN03. Add 10 mL
Type I water.
.000
xd solution, stock, 1 mL - 100 /zg Ho:
in 10 mL ASTM Type I water and 10 mL
warm the solution to degas. Add 10
with ASTM Type I water.
4.6.2.3/ Indium internal standard solution, stock, 1 mL - 100 /tg In:
DissoJ^ve /0.1000 g indiu^ me\al in 10 mL cone. HN03. Dilute to 1,000 mL
Type I water.
4.6^2.4 lithium internal/standard solution, stock, 1 mL •= 100 ng 6Li:
Dissolve o7feS12 g 95 atoift percent enriched 6Li, Li2C03 in 10 mL of ASTM
Type I wa"6er anSKLO mL Jfi&QV. After dissolution is complete, warm the
solution to^aft^asT^^Add l^mL cone. HN03 and dilute to 1,000 mL with ASTM
Type I water.
December, 1991
Page D-42
-------
Exhibit D
Metal Analysis of Ambient Air
4.6.2.5 Rhodium internal standard solution, stock,
Dissolve 0.3593 g (NH<,)3RhCl6 in 10 mL ASTM Type I
cone. HC1 and dilute to 1,000 mL with ASTM Type I
4.6.2.6 Scandium internal standard solution, stO;
Dissolve 0.15343 g Sc203 in 10 mL (1:1) hot HN03;
dilute to 1,000 mL with ASTM Type I water.
4.6.2.7 Terbium internal standard solution,
Dissolve 0.1828 g Tb2(C03)3.5H20 in 10 mL (
is complete, warm the solution to degas.
to 1,000 mL with ASTM Type I water.
4.6.2.8 Yttrium internal standard sol;
Dissolve 0.2316 g Y2(C03)3«3H20 in 10
and dilute to 1,000 mL with ASTM Typ
4.6.3 Mixed calibration standard solutions
solutions to levels in the linear range for
consisting of one percent (v/v) HN03 in ASTM
selected concentration of inte
appropriate internal standard
D-7). Prior to preparing the
analyzed separately to determine
presence of impurities. Care must
standards that the elements are comp
standard solutions to freshly acid-cle"
fluorocarbon bottles for
as needed with the rea
Calibration standards
sample and monitored/we
required, some typ
100 jig Rh:
Add 100 mL
100 jtg Sc:
one. HN03 and
ml. •*
/HN03. After
'5 mL cone. HN03 and dilute
dissol
mL - 100 /ig Y:
Add 5 mL cone. HN03
Mixed standardNsol
,/and terbium. \
nixed standard sol
the stock-standard
the Instrument in a solvent
Type I wa^er along with the
such that ChejTe is an
.e^analytes (see Table
solution must.be
ferences or the
in preparing the mixed
stable. Transfer the mixed
t previously used FEP
standards must be prepared
ons can change on aging.
using a quality control
iough not specifically
inations follow.
4.6.3.1 Mixed
silver, bar!
se, beryllium, cadmium, lead,
, nickel and zinc.
4.6.3.2 Mixed
aluminum.
4.
II: Arsenic, chromium, thallium, and
x
iplutionxEH/: Antimony, vanadium, iron.
:ion IV: Bismuth, holmium, indium, scandium,
on V: Rhodium.
NOTE: If-vrte afcd^tion cff silver to the recommended acid combination
results, in ahxinitia^L precipitation, add 15 mL of ASTM Type I water and
December, 1991
Page D-43
-------
Exhibit D
Metal Analysis of Ambient Air
warm the flask until the solution clears. Cool and /dilute to 100 mL
with ASTM Type I water. For this acid combination/the/silver
concentration must be limited to 2 mg/L. Silver vendee these conditions
is stable in a tap water matrix for 30 days.
4.6.4 Three types of blanks are required for the dhalys
calibration blank is used in establishing and nipni/coring the^&alibra>SDlution(sK(l6fi) is prepared to contain
known concentrations/of inTesfering elements thkt will demonstrate the
magnitude of interferences ano\ pn0vT3exan adequate test of any
corrections. The IcS/solution/is detailfed^in Table 3, Exhibit C. The
chloride concentration provides a/meah&vto evaluate software corrections
for chloride-relAtecQ.nterfe/eno4s such £Sr-?*Cl160+ on 51V+ and *°Ar35Cl* on
75As+. Since thfevnatufcal abundance of 35C1 at 75.8 percent is 3.13 times
the 37C1 abundanceXb-£24/^percent, the ion corrections can be calculated
with adjustments for is^par.iexjontributions. " Iron is used to demonstrate
adequate resolution of thexsoecttxmeter on manganese. Molybdenum serves
to indicate/6xide efffects oneadmiunhsisotopes. The other'components are
present t0 evaittate^the aMlity fff^Jne measurement scheme to correct for
various^ol^ular-ionHsobaric interferences. The ICS is used to verify
that the interference lefcelsN^re corrected by the data system within
qualipy control limits.
4.8x5.1 »tpck solutions &>r/preparing ICS solutions A and AB may be
provided it^ailable from ^PA. Otherwise, refer to Table 3, Exhibit C.
They mus^^e diluted bet"or/e use according to the instruction provided.
The prepared^ICJj soiujaons A and AB must be prepared weekly.
December, 1991
Page D-44
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Exhibit D
Metal Analysis of Ambient Air
4.6.5.2 Mixed ICS solution I may be prepared by adding "1£.903 g
Al(N03)3«9H20, 2.498 g CaC03 dried at 180°C for 1 hovr/before weighing,
1.000 g Fe, 1.658 g MgO, 2.305 g Na2C03> and 1.767 /K^/Oj to 25 mL of
ASTM Type I water. Slowly add 40 mL of (1:1) HNOvT ^ffter dissolution is
complete, warm the solution to degas. Cool and dllute^t^ 1,000 mL with
ASTM Type I water.
4.6.5.3 Mixed ICS solution II may be prepared/by/slowly adding 7?A^4 g
85 percent H3POV, 6.373 g 96 percent H2SOA, 40vfr24 g 37 percental,
10.664 g C607H8 to 100 mL of ASTM Type I wajzer./ Dilute to 1,000
ASTM Type I water.
4.6.5.4 Mixed ICS solution III may be prep/red by ziddihg 5 mL each of
arsenic stock solution, chromium stock/solution, ropner stock solution,
and zinc stock solution, 10 mL each or cobalt stcfck /solution, nickel
stock solution, and vanadium stock soi\ition>vat«l 2/5 mL of cadmium stock
solution. Dilute to 100 mL with two percent HN03!
4.6.5.5 ICS A may be prepared by adding 10 mL df^mixetixICS solution I,
10 mL each of titanium stock solution, and molybdenum stotek solution,
and 5 mL of mixed ICS solution/TTr—Diiute to 100 mL with/ASTM Type I
water. ICS solution A must
prepared frel
4.6.5.6 ICS AB may be prepared lav adding
10 mL each of titanium stock solut
mL of mixed ICS solution II, and :
to 100 mL with ASTM Type I water. 1O§ soJ
fresh weekly.
ICS solution I,
fybdenum stock solution, 5
ICS solution III. Dilute
ition AB must be prepared
4.7 QUALITY CONTROL
To obtain analyte
more than the analyte
corrections. If the,
Zr, W) are below th
uncorrected equations
be noted that monitoring
monitoring the interference
monitored to
equations are
interference/co
include thi
sulfur molecular ions which
interfer
to indi
(b) an unctf
molecular-ion
tests will enable
that distort the ace
ita/of known quality,
concentrations /of interl
leveta that show
int
of
is necessary to measure for
iow the required interference
mce sources (such a C, Cl, Mo,
an effect on the analyte level,
ed/provided all QA criteria are met. It should
:erence sources does not necessarily require
it that a molecular spec'ies may be
interference. When corrected
Iso be met. Extensive QC for
uired at all times. The monitored masses must
n, hydroxyl, chloride, nitrogen, carbon and
impact the analytes of interest. When an
sample elements impacted must be flagged
rference correction applied to the data or
The isotope proportions for an element or
information useful for quality assurance. These
detect positive or negative interferences
reported values.
December, 1991
Page D-45
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.1 Instrument Calibration
4.7.1.1 Summary
Prior to the analysis of samples and required QC^^ach ICP-MS
system shall be initially calibrated to
sensitivity.
4.7.1.2 Frequency
Instruments shall be calibrated dai
each time the instrument is set up.
once every 24 hours and
4.7.1.3 Procedure
Calibration standards shall be
matrix and at the same concentration a
following sample preparation.
Calibrate according to instrument manufactured
procedures using at least
Before beginning the sample
calibration standard as if it
4.7.1.4 Calculations
4.7.1.5 Technical
Recovery f;
within ± f iv<
libration standard shall be
(i.e., 95-105 percent).
4.7
the same type of
blank
immended
lank.
est mixed
Eq. D-16
4.7.1.6 Correctivl
Follow
problem
perfo
raw dat
er's recommendations to correct the
rectlbon is acceptable as long as it is
rveryNsample mt^arter the continuing calibration
ion and blank check; resloping is acceptable as long as it is
diately followed by a CCV and a CCB.
lized data and time shall be included in the
The^-final onentration should be in
December, 1991
Page D-46
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.2 Initial Calibration Verification
4.7.2.1 Summary
Immediately after the 1CP-MS system has be
accuracy of the initial calibration shall be
for every analyte by the analysis of EPA In
Verification Solution(s) (ICV) at each mas
4.7.2.2 Frequency
Each time the instrument is calibrate
immediately following the calibratio
analyzed.
4.7.2.3 Procedure
If the ICV solution(s) are not available from\EPA, or where a
certified solution of an analyte is not avail^le frwrn any source,
analyses shall be conducted on an independent stanadard^t a
concentration other than tha£~u"5ed-J;Qj:instrument calibration, but
within the linear range, fm independent~sT^ndaxdis defined as a
standard composed of the analytfc^sr^om-^differentsj&urce than those
used in the standards for the\Li
;hall be run
les are
4.7.2.4 Calculations
% Recover^
4.7.2.5 Technical
Recovery tpt
value (i.e.,
4.7
Eq. D-17
10 percent of the true
4.7.2.6 Correcti
When recoveries
criteri
inst:
the technical acceptance
beeerminated, the problem corrected, the
e/calibration reverified.
icentration (pg/L), true concentration
on FORM II-AAIN.
December, 1991
Page D-47
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.3 Continuing Calibration Verification
4.7.3.1 Summary
To ensure calibration accuracy during an
continuing calibration verification solutio
reported for every mass used for the analy:
4.7.3.2 Frequency
The CCV is run at a frequency of lj
during an analysis run, whichever is
The CCV is also run after the
analysis run.
4.7.3.3 Procedure
The same CCV shall be used throughout all analysis r)ans for a Case
of samples received. The a/ualyt^Tjenx^gntrations in tkfi continuing
calibration standard shallsbe anEPA solutTStr-oiL^Cpntractor prepared
standard solution and should\be\ator~~near ±_10 percent of the mid-
range levels of the calibration c\rve.
very two hours
ample in the
prece
Each CCV analyzed shall reflect:
of the associated analytical sampl
samples or the
The duration of
affect the CCV mi
greater extent
samples. For
and the bla;
time betweei
it shall no^
consecutive anal
4.7.3.4 Calci
iditions of analysis for all
(ttfe preceding 10 analytical
lytical ^samp^s up to the previous CCV).
ysis, rinses and other\ related operations that may
suLt shall no\be\applied to the CCV to a
an/the exVente^appSL^ed to\jme" associated analytical
time between a CCV analysis
sdiately/foliowirtgsit aA well as the difference in
and/the/ analytical/sample immediately preceding
lest difference in time between any two
associated with the CCV.
)les
Fohnd Concentration
Ti uensoncen tra ti on
x 100
Eq. D-18
4 . 7 .Js . 5/Technical Acceptance, Criteria
Recbvery for the GCti sttall be within ± 10 percent of the true
( i . e>>, 90 - 1 10 perce/t ) .
December, 1991
Page D-48
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.3.6 Corrective Action
When recoveries of the CCV exceed the technic
criteria, the analysis shall be stopped, the pr
instrument recalibrated, the calibration reveri
10 analytical samples reanalyzed (or all analyti
last compliant CCV).
4.7.3.7 Documentation
Report the CCV found concentration
(/zg/L) , and percent recovery on FORM
iceptance
corrected, the
id the preceding
since the
), true concentration
4.7.4 CRQL Standard
4.7.4.1 Summary
To verify linearity near the CRQL, the
ICP-MS standard at two times the MQL or two
greater. This standard shall be run for every
4.7.4.2 Frequency
The CRQL standard shall
sample analysis run, or a mini
is more frequent.
4.7.4.3 Procedure
The CRQL stam
4.7.4.4 Calculat
x 100
or shall analyze an
, whichever is
used for analysis.
id end of each
ce/per eight hours, whichever
the ICV solution.
Eq. D-19
4.7.4.5 Technical Ao
Reco'
true
4.7.4
hall be within ± 15 percent of the
analysis.
s not fall within the control limit, the
id, the problem corrected and the analytical
liant CRQL standard reanalyzed.
December, 1991
Page D-49
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.4.7 Documentation
Report the CRQL standards found concentratio
concentration (/ig/L) , and percent recovery on
4.7.5 Linear Range Analysis (Quarterly)
4.7.5.1 Summary
The concentration range over which
remains linear must be determined and
range shall be diluted and reanalyze
4.7.5.2 Frequency
For all ICP-MS analyses, a linear
standard shall be analyzed and reported
months) for each element on the target anal
C). The standard shall be analyzed during a
performed under this contra<
masses used for each analy
MS calibration curve
ive this linear
4.7.5.3 Procedure
The standard shall be analyzed
analytical sample (i.e., each meas\
and/or any other proc^dur^ normally
. separate samples).
4.7.5.4 Calculatioi
'Re
x 100
Concenfratfi on
Criteria
ication check
3 calendar
able 2, Exhibit
ytical run
in for all
Igh it were a separate
shall be followed by a rinse
rmed between the analysis of
Eq. D-20
4.7.5.5 Technica
Recove
of the
4.7.5.6,
standard shall be within
rcent).
± 5 percent
the \linear range standard does not meet the
[.teria, then the analysis shall be terminated
of the standard shall be reanalyzed until the
concentration of this standard that meets
'the7 upper limit of the instrument linear range
caimot be reported under this contract without
^analytical sample.
December, 1991
Page D-50
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.5.7 Documentation
Report the linear range standards found concentration (in
true concentration (in Mg/L) and percent recovery for each analyte on
FORM III-AAIN. /
/ Xs-
4.7.6 Initial Calibration Blank
4.7.6.1 Summary
To verify that the ICP-MS system is/not/contaminated, an initial
calibration blank (ICB) shall be analy/edafter calibration.
is calibrated and
MQL, the
e Criteria
theXlCB must
4.7.6.7 Documentation
4.7.6.2 Frequency
The ICB shall be analyzed each*
immediately after the ICV.
4.7.6.3 Procedure
If the absolute value o
result shall be reported.
4.7.6.4 Calculations
Not applicable.
4.7.6.5 Technical Acce
The absolute
4.7.6.6 Correcti
le«s than the CRQL.
When the
criteria, t
the calibratio
set the technical acceptance
correct the problem, recalibrate, verify
Lyze the ICB.
on FORM IV-AAIN.
tern is not contaminated during the analysis
run, cbntinuihccalibration blanks (CCB) are analyzed.
December, 1991
Page D-51
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Exhibit D
Metal Analvsis of Ambient Air
4.7.7.2 Frequency
Analyze the CCB at a frequency of 10 percen
whichever is more frequent.
Analyze the CCB after every CCV.
4.7.7.3 Procedure
A CCB shall be run after the last
absolute value of the CCB is greater
reported.
4.7.7.4 Calculations
Not applicable.
4.7.7.5 Technical Acceptance Criteria
The absolute value of
4.7.7.6 Corrective Action
When the CCB concentration
criteria, terminate analysis, coi
the calibration, and reanalyze the\
all analytical sample*—&ince the
every two hours,
the analysis run. If the
:he result shall be
CRQL.
t the technical acceptance
problem, recalibrate, verify
10 analytical samples (or
liant CCB).
4.7.7.7 Documentation
Report the
4.7.8 Preparat
i
4.7.8.1 Summary
To ensu£g_^gainst
preparation blan
4.7.8.
;V-AAIN.
4.7.8
The PB
sample prepari
during sample preparation, a
prepared and analyzed with every SDG or
digested, whichever is more frequent.
of ASTM Type I water processed through each
analysis procedure step.
December, 1991
Page D-52
-------
Exhibit D
Metal Analysis of Ambient Air
The first batch of samples in a SDG shall be as/igJ^ed to PB one,
the second batch of samples to PB two, etc.
4.7.8.4 Calculations
Not applicable.
4.7.8.5 Technical Acceptance Criteria
The absolute value of the PB must be/les/ than the CRQL.
4.7.8.6 Corrective Action
If the absolute value of the co;
or equal to the CRQL, no correctiv'
:he PB is less than
If any analyte concentration in the PJfrNus aboVe the CRQL, the
lowest concentration of the analyte in the asaociat&d^samples must be
10 times the PB concentration. Otherwise, all samples^ssociated with
the PB and with the aiialyteVs"""c"oTneentratipn less thkhsj» times the PB
concentration and above theQ CRQLshallbe~~tBdige§ted and reanalyzed
for that analyte. The sample. copSSfitratipn is notto be corrected for
the PB value.
If an analyte concentration
then all samples reported below
shall be redigested
4.7.8.7 Documentation
The values
7.9 ICP Interfen
<
4.7.9.1 Summary
To verify_intereleiBBot anc
Interference ChecfcvSample
PB/is below the negative CRQL,
CRQL associated with the PB
in fig/L on FORM IV-AAIN.
correction factors, an ICP
analyzed.
4.7.9.2
m:
The ICS c
Solution A
beginning and end of each analysis run or a
hour working shift, whichever is more
.e ICV.
/two solutions: Solution A and Solution AB.
the interferents, and Solution AB consists of
December, 1991
Page D-53
-------
Exhibit D
Metal Analysis of Ambient Air
the analytes mixed with the interferents. An ICS
analyzing both solutions consecutively (starting/wit
all masses used for each analyte reported by ICP'-MS
lysis consists of
Solution A) for
The ICS shall be obtained from EPA (EMSL/lfr) i^Kavailatle and
analyzed according to the instructions suppl/led/with eke ICS
If the ICP ICS is not available from
shall be prepared with interferent and a;
levels specified in Table 3, Exhbit C.
deviation shall be established by ini
five times repetitively for each ana'
an independent
:e concentrations
mean value and standard
the ICS at least
If true values for analytes coi
ICP-MS are not supplied with the I(
initially analyzing the ICS at least
particular analytes. This mean determinal
analytical run where the results for the prevH
met all contract specifications. Additionally,
initial mean determination j£to~~be—used as the
lifetime of that solution
4.7.9.4 Calculations
% Recovery ••
4.7.9.5 Technical Ac
Recovery for/tb
value (i.e.,
4.7.9.6 CorrectfiveCAction
If the ICS
criteria, terminat
Jfy
analytl
4.7.9.
S and analyzed by
all be determined by
repetitively for the
be made during an
lied EPA ICS
It of this
true^va'lue for the
m is exhausted).
Eq. D-21
percent of the true
es not meet the technical acceptance
sis, correct the problem, recalibrate the
ion, and reanalyze all of the
lastscompliant ICS was analyzed.
pcentration (/ig/L), true concentration
an and standard deviation on FORM V-AAIN.
Leviation shall be reported in the raw data.
December, 1991
Page D-54
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Exhibit D
Metal Analysis of Ambient Air
4.7.10 Spike Sample Analysis
4.7.10.1 Summary
To provide information about the effect of
the digestion, a known amount of analyte is
sample.
4.7.10.2 Frequency
At least one spike sample analysis
group of samples for each SDG. EPA
sample analysis upon special request
the Contractor will be paid.
le matrix on
into a
be performed on each
tional spike
Officer, for which
If two analytical methods are
for the same analyte within a SDG (e
samples shall be run by each method use
4.7.10.3 Procedure
The spike is added bef
digestion) at concentratio:
indicated in Table D-3.
Samples identified as field
sample analysis. EPA may
the spike sample analysis. In
one spike sample
contract criteria/f flae->all
method in the SI
4.7.10.4 Calcul
x 100
ie reported values
and GFAA), then spike
ation (i.e., prior to
>le solution as
be used for spiked
specific sample be used for
ice where there is more than
le recovery is not within
.e same matrix, level, and
Eq. D/IN-22
performed on the same sample that is
le analysis, spike calculations shall be
of the sample designated as the "original
Duplicate Sample Analysis) . The average of
be used for the purpose of determining
December, 1991
Page D-55
-------
Exhibit D
Metal Analysis of Ambient Air
-rument
emulating percent
When the sample concentration is less than the
detection limit, use SR -= 0 only for purposes of
recovery.
4.7.10.5 Technical Acceptance Criteria
Recovery for the spike should be within
amount (i.e., 75-125 percent).
4.7.10.6 Corrective Action
If the spike recovery is not with:
the data of all samples received ass
determined by the same analytical
letter "N" on FORMs I-AAIN and VI-
An exception to this rule is granted>in situations where the
sample concentration exceeds the spike conc^n^ratibnby a factor of
four or more. In such an event, the data shall>be rep^srted unflagged
even if the percent recovery//~does_jiot meet the 75^125^ percent recovery
criteria.
iked
75-125 percent,
t spike sample and
lagged with the
4.7.10.7 Documentation
Report the spiked sample
percent recovery for the spike
The units for
7.11 Duplicate Sampl
4.7.11.1 Summary
e results, spike added and
is on FORM VI-AAIN.
will be in
Duplicat
and analysis
analytical metho
4.7.11.2 Fr
for the^same
duplicate
ample are carried through the preparation
jfde information about the precision of the
as matrix effects.
te sampler analysis shall be performed on each
SDG. EPA may require additional duplicate
il request by the Project Officer, for which
/ds are used to obtain the reported values
Lth/n a SDG (e.g., ICP-MS and GFAA), then
LI /be run by each method used.
December, 1991
Page D-56
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Exhibit D
Metal Analysis of Ambient Air
4.7.11.3 Procedure
Samples identified as field blanks cannot be jasefi for duplicate
sample analysis.
EPA may require that a specific sample be,
sample analysis.
In the instance where there is more
SDG and one duplicate result is not with;
the samples of the SDG.
Duplicate sample analyses are rec
relative percent difference.
4.7.11.4 Calculations
RPD =
Eq. D/IN-23
where:
RPD - Relative Pe"
S - First Sample \al
D = Second Sample
Duplicates cannot be averaged
4.7.11.5 Technical Acereptance^riteria
A control 1
and duplicate
(Exhibit C).
values less
If one restf
below, use the ±
If
flag with
with that
dup]
Die
ate).
'orting on FORM I-AAIN.
hall be used for original
equal to five times CRQL
11 be used for sample
le five times CRQL level and the other is
than the MQL, the RPD is not
for each analyte will be added to FORM IX-
on precision results.
results are outside the control limits,
the data for samples received associated
December, 1991
Page D-57
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Exhibit D
Metal Analysis of Ambient Air
4.7.11.7 Documentation
The results in fig/'L of the duplicate sample
reported on FORM VIII-AAIN.
The absolute value of the control limit
the "CONTROL LIMIT" column on FORM VIII-
4.7.12 Laboratory Control Samples
4.7.12.1 Summary
A laboratory control sample (LCS
ensure against analyte loss in the/s
4.7.12.2 Frequency
One LCS shall be prepared and analyzed for
in a SDG, or for each batch of samples, whicheve
ered in
4.7.12.3 Procedure
A LCS shall be analyzed
preparations, analytical methoc
EPA samples received.
The LCS solution
other EPA Quality
may be used.)
4.7.12.4 Calcula
x 100
pup of samples
frequent.
same sample
procedures employed for the
;m EPA. (If unavailable,
other certified materials
4.7.12.5 Technical Ac
4.7.1
pr
and re
Eq. D/IN-24
Ithin ± 20 percent of the true
the exception of Ag and Sb.
for the LCS falls outside the technical
;he analyses shall be terminated, the
samples associated with that LCS reprepared
December, 1991
Page D-58
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.12.7 Documentation
Report the LCS found concentration (/ig/L), tr^e Concentration (in
/ig/L), and percent recovery on FORM IX-AAIN.
4.7.13 Performance Evaluation Sample (PES)
4.7.13.1 Summary
The performance evaluation sample
monitoring the laboratory performance fc
quantification.
sists the Agenc
lyte i
4.7.13.2 Frequency
One PES shall be delivered, pr
of samples in a SDG, or for each ha*
frequent.
4.7.13.3 Procedure
A PES shall be analyzed
preparations, analytical mi
EPA samples received.
The PES solution shall be o
contractor must contact the Agen<
4.7.13.4 Calculations
Not applicabl
4.7.13.5 Technic
Recovery
of analyte.
4.7.13.6 Corrective
ed for every group
, whichever is more
te using the^same sample
QA/QC~~prtJeedur_es employed for the
EPA. (If unavailable, the
for instructions.)
75 percent of the true value
PES falls below 75 percent, the
to the following actions:
not 1
and/or\CurX Notice for unacceptable performance;
Eduction of the number^ of samples shipped to the laboratory;
iipment;
A si£e
-------
Exhibit D
Metal Analysis of Ambient Air
• A full data audit; or
Require the laboratory to analyze remedial P/
In addition to the above cited actions,
provide the Technical and Administrative Pro,
correction action report on every unaccept
PES score within seven days of written or
personnel.
4.7.13.7 Documentation
Report the PES results on Form
4.7.14 Internal Standards for ICP-MS
4.7.14.1 Summary
A minimum of three internal standards,
shall be used to check and correct the ICP-MS
of physical interferences.
4.7.14.2 Frequency
Analyze with each sample,
CCB.
4.7.14.3 Procedure
shall also
written
xcent)
Each sample,
internal standa:
same sample pr
employed for
4.7.14.4 Calcuiati^
the mass range,
the presence
ysis, PES, CCV, and
x 100
be spiked with the
each analyte using the
and QA/QC procedures
Eq. D/IN-25 :
4.7.14.
The inte
duplicate,
spiki
of the internal standard in the blank
on standard;
of internal standard in the EPA Sample No.;
fference.
e Criteria
of an internal standard for each sample,
\, and PES shall agree within ± 50 percent of
December, 1991
Page D-60
-------
Exhibit D
Metal Analysis of Ambient Air
the intensity level of the internal standard of th<
calibration blank standard solution (SOT) . MQLs shal,
in Exhibit C.
itial
be < the CRQLs
The intensity levels of the internal standard fcJTS^the ICV, ICB,
CCV, and CCB solutions must agree within ± 20/pei?cent
instensity level of the internal standard of/th/ initial calibration
blank solution (SOj).
4.7.14.6 Corrective Action
If the internal standard intensity
percent of the sample, the sample mus
five fold (1:4) dilution and reanaly;
percent difference (ZD) remains gr<
interference must be suspected,
flagged with an "E." The analyt
be listed in the comment section on
AA1N, and VIII-AAIN.
does not agree ± 50
ter performing a
:ensity level
cent, a physical
XV-AAIN must be
.e interferences must
ate FORM I-AAIN, VII-
If the internal standard Jjitensity level does not agree within ±
20 percent for the ICV andylCB/~ERe-«aa]«ysis shall be^^terminated, the
problem corrected, and a new analytical rurPsTtaiUje^ started.
If the internal standard intensity Leve/does~~~no't agree within ±
20 percent for the CCV and CCB,\terBn.nateid the analysis, correct the
problem, and reanalyze the CCV/CCfi only /nee. If the first CCV/CCB
reanalysis yields a ZD value within, the/control limits, then the
preceding 10 analytical—samples or ail analytical samples analyzed
since the last compliant calibration verification may be reanalyzed
for the analytes/affe'cteak Otherwise, she ^Instrument shall be
recalibrated, t)ae oalibratlonrvertfied arid/the affected analytical
samples rerun /n tzne content of^a new"
4.7.14.7 Doct
itacion
The internal
for each ICP-MS
jercent difference (ZD) shall be reported
FORM XV-AAIN.
4.7.15 Metl
4.7.15.;
:ion Limits
iry
?rlor to sample an^lys
sh-all/be determined
(.5.2 frequency
Ls, the method quantitation limit (MQL)
instrument that will be used.
MQ:
contract
the end of
shatlxbe determined within 30 days of the start of the
at jbeg.s't quarterly (every three calendar months) until
thVvContrac
December, 1991
Page D-61
-------
Exhibit D
Metal Analysis of Ambient Air
4.7.15.3 Procedure
MQLs (in ng/L) shall be determined by multip,
average of the standard deviations (un_i)
nonconsecutive days from the consecutive anal;
PB extracts. Each measurement must be perf
separate analytical sample (i.e., each mea:
a rinse and/or any other procedure normal
analysis of separate samples). MQLs
for each mass and mass number used in t!
by three, the
on"
se\
\
as
lent must
shaj
The quarterly determined MQL for
used as the MQL for that instrument;
instrument is adjusted in anyway tl
that instrument shall be redetermii
use as the established MQL for that ins
the quarter.
4.7.15.4 Calculations
MQ.
iall always be
ter. If the
MQL, the MQL for
results submitted for
or the remainder of
Eq. D/IN-26
4.7 .15.5 Technical Acceptance Cri,
The MQLs shall be < the CRQLs'
4.7 .15.6 Corrective Actj.
If an instrum.
instrument cann<
concentration
2, Exhibit C.
or an analyte, that
less the analyte
ive times the reported MQL.
4.7.15.7 Doc
MQLs shall
FORM.XI-AAIN for e
used for the_ajaalysis
the
SDG.
4.7.16
4.7/16
intere
each analjr
with each data package and reported on
snt used. If multiple instruments are
te within a SDG, the highest MQL for
jrting concentration values for that
tral and isobaric interferences,
[factors are determined for all masses used for
ICP-MS.
December, 1991
Page D-62
-------
Exhibit D
Metal Analysis of Ambient Air
/contract, the ICP
'within three
atvieast annually
4.7.16.2 Frequency
Before any field samples are analyzed under
interelement correction factors shall be determ
months prior to the start of contract analyses
thereafter.
4.7.16.3 Procedure
Correction factors shall be determined under the same
conditions used for sample analysis. If the instrument was adjusted
in any way that may affect the interelemein; correction factors, the
factors shall be redetermined and the/results submitted for use.
Follow the instrument manufacti;
interelement correction factors.
4.7.16.4 Calculations
Not applicable.
4.7.16.5 Technical Accept
Not applicable.
4.7.16.6 Corrective Action
Not applicable.
4.7.16.7 DocumentXtio,
Results fro:
be reported o
tions for applying
4.8 PROCEDURE
4.8.1 Initiate
computer.
4.8.2 Sey up
at least
samples / I;
soluti
of lea's
4.8.3 ^Sonduc
solution (
the forms in
factors determination shall
parameters.
configuration of instrument
proper operating parameters. Allow
•instrument to equilibrate before analyzing any
station is verified by running the tuning
>t four times with relative standard deviations
\thq analytes contained in the tuning solution.
n and resolution checks using the tuning
Lements Li, Co, In, and Tl). The intensities on
Cable D-6) for the response factor criteria
December, 1991
Page D-63
-------
Exhibit D
Metal Analysis of Ambient Air
are recommendations which might be helpful when setti
but are not required criteria. The mass calibration
criteria specified in Table D-6, if mass calibratio
then the mass calibration must be adjusted to the
resolution must also be verified to be less than
percent peak height. To verify, the tuning sol
the beginning and end of each eight hour shift
criteria.
4.8.4 Calibration and Sample Analysis
the instruments
meet the
iteed those criteria
^values. The
jwidth at 10
zed at
4.8.4.1 Calibrate the instrument for the atfalytes
calibration blank and at least a singl standard
manufacturer's recommended procedure
which will be used in analysis. Fl
between each standard solution. Repor
calibration and sample analysis and use
integrations for both standardization and samjJi^ ana
two replicate integrations are required for both
analysis. The raw data must insludethe
interest using the
ding to the
configuration
the rinse blank
ation during the
of the multiple
,sis. A minimum of
JLibraXj-on and sample
elements in
each integration as well as
detector configurations are
detector configuration is b
concentrati
lie averager—Additionally ,^if different
datamustr-Mwiicate which
NOTE: Some elements (such as Hg,
times which need to be determined fi
memory tests on the solution in Table*
will not affect the 4*Ca"~qua>lity.
'MoX require extended flushing
each/instrumental system. Run the
>-7\to verify that memory problems
mass
4.8.5 As a minimum
monitored to determine/potential effec
analyte peaks.
as a minimum mus
listed in Table
simultaneously in
informatj
include the
ifch
would\af£ect data quality must be
fromSmatrix components on the
to assess data quality and
e boldfaced and underlined,
lement. TbTese masses must be monitored
an or at the time quantification occurs.
4.8.6 Flush the system^
seconds
least 30
ollectl
4.9
jilnte and reanalyz*
aoee for an analyse
eac
rinse blank solution for a least 30
ample. Aspirate each sample for at
4.9.2 To obtain tm
interference-corrected'
amples that are more concentrated than the
'ormed, the appropriate corrections must be
!yte air concentration (in jtg/m3), multiply the
ilyte values (in /ig/L) by nine times the
December, 1991
Page D-64
-------
Exhibit D
Metal Analysis of Ambient Air
appropriate volume (in liters) used in the extraction
volume of air (in standard m3) sampled and the number
digested for the sample. The factor "9" represents
in2) of the Hi-Vol filter exposed to .the air stream/drv
area (7 in2) in one 1" x 8" strip.
ivide by the
x 8" strips
otal area (63
ded by the exposed
Analyte Cone.
In aii,
(9) (
Interference-Correct
Value, yg/L
no.ofstrips „
digested x
L- D-27
4.10 DOCUMENTATION
4.10.1 Report the air concentration val/
corrected analyte value in Mg/L om FOE
the interference-
December, 1991
Page D-65
-------
Exhibit D
Metal Analysis of Ambient Air
SECTION 5
SAMPLE ANALYSIS
BY
GRAPHITE FURNACE ATOMIC ABSORPTION (GF
5.1 INTRODUCTION
5.1.1 GFAA analysis procedures are provic
quantitation limits (where required) for the
listed in Table 1 the Target Analyte List/in,
ilysis of metal analytes
libit
5.1.2 Because of the differences among various
satisfactory instruments, no detailed/instrument
can be provided. Instead, the analyst^is rerBrr>6d
provided by the manufacturer of that instrument.
5.2 SUMMARY OF METHOD
s/and models of
Operating instructions
o the instructions
5.2.1 Using the furnace tec!
absorption spectrophotometer, (a raptesentative"
placed in a graphite tube in th\ furnace,
and atomized. Radiation from a givetK exci
the vapor containing ground state
the transmitted radiation decreases
ground state element in the vapor. The me
placed in the beam of radra^ipn by incr\as
furnace thereby causing the injected spe
monochromator isolates ;Cne~"characteristic
lamp or an electrcmles/s furnace
the attenuated transmitted raaiation
junction witn>an/atomic
t of a sample is
to7dryness, charred,
s passed through
element. The intensity of
tion to the amount of the
atoms to be measured are
the temperature of the
to be volatilized. A
tion from a hollow cathode
tosensitive device measures
5.3 INTERFERENCE
5.3.1 .The compos iTfc^n of the sample matrix can have a major effect on
the analysis. By modf^ing the sample matrix, either to remove
interferences—et—tostabilize tttfexanalyte, interferences can be minimized.
Examples afe the addi^on of^ammonrfojn nitrate to remove alkali chlorides
and the /additr±oTr~D£^ammat^.um phosphate to retain cadmium.
& furnace during atomization may have
[compassing the analytical wavelength.
:d correction is required for all furnace
5.3.3
background in
compensated for,
ounfl correction cannot correct for all types of
en the background interference cannot be
:n alternate wavelength, chemically separate the
December, 1991
Page D-66
-------
Exhibit D
Metal Analysis of Ambient Air
ackground
/ix can sometimes
5.erature or
>e taken to
analyte from the interferant, or use an alternate form
correction (e.g., Zeeman background correction).
5.3.4 Interferences from a smoke producing sample
be reduced by extending the charring time at a higi
utilizing an ashing cycle in the presence of air.
prevent loss of analyte.
5.4 APPARATUS
5.4.1 Atomic absorption spectrophotometer:/ Single or dual channel,
single or double beam instrument having a grating monoehromator,
photomultiplier detector, adjustable slit^7 j wave length/^ range of 190- to
800-nm, background correction, and prov^siops for interfacing with a
recording device.
5.4.2 Graphite furnace: Any furnace dev
specified temperatures is satisfactory.
5.4.3 Operational requirements:
various makes and models of sat
operating instructions can be
follow the instructions provided\by
instrument. Sensitivity, inst
dynamic range, and interference
established for each individual anal;
is the responsibility of the analyst
configuration and operating ^conditions
requirements set forth >£n this
data confirming instrumen;
of reaching the
between
ovided. Insl
tacturer
it lietectidn
ef:
cfoi
Because of the dii
instruments,
,e_ analyst should
ie particular
feeision, linear
investigated and
t particular instrument. It
:y that the instrument
tisfy the analytical
maintain quality control
ical results.
veri
cument ar
ice and
5.5 Reagents and Standard
5.5.1 Matrix ma/chi
standards, and qua!it
values due to poss]
5.5.2 Cal ibrations tandal
solutions atxCKetim&--«f ana]
least thrae calibration
range byycomjmiing
flask. /The/calibration S^ant
acid oy c<
ie /samples tsjiandatory for all blanks,
>1 /amples, to avoid inaccurate concentration
curve deviations.
repared by diluting stock metal
are discarded after use. Prepare at
raduated amounts in the appropriate
late volume of stock solution in a volumetric
.rds must be prepared using the same type of
the same concentration.
5.5.3. Twd
calibrabipn
preparatio:
from the reage
required for GFAA analysis; the
tablishing the analytical curve while the
used/to /Indicate possible contamination resulting
s used in the sample processing.
December, 1991
Page D-67
-------
Exhibit D
Metal Analysis of Ambient Air
5.6 QUALITY CONTROL
5.6.1 Instrument Calibration
5.6.1.1 Summary
Prior to the analysis of samples and re
shall be initially calibrated to determine
5.6.1.2 Frequency
Instruments shall be calibrated
each time the instrument is set up.
5.6.1.3 Procedure
Calibration standards shall be
solutions at the time of analysis, and
Calibration standards shall be prepared usi
acid or combination of acids/^-and at the same
result in the samples foil'
system
oncexevery 24 hours and
The instrument shall be ci
manufacturer's recommended profe
points. Beginning with a calibz
highest standard, run at least tree
standard shall be a blank, and another
Baseline corretio
each and every
Resloping
immediately
the stock
ded after use.
type of
ion as will
.nstrument
four calibration
and working towards the
standards. One calibration
11 be at the CRQL.
as it is performed after
CB, respectively.
is immediately preceded and
5.6.1.4 Calcula
Not applicable.
/- '
5.6.1.5 Technical
5.6.
L
5.6.1.7
The inst
the raw data
irdization date and time shall be included in
Orations shall be in fig/L.
December, 1991
Page D-68
-------
Exhibit D
Metal Analysis of Ambient Air
5.6.2 Initial Calibration Verification
5.6.2.1 Summary
Immediately after the GFAA system has been
accuracy of the initial calibration shall be
for every analyte by the analysis of EPA In
Verification Solutions(s) (ICV) at each wa-
5.6.2.2 Frequency
Each time the instrument is calibr
immediately following the calibratio
analyzed.
5.6.2.3 Procedure
, the
documented
s.
the ICV shall be run
samples are
instrume
If the ICV solution(s) are not
certified solution of an analyte is not
analyses shall be conducted on an independe
concentration other than that used for
within the calibration r
> standard composed of the
used in the standards for
5.6.2.4 Calculat ions
% Recovery =
5.6.2.5 Technical
Recovery fo:
value (i.e.,
5.6.2.6 Corre
When reco
criteria, the .ana
instrument
5.6.2.7
EPA, or where a
from any source,
rd at a
ation, but
'is defined as a
erent source than those
Eq. D-28
recalibra
0 percent of the true
ICV exceed the technical acceptance
LI be terminated, the problem corrected, the
calibration reverified.
concentration (in /ig/L), true concentration
overy on FORM II-AAIN.
Verification
To ei
continuing
reported for e\
accuracy during an analysis run, a
verification solution (CCV) is analyzed and
length used for the analysis of each analyte.
December, 1991
Page D-69
-------
Exhibit D
Metal Analysis of Ambient Air
two hours
5.6.3.2 Frequency
The CCV is run at a frequency of 10 percent,
during an analysis run, whichever is more fre
The CCV is also run after the last anal
analysis run.
5.6.3.3 Procedure
The CCV shall contain the analyte
the mid-range of the calibration c
The same CCV shall be used thr
of samples received.
If the ICV solution(s) are not availal
certified solution of an analyte is not aval
analyses shall be conducted on an independent s
concentration other than tha~t
within the calibration range. ^AnindepeS
standard composed of the analyci»s~~?ftTO-~a, different
used in the standards for the\ins£rument
runs for a Case
or where a
any source,
t a
ration, but
d is defined as a
urce than those
Each CCV analyzed shall reflect
the associated analytical samples\the
or. the preceding analytical samples
duration of analysis, rinses and othe1
affect the CCV nu4sure7r*-cesu\t shall
greater extent iKianr the
samples. For /nstzance,
and the blank/immediately/
time between/the{ CCV
it shall i
consecutive
tions of analysis for all
receding 10 analytical samples
the previous CCV). The
related operations that may
be\ applied to the CCV to a
t>s. /he associated analytical
time between a CCV analysis
well as the difference in
sample Immediately preceding
st difference in time between any two
les associated with the CCV.
different
it
analytii
5.6.3.4 Calci
eecov
icentzation
Tzue^Qbncentzation
x 100
Eq. D-29
5.6.,8-5/Technical Accept
Criteria
Rec^s^ery for the CCfr sldall be within ± 10 percent of the true
90-110 p/rcent).
(i.
5.6.3.6 Corr^ctive^
When recover
criteria, the anal;
[S Ol
the CCV exceed the technical acceptance
shall be stopped, the problem corrected, the
December, 1991
Page D-70
-------
Exhibit D
Metal Analysis of Ambient Air
instrument recalibrated, the calibration reverifie
10 analytical samples reanalyzed (or all analytic
last compliant CCV) .
5.6.3.7 Documentation
Report the CCV found concentration (in
(in fig/L) , and percent recovery on FORM
d the preceding
les since the
5.6.4 CRQL Standard
5.6.4.1 Summary
To verify linearity near the
GFAA standard at two times the CRQJ
greater. This standard shall be
analysis.
5.6.4.2 Frequency
The CRQL standard shall fee—sun__at the
sample analysis run, or a minimum
is more frequent.
^~^/
fore the ICV solution.
Recovery o
true value for
r shall analyze a
,e MQL, whichever is
•e length used for
end of each
Hours, whichever
5.6.4.3 Procedure
The CRQL standard is not to
5.6.4.4 Calculations
%
x 100
Eq. D-30
5.6.4.5 Techni
5.6.
Report
concentration
indard shall be within ± 15 percent of the
used for analysis.
.recovery does not fall within the technical
Lnate the analysis, correct the problem and
lies since the last compliant CRQL
ird's found concentration (in ^g/L), true
and percent recovery on FORM III-AAIN.
December, 1991
Page D-71
-------
Exhibit D
Metal Analvsis of Ambient: Air
5.6.6 Continuing
5.6.5 Initial Calibration Blank
5.6.5.1 Summary
To verify that the GFAA system is not cont/
calibration blank (ICB) shall be analyzed afj
5.6.5,2 Frequency
The ICB shall be analyzed each time
immediately after the ICV.
5.6.5.3 Procedure
If the absolute value of the I
result shall be reported.
5.6.5.4 Calculations
Not applicable.
5.6.5.5 Technical Acceptance C
The absolute value of the I1
5.6.5.6 Corrective Action
ss than the CRQL.
When the ICB
criteria, tennina
the calibration,
the technical acceptance
>blem, recalibrate, verify
/«g/L on FORM IV-AAIN.
stem is not contaminated during the analysis
blanks (CCB) are analyzed.
'equency of 10 percent or every two hours,
ir. every CCV.
December, 1991
Page D-72
-------
Exhibit D
Metal Analysis of Ambient Air
s run.
ie MQL, the
5.6.6.3 Procedure
A CCB shall be run after the last CCV in the
If the absolute value of the CCB is greate
result shall be reported.
5.6.6.4 Calculations
Not applicable.
5.6.6.5 Technical Acceptance Criteria
The absolute value of the CCB
5.6.6.6 Corrective Action
\" t
When the CCB concentration does not rne^t thev^echnical acceptance
criteria, terminate analysis, correct the problem/^secalibrate, verify
the calibration, and reanalyze the preceding lo^analytlpal samples (or
all analytical samples sinc^The—las_t_compliant
5.6.6.7 Documentation
Report the ICB values in
5.6.7 Preparation Blanks
5.6.7.1 Summary
To ensure
preparation
5.6.7.2 Frequi
At least o
or with each bat
5.6.7.3 P:
ample preparation, a
bl
>t be prepared and analyzed with every SDG
Les digested, whichever is more frequent.
of
ASTM Type II water processed through each
lysis procedure step (see Exhibit D).
les in an SDG is to be assigned to PB one,
to PB two, etc.
December, 1991
Page D-73
-------
Exhibit D
Metal Analvsis of Ambient Air
5.6.7.5 Technical Acceptance Criteria
The absolute value of the PB must be less
5.6.7.6 Corrective Action
If the absolute value of the PB concen
equal to the CRQL, no corrective action
If any analyte concentration in the,
lowest concentration of that analyte
10 times the blank concentration.
with the blank and with the analyte
the blank concentration and above
reanalyzed for that analyte. The
corrected for the blank value.
If the concentration of the blank is bel
all samples reported below 10 times CRQL associa*
shall be redigested and re
5.6.8.2 Frequ
At least one
group of sangles for
sample
the Cc
above the CRQL, the
j/ted samples must be
>les associated
less than 10 times
be redigested and
cation is not to be
Lative CRQL, then
the blank
5.6.7.7 Documentation
The values for the PB shall"
5.6.8 Spike Sample Analysis
5.6.8.1 Summary
To provide infoymation\ab
the digestion,/a
sample.
in /tg/L on FORM IV-AAIN.
of the sample matrix on
s added (spiked) into a
paid.
analysis shall be performed on each
(EPA may require additional spike
sst by the Project Officer, for which
.methods are used to obtain the reported values
SDG (e.g., ICP and GFAA), then spike
:h method used.
5.6.87
The
digestion)
indicated in
efore the sample preparation (i.e., prior to
tttration levels in the Spike Sample solution as
December, 1991
Page D-74
-------
Exhibit D
Metal Analysis of Ambient Air
Samples identified as field blanks cannot be us^o^or spiked
sample analysis.
EPA may require that a specific sample be us^d £or the spike
sample analysis.
In the instance where there is more than/one/spiKtexsanipvbevT>er
method per SDG and one spike sample recovery is not witfein^ contact
criteria, flag all the samples for the saijnsCmethod in the
5.6.8.4 Calculations
% Recovery =
where:
SSR = Spiked Sample Result^
SR - Sample Result,
SA - Spike Added, /Jg/L.
If the spike analysis is
chosen for the duplicate s
performed using the results
sample" (see 5.6.9 Duplicate
duplicate results cannot be
percent recovery.
When the sample concentration isN
detection limit, use SR -o\pnly for
recovery.
5.6.8.5 Technicay Acceptance/Criteria
Recovery
amount (i.e .C 75
on the same sample that is
calculations shall be
as the "original
average of the
ose of determining
than the instrument
es of calculating percent
in ± 25 percent of the.spiked
5.6.8.6 Corrective
even
criteria
or within the limits of 75-125
received associated with that spike
the same analytical method shall be flagged
I-AAIN and VII-AAIN.
Le is granted in situations where the
the spike concentration by a factor of
/event, the data shall be reported unflagged
does not meet the 75-125 percent recovery
December, 1991
Page D-75
-------
Exhibit D
Metal Analvsis of Ambient Air
When the digestion spike recovery falls
acceptance criteria and the sample result does
the spike added, an analytical spike must be p
metals that do not meet the specified criteri
Spike the unspiked aliquot of the sample at
level or two times CRQL, whichever is great
5.6.8.7 Documentation
Report the spiked sample results,
percent recovery for the digestion spj
AAIN.
The units for reporting spike
5.6.9 Duplicate Sample Analysis
5.6.9.1 Summary
Duplicate aliquots of a
and analysis steps to pr
analytical methods as well
5.6.9.2 Frequency
outsic
technical
:eed four times
for those
Ag).
enous
througK/the preparation
e precision of the
results, spike added and
sis on FORM VI-
At least one duplicate sample
group of samples for^eeeh^SDG
sample analysis upon speci
the Contractor will b€T>aid.
If two ana
for the same
samples sha
5.6.9.3 Procedure^
Samples idgntifie
sample
cr
Dupli
percent
s shall be performed on each
e additional duplicate
Project Officer, for which
obtain the reported values
P and GFAA), then duplicate
d.
blanks cannot be used for duplicate
^/
a. specific sample be used for the duplicate
Ijhere is more than one duplicate sample per
Licate result is not within contract
samples for the method in the SDG.
yses are required for calculation of relative
diffe
December, 1991
Page D-76
-------
Exhibit D
Metal Analysis of Ambient Air
Duplicates cannot be averaged for reporting on
5.6.9.4 Calculations
I-AAIN.
where:
RPD - Relative Percent Ditterefnc
S - First Sample Value (original), MgA;
Differ.
Eq. D-32
D - Second Sample Value
5.6.9.5 Technical Acceptance Criteri
L.
A control limit of ± 20 percen'
and duplicate sample values greater
(Exhibit C). A control limit of ± CRQL
values less than five times CRQL.
If one result is above
below, use the ± CRQL cri
For duplicate results
absolute value of the CRQL in
AAIN.
If both sample va
calculated.
Specific control/ limit
be used for original
to five times CRQL
for sample
the other is
enter the
LIMIT" column of FORM VIII-
ie MQL, the RPD is not
ill be added to FORM VIII-
results.
/ / / X-\ ^
5.6.9.6 CorrecytiWAction
If the duplicate sample results .are outside the control limits,
flag all the data^Sor samples received associated with that duplicate
sample with an asterisk "*.
5.6.9.7
licate sample analyses must be reported on
.e control limit (CRQL) shall be entered in
of FORM VIII-AAIN.
December, 1991
Page D-77
-------
Exhibit D
Metal Analysis of Ambient Air
5.6.10 Laboratory Control Samples
5.6.10.1 Summary
A laboratory control sample (LCS) is dige
ensure against analyte loss in the sample p
5.6.10.2 Frequency
One LCS shall be prepared and anal;
in a SDG or for each batch (i.e., a
same time) of samples, whichever is
5.6.10.3 Procedure
The LCS shall be analyzed for eacn"
preparations, analytical methods and QA/
EPA samples received.
cor every group of samples
prepared at the
The LCS solution shall
ICV solutions may be used)
If the EPA LCS is unavail
samples or other certified mat
5.6.10.4 Calculations
ing the same sample
es employed for the
d from EPA (if
on
5.6.10.5 Techni
Recovery
value (i.e./
Technical acce
determined at a
5.6.10.6
x 100
•ailable, the
Assurance Check
Eq. D-33
later
20 percent of the true
with exception of Ag and Sb.
teria for Ag and Sb in the .LCS will be
for the LCS falls outside the technical
lyses shall be terminated, the problem
associated with that LCS reprepared and
Report the
0*g/L)» and
perce
concentration (pg/L), true concentration
on FORM IX-AAIN.
scovery
December, 1991
Page D-78
-------
Exhibit D
Metal Analysis of Ambient Air
5.6.11 Performance Evaluation Sample (PES)
5.6.11.1 Summary
The performance evaluation sample (PES) as
monitoring the laboratory performance for a;
quantification.
5.6.11.2 Frequency
One PES shall be delivered, prepare
of samples in a SDG, or for each bate!
frequent.
5.6.11.3 Procedure
A PES shall be analyzed for each
preparations, analytical methods and
EPA samples received.
and
The PES solution shall
contractor must contact thi
5.6.11.4 Calculations
Not applicable.
5.6.11.5 Technical Acce
Recovery for
of analyte.
5.6.11.6 Correct
If the. p
Agency may t
and/or
analyzed for every group
whichever is more
the same sample
employed for the
from EPA. If^vjjavailable, the
nstructions.
ercent of the true value
the PES falls below 75 percent, the
limited to the following actions:
for unacceptable performance;
jer otxsatfles shipped to the laboratory;
lipment;
to analyze a remedial PES.
December, 1991
Page D-79
-------
Exhibit D
Metal Analysis of Ambient Atr
In addition to the above cited actions, the 1
provide the Technical and Administrative Project
correction action report on every unacceptable
PES score within seven days of written or verb
personnel.
5.6.11.7 Documentation
Report the PES on Form I-AAIN (in
5.6.12 Analytical Spike Sample Analysis/Met
5.6.12.1 Summary
To ensure against bias resultii
analyses, the Method of Standard AdditB
special procedures summarized in Figure
quantitation.
5.6.12.2 Frequency
All GFAA analyses for ea<
one analytical spike.
Stry shall also
a written
than 75 percent)
by Agency
A maximum of 10
may be performed tie
blanks. Each fu/1
determining 10
performed be
5.6.12.3 Proc
All GFAA analyst
range.
Ex-
Only
The frequency of MSA will de
spike.
The rec
the preparatic
calibration curve"
r all analytes.
d Additions
ence effects in GFAA
is utilized. The
required for
require at least
recovery of the analytical
maximum of 20 injections
ion verifications and
cal samples towards
.e., five full MSAs can be
ing MSA shall fall within the calibration
A, alKajrialyses require duplicate injections.
required for MSA quantitation. Average
ed for reporting purposes.
two times CRQL) of a sample must be run
le. The percent recovery of the analytical
thod of quantisation for the sample.
analytical spike will include the LCS and
The LCS must be quantitated from the
corrective action, if needed, taken accordingly.
December, 1991
Page D-80
-------
Exhibit D
Metal Analysis of Ambient Air
MSAs are not to be performed on the LCS or preparat
regardless of spike recovery results. If the pre;
analytical spike recovery is out of the control J/im:
the spiking solution must be verified by respikj
preparation blank once. If the preparation b
recovery is still out of control, correct the/prj
reanalyze all analytical samples associated
analytical spike is not required for the p
blank,
:ion blank
:s 85-115 percent,
ind rerunning the
'tical spike
respike and
gestion sp^ke sample.
T^7
If the spike recovery is < 40 percent^ tHe sample must be
by a factor of five to ten and rerun with another spike. This
must only be performed once. If after/the dilution the spike recovery
is still < 40 percent, report data fr/om the initial/undiluted analysis
and flag with an "E" to indicate interference p^objems.
If the spike recovery is > 40 p^rcen^xand/the/ sample absorbance or
concentration is < 50 percent of the spake, report the sample results
to the MQL. If the spike is less than eUxgerceht^or greater than 115
percent, flag the result with a "W."
If the sample absorbance
spike and the spike recove
percent, the sample must be
curve and reported down to tft
entration is < S&^p^rcent of the
is at orb"e"tweeiLJJ5percent and 115
directlyrfdm the calibration
If the sample absorbance or
spike and the spike recovery is >N85 percent
percent, the sample m\is_t:be quantit
ion is < 50 percent of the
or greater than 115
y MSA.
For analytical/ rupe—containing only
used for QC samples/duringN, t
an MSA mode onyy, KSA can pe used to\4etei
run.
single injections can be
struments that operate in
nine QC samples during that
The
quantitation
from use in the
£hree/spikes must be analyzed consecutively for MSA
:iajr spike run data is specifically excluded
.auantsLtation) .
areeT^guch that:
tely SO percent of the sample concentration;
,ely 100 percent of the sample concentration;
ly 150 percent of the sample concentration
xpressed in /ig/L).
December, 1991
Page D-81
-------
Exhibit D
Metal Analysis of Ambient Air
5.6.12.4 Calculations
% Recovery = SSR_~ SR x 100
Eq. D-34
where:
SSR = Spiked Sample Result;
SR - Sample Result; and
SA - Spike Added.
where:
RSD = Relative Standai
a,,.! « Standard deviation f"
x - Mean
5.6.12.5 Technical Acceptance
For concentrations >
within ± 20 percent of RSD o
s must agree
The analytical spike recoveries
control limits of ± 15 percent
or PB).
5.6.12.6 Corrective^Action
If the RSD /CV)/technical "accep
the sample
reported on FORM/I-AAIN
LCS and PB shall be within
is NOT performed on the LCS
teria are not met, rerun
11 not met, flag the value
H".
NOTE: The "
the sample.
ired for the analytical spike as well as
If the-?B~a«alyticar^fipike"x6echnical acceptance criteria are not
met, ve'rify the spikajig solti^eria\are stil* not met, correct the problem and
samples associated with the blank.
Sjpike technical acceptance criteria are not
id reanalyze all analytical samples
5.6.12.7
If the spikeNr^coyery is < 40 percent, the sample must be diluted
by a factor of five^co ten and rerun with another spike. This step
December, 1991
Page D-82
-------
Exhibit D
Metal Analysis of Ambient Air
must only be performed once. If after the dilutio
is still < 40 percent, report data from the initi
and flag with an "E" to indicate interference
If the spike recovery is £ 40 percent and
concentration is < 50 percent of the spike,
to the MQL. If the spike is less than 85 p
percent, flag the result with a "W."
spike recovery
^diluted analysis
ns.
absorbance or
le results
than 115
If the sample absorbance or concentration is < 50 percent oJ
spike and the spike recovery is at or between 85 percent and 115
percent, the sample must be quantitate/o djftrectly fcom the calibration
curve and reported down to the MQL.
The raw data package must inclu/fe aijsorbanc;
values for both injections, the average value
variation (or RSD).
id concentration
arid the coefficient of
The data for each MSA analysis must be clearly ^tientified in the
raw data documentation (using added concentrationxas ths x-variable
and absorbance as the y-variaTSte-}—along with the slbp^/x-intercept,
y-intercept, and correlation coe^fficienT^r-)~-f£»r__j:he least squares fit
of the data.
Reported values obtained
"S" on FORM I-AAIN if the correll
correlation coefficient is < 0.99!
XII-AAIN with a "+".
5.6.13 Method Quant i
5.6.13.1 Summary
The metho
samples are
iall be determined before any
instrument that will be used.
flagged with the letter
ficient is > 0.995. If the
the data on FORMs I-AAIN and
5.6.13.2 Frequency
MQLs
contr.
5.6.13/3
^rmined^wi thin 30 days of the start of the
every three calendar months).
be] determined by multiplying by three the
deviations (an-i) obtained on three
le analysis of a standard solution (each
at a concentration three times to five times
jfcturer's suggested instrument detection limit
consecutive measurements per day. Each measurement
December, 1991
Page D-83
-------
Exhibit D
Metal Analysis of Ambient Air
must be performed as though it were a separate
(i.e., each measurement shall be followed by a rd
procedure normally performed between the an
samples). MQLs shall be determined and report/
used in the analysis of the samples.
Leal sample
'and/or any other
separate
wavelength
The quarterly determined MQL for an inst
used as the MQL for that instrument during
instrument is adjusted in any way that
that instrument shall be redetermined
use as the established MQL for that ir
the quarter.
MQL must be determined in Mg/L.
5.6.13.4 Calculations
MQL = 3 x on.j
or
Eq. D-36
where :
— Standar
5.6.13.5 Technical Acceptance
The MQL shall meet the CRQLs
5.6.13.6 Corrective
If an inst
instrument
concentration
,ed in Exhibit C.
L for an analyte, that
lyte unless the sample
5.6.13.7 Doc
For each
and submitted with'
are used for_th_e
the GFAAsshall
SDG.
sd, MQLs shall be reported on FORM XV-AAIN
package. If multiple GFAA instruments
vmetal within a SDG, the highest MQL for
:ing concentration values for that
5.7 INSTRl
>t up the instrument with the proper operating parameters
the instrument manufacturer. The individual steps (drying,
Hid abomization) /require careful consideration to ensure each
process is carriedNout effectively. The instrument shall be allowed to
become therman^stabl^e^/befiore beginning any analysis. This usually
requires at least3Q minutes of operation prior to calibration.
Background correctionrsljgfll be used.
December, 1991
Page D-84
-------
Exhibit D
Metal Analysis of Ambient Air
5.7.2 Calibrate the instrument according to the manuf.
recommended procedures using calibration standard sol
5.7.3 In order to determine if the sample result
MSA, an analytical spike at two times CRQL shall b
after each sample analysis. The analytical spike,
to determine the need for MSA as explained in 5.y
solution volume shall not exceed 10 percent of
5.7.4 Dilute and reanalyze samples that ar
linear range (i.e., top calibration standarj
5.8 PROCEDURE
.rer's
be calculated by
and analyzed
be used
5.8.1 Calibration
5.8.1.1 Set up the instrument with
instrument shall be allowed to become the
analysis. This requires at least 30 minutes
lit prior to calibration.
5.8.1.2
if used.
Initiate appropriate; operating cor
pro
Ing parameters. The
before beginning
with the lamp
;ion of the computer,
5.9
5.8.1.3 Calibrate the instrument
calibration standard solution(s). "The
left to the discretion of the operator but;
calibration blank and a£_least three s\and
aware of the requirements inExhibits D
assurance that all sample—valued are with}
5.8.1.4 All stan«j
matched. A chi
calibration cui
Analysis Sequel
blanks, and s£
the acid s>£reit§th cl
can causer inacci
appropriate matrix matched
;r of standards utilized is
shall include a minimum of a
:ds. The operator should be
that provide for the
the calibration range.
solutions shall be matrix
iges the slope of the
'results.
5.9.1 Before beginnit
and CRA
analyses/
true
withit
may got
eles
apj
addit3
5.9.2 Upon"
PB extract(s) pi?
lie analysis run, analyze the ICB ICV,
tions intended for sample
concentration values shall not deviate from the
percent. The CRA recovery values must be
,rue values. The calibration blank values
these conditions are not met for any
discontinued and corrective action
'are met (see Exhibits D and E for
lysis of the ICV and ICB, analyze all method
the digested samples. If any of the
December, 1991
Page D-85
-------
Exhibit D
Metal Analysis of Ambient Air
blank(s) are not less than or equal to the CRQL, see,
for the appropriate action.
5.9.3 If the method blank(s) values are accep
If any LCS values deviate from the acceptable ring
E for the appropriate action.
5.9.4 If the LCS values are within the
method spike sample. If the recovery of
acceptable ranges, see Exhibits D and E ff
Proceed to the analysis of samples if
after consulting Exhibits D and E.
D and E
the LCS.
ibits D and
appropriate action.
acceptable or
joveries/vare
ilfezed aft
devO
dur5
5.9.5 The CCV and the CCB must be
sample analyses. CCV values shall
more than ± 10 percent. In addition, tfife^absol
calibration blank shall be lower than the
If these conditions are not met at any time
discontinue the analysis and see Exhibits D and
action.
5.9.6 At the end of the s
CCV. If the values for any of
limits, see Exhibits D and E.
5.10 Sample Analyses
5.10.1 All sample ex
Diluting sample extracts
dilution does not r
5.10.2 All cone
established call
within the cali
ivery 10 analytical
ron" the actual values by
values for the
yiantitation limits.
analysis,
appropriate
the CRA, CCB, and
'from the required
•zed without any dilution.
,sary provided that the
on below CRQL.
obtained within the
sis run. All concentrations
analyte are to be reported.
5.10.3 In order to dfefeerminex^f the sample result is to be calculated by
MSA, an analyticalsp ike atvstwo times CRQL shall be performed and analyzed
immediately/a'fter eafih-vsample^analys^is. The analytical spike recovery is
used to de€ermi«e-^the nee^dff or MS^as7^ explained in part 5.6.12 and Exhibit
E. The ^piking solution^ volume shall not exceed 10 percent of the sample
volume./
5.10.A eacbi aliquot shall not exceed 10 percent of the
volume of the al^xjuotx^Add/the appropriate amount of blank solution to
each aliquot to ma*ke^ the t^otal of spike plus blank volumes added equal.
December, 1991
Page D-86
-------
Exhibit D
Metal Analysis of Ambient Air
5.10.5 Using a calculator or a statistical package on/a^omputer,
determine the slope, the intercepts of the ordinate (V-ax/s) and the
abscissa (x-axis) , and the correlation coefficient usring/the found
concentration as the ordinate and the standard additfioi^ concentration as
the abscissa. The absolute value of the intercept/of tfte^abscissa is the
concentration of the analyte in the dilute soluti
coefficient is less than 0.995, then the analysed sKall"b< repeated. If
the second analysis correlation coefficient is /iesjs than
repeat the analysis using a smaller aliquot oi
certain to correct for the difference in volume
sample digest aliquot. If the correlation ^coefficient is still less tt
0.995, flag the sample data with a "+."
5.11 Calculations
5.11.1 Determine the method detectiol
deviation of the method blank analyte
addition plot.
5.11.2 Calculate sample extract concentrations
analyte concentration calculate^
in Sections 5.8.1. Calculate
/ig/m3 by multiplying the analyti
volume (liters) times 9 and divic
(standard m3) per filter and the
factor "9" represents the area (63 ih2)
the air stream divided by the exposed
r strips digested. The
Hi-Vol filter exposed to
in2) in one I"x8" strip.
_ airvolume
x sampled, std.m*
om the standard
d on the standard
Itiplying the
factors used
for each analyte in
extract
air sampled
Analyte
In aii.
Eq. D-37
Calcul
sample
levels relative to the corresponding unspiked
of
.t difference (RPD) for both the method and
the RPD by dividing the absolute value of
le value and the duplicate value by their
December, 1991
Page D-87
-------
Exhibit D
Metal Analysis of Ambient Air
RPD
15-01
S + D
x 100
Eq. D-38
where:
RPD -
S -
D -
Relative Percent Differern
First Sample Value (ori
Second Sample Value (dup'li^ate) , jug/L
December, 1991
Page D-88
-------
Exhibit D
Metal Analysis of Ambient Air
SECTION 6
BIBLIOGRAPHY
Winge, R.K., V.J. Peterson, and V.A. Fassel, "Inducti
Atomic Emission Spectroscopy Prominent Lines," EPA-6
Winefordner, J.D., "Trace Analysis: Spectroscopic,
Chemical Analysis, Vol. 46, pp. 41-42.
Handbook for Analytical Quality Control in Wat
EPA-600/4-79-019, USEPA Environmental Monitor
Cincinnati, Ohio, March 1979.
Garbarino, J.R. and Taylor, H.E., "An Indi
Emission Spectrometric Method for Routine
Spectroscopy 33, No. 3(1979).
Methods for Chemical Analysis of Water and Wastes.
Annual Book of ASTM Standards. Part/
Plasma-
and Wastewater Laboratories.
t Laboratory,
"Safety in Academic Che:
Publications, Committe
"Inductively Couple
Elements Analysis o:
Data/Protocol Review
EMSL/Cincinnati.
Federal Registe
"Standard
Filters,"
Research
Plasma Atomic
esting," Applied
-79-020.
"Carcinogens - Working With Carcindseriiv^-eeiiartaiient of Health, Education, and
Welfare, Public Health Service, Centex £>r Disease/Control/ National Institute
for Occupational Safety and Health, PuMidatioji Ncf. 77-206, Aug. 1977.
"OSHA Safety and Health Standards, General Industry," (29 CFR 1910),
Occupational Safety and Health Administration, >OSHA 2206, (Revised, January
1976).
Chemical Society
'ition, 1979.
£trometric Method of Trace
Method 200.7 modified by CLP Inorganic
method by Theodore D. Martin,
-46261.
Microwave Extraction of Glass-Fiber
U.S. Environmental Protection Agency,
1990.
G. Horl
A. L. Gray, S
J. J. Thompson and R
a 40B, 1555 (1985).
, 1525 (1985); 41B, 151 (1986).
Houk/Appl. Spectrosc. 41, 801 (1987).
December, 1991
Page D-89
-------
Exhibit D
Metal Analysis of Ambient Air
J. W. McLaren et al., Anal. Chem. 57, 2907 (1985).
F. E. Kichte et al., Anal. Chem. 59, 1150 (1987).
S. H. Tan and G. Horlick, Appl. Spectrosc. 40, 445 (1/986J>.
M. A. Vaughan and G. Horlick, Appl. Spectrosc. 40, A34/(1986).
/V
D. Beauchemin et al., Spectrochim. Acta 42B, 467/(19TB7).
R. S. Houk, Anal. Chem. 58, 97A (1986).
December, 1991
Page D-90
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-l / >
RECOMMENDED ICF WAVELENGTHS AND ESTIMATED/
INSTRUMENTAL DETECTION LIMITS / /
Element
Wavelength, nm1
' f^\ \
Estimated Detection
/ Limit, pfe^2 ^^
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Tin
Vanadium
Zinc
308.215
206.833
193.696
455.403
313.042
249.773
226.502
317.933
267.716
228.616
324.754
25
2
279\07
257.
202.03
231.604
766.491
(D
(2)
The wavelengths Tinted are ^recommended because of their sensitivity and
overall acceptance .^^^therStayelengths may be substituted if they can
provide theneeded sensifciyity^and are treated with the same corrective
techniqueXior spectsal interference. The use of alternate wavelengths
shall bpreperted-^in ran) with the/sample data.
ited instrumental detection limits as shown are taken from
rely Coupled Plasma-Atomic Emission Spectroscopy-Prominent Lines,"
5^4-79-017. They are \given as a guide for an instrumental limit.
method detection /limits are sample dependent and may vary as
sle^matrix varies^
(3) Highly
snt
operating conditions and plasma position.
December, 1991
Page D-91
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-2
/
EXAMPLE OF ANALYTE CONCENTRATION EQUIVALENTS /MG/1) ARISING
FROM INTERFERENTS AT THE 100 MG/L JUSVEL^
/ /^x.
Analyte
Aluminum
Antimony
Arsenic
Barium
Beiyllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Selenium
Silicon
Sodium
Thallium
Vanadium /
Zinc
Wavelength
(rim)
308.215
206.833
193.696
455.403
313.042
249.773
226.502
317.933
267.716
228.616
324.754
259.940
220.353
279.079
257.610
202.030
231.604
196.026
28&158
,888.385
/ 19/864
292.402
^^^s.sseX,
InterfjwenJ/ ^\ ^\
Al
-
0.47
1.3
—
—
0.04
-
—
-
-
—
~
0.17/
/ ,
M
^0.05X
^X.
0.23
~-X
_"\
0.30
—
-
Ca
-
-
-
-
—
-
-
—
-
-
-
^^
S=^
0.02
~ /
^ •*/
\y
- {.
\^
^X"
x -\
\ '
-)
; ,
Cr
-
2.9
0.44
—
-
-
/"= — -
(0.08^
x^
0.03\
-
x ~
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>.)r
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f
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^BJ^
*x
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) 0.05
/
Cu
-
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-/
k
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-
—
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0.14
f/^
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\^
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~~OOT-
^803^
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P003
\
\-N
oV
1^02
0.03
—
0.09
—
—
—
0.005
-
/Mg
-
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/
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<
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-
-
—
-
—
—
-
-
Nl\
-
—
—
-
-
-
0.02
-
-
0.03
—
—
-
-
—
—
-
-
-
-
-
-
0.29
^ T"^
\y
0.25
—
-
0.04
-
-
0.03
-
0.15
0.05
-
-
0.07
-
-
-
-
-
0.08
-
0.02
-
V
1.4
0.45
1.1
-
0.05
-
-
0.03
0.04
-
0.02
-
-
0.12
-
-
-
-
0.01
-
-
-
-
December, 1991
Page D-92
-------
Exhibit D
Metal Analvsis of Ambient Air
TABLE D-3
SPIKING LEVELS FOR SPIKE SAMPLE ANAL3
FOR INORGANIC ANALYSES
For ICP
and
ICP-MS
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Nickel
Potassium
Selei
Silj/er
Sc
nts fritiurat spike levels and
with ;an asterisk, must be
priate levels.
December, 1991
Page D-93
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-4
TONIG SOLUTION FOR ICP-MS
Concentration
Jft*g/6
'Lithium
Cobalt
Indium
Thallium
NOTE: Th
shall cons
analytes
concentratio
December, 1991
Page D-94
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-5
TUNING, RESPONSE FACTOR AND MASS CALIBRAT,
TUNING CRITERIA / /
m/z
7Lithium/59Cobalt
59Cobalt/59Cobalt
115Indium/59Cobalt
205Thallium/59Cobalt
Ion Abt^dayce Criteria
RESPONSE FACTOR
m/z
7Lithitan
59Cobalt
115Indium
102Ruthenium
205Thallium
Response Fa
Criteria
,000
MASSCALIBRATIONN
7Lithiufa /
59Cobait /
jW
alMum
20
EtactN^ass
L9160V7.1160
58/63^2-- 59.0332
IXJJ0407- 115.0040
204>7*4 - 205.0744
December, 1991
Page D-95
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-6
MEMORY TEST SOLUTION FOR ICP
The memory solution shall consist of the f
Analyte
Aluminum (Al)
Antimony (Sb
Arsenic (
Barium (
Beryllium
Calcium (Ca)
Cadmium (Cd)
Carbon (C)
Ch
(Se)
Silver (Ag)
lum .(Na)
(S)
(Ti)
Tritium (T)
Vanadium (V)
Zinc (Zn)
December, 1991
Page D-96
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-7
INTERNAL STANDARDS WHICH MAT BE USED IN
Internal Standard
Scandium (Sc)
Yttrium (Y)
Rhodium (Rh)/
Indium (In)
Terbium
Holmium
Bismuth (Bf)
Lithium (Li)
December, 1991
Page D-97
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-8
RECOMMENDED ELEMENTAL EXPRESSIONS FOR ISOBARIC IN
INCES
Analyte
Aluminum (Al)
Antimony (Sb)
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Cadmium (Cd)
Calcium (Ca)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Magnesium (Mg)
Manganese (Mn)
Nickel (Ni)
Silver (Ag)
Thallium (Tl)
Vanadium (V) /
Zinc (Zn) \
6l_ithium (Li)
Scandium (Scj^_—
Yttrium (Y/
Rhodiurn (Rnf
Indium (\ty
Torbiurrpp^))
HolmiurB^(Ho) x^
Bismuth (Bi)\
Isobaric
Correction
None
None
ArCI, Se
None
None
MoO, Sn
None
None
None
None
None
None
None
None
None "-
/No;«6~X
/ Jrone
f /C\0,Cr /
^ Ntarje /
^-fclpne ^
-^ Non>\
None,
Nene \
sn\ N
None j
None/ /
\Nqr4 /
Expression ProportionaUo Analyte
ConceynrationX^
(1.0000)(27M) / /^X^ ^\
(1.0000)(121M) ^ / ^\ ^X,
(1.0000)(75M) - (S/^f^M) + (2.5288)(82M)\
(1.0000)(135M)/ /
(LOOOO^M)/ / /">
(1 .0000)(1/M)/(0.0268)(^8M/- (1 .6285)(108M)
(LOOOOJ^S^ ^\/ /
^ I .uyuo^^iifi^ ^x^^ xNk^
/^ r\fW\\^^K/IN ^^x^ ^*x^
!?roeeoH!!M) "\/
<(i.oaeo)^M) ^~^^---~^_
(i^pobK2^^ y(i.pDix^97^+ (i.oooo)(206M)
(i.oobp)(^M)/ /
(1.0000)(^M) /
^LOOOOJ^MX \
(1\0000)(107M)\ ^
lo.oooo)?05^ v
(•K0^5^*4I- ^1158)^) + (0.3533)^)
/fl.OOOOJ^M)
(LOOOOJ^M)
(^GQOOJ^M)
V^QPOW^M)
(1.0000)(103M)
(1.0000)(115M) - (0.0005) (118M)
(1.0000)(159M)
(1.0000)(165M)
(1.0000)(165M)
= The total ion JXjun/ rate at the specified mass.
December, 1991
Page D-98
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-9
CONTRIBUTIONS OF CONCOMITANT ANALYTES TO NEARY ANALYTES FOR ICP-MS
WHEN RESOLUTION AND MEASUREMENT SCHEMES
(
NOT
int
Analyte
121Sb
121Sb
75AS
9Be
112Cd
114Cd
116Cd
5ZCr
^Cr
^Co
^Cu
^Cu
^Ni
^Cu
206pb
aBpb
^Mn
202Hg
^Ni
^i
107Ag
107Ag x--~
109^ x^-
1^Ag/
/^V
51V\
^*Zf^ \
e6ln \.
Interferent
Analyte
120Sn
122Te
74Se. 76Se
10B
1l3ln
115ln
115ln
51V
^Fe
S8|^j 60p^|
62fjj 64Mj
"Zn
^Ni
64Zn,66Zn
ao&n ^ —
"a/ ^^
O*tp^ OOffM
nVf f™
ISFfft f
/59cC /
^Cy ^sx/
106Pd/Nl^cl
-W6QJ lOBQ,^.
-**R(i11V
^cd,^^ N
^^b \
^r )
^Cu. ^Cu /
^bt»\ / /
Peak Width at 10% of the Pftak Height
1.0 amu
Integration Width
0.9 amu
60
360
50
100
40
1.5
15
140
5
/TIT
\ 30^ — .
^5 \
»\
20 X
\ 110
\2
J ^^
/ ojjr^
/10
/ 1
^^ w»
\ 500\
"vy
70
\ 30
I «
/ 20
60
0.3 amu
300
730 /
40/
Njrfne /
/560/
/ 3^
KXX25 ^
110^
7
. _610
^ 30
SB?
\ 3/ /
v V
\50\
iV N
\25Q\
Vv
>>5/
50
210
530
210
510
60
200
110
60
/ 0.8amu
Irttegratton Width
0.9 amu
/ 4
^940
/ 160
None/\
68/ /
t*/
•JoJ
iW
^fik "
300^
— —*««»_
zO — —
/— »^y
20
10
1
\ 160
' 120
40
160
20
5
80
5
90
140
170
70
80
0>amu
"^aio ^
600\
35
None
None
670
25
90
^^ 7
\/660
20
20
20
20
30
90
310
None
90
60
280
540
270
530
80
220
140
60
^
TE: Concentrations listed are the approximate level (mg/L) of
:erferent which givro an analyte concentration of 10 /*g/L.
December, 1991
Page D-99
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-10
ISOBARIC MOLECULAR-ION INTERFERENCES WHI'
AFFECT THE ANALYTES
Chlorine
Inter.
Hydroxyl
Inter.
Nitrogen
Inter.
PdO
AgO
CoO
SnO
SbO
SnO
SnO
SnO
SnO, CdO
CdO
NiOH
SbOH
SnOH
SnOH
SnOH
SnOH
InOH
CdOH
M
MoCI
MoCI
MoCI
SnN
SnN
SnN, CdN
MoN
MoN
MoN
MoN.ZrN
MoO
MoO, ZrO
MoO
MoO, ZrO
MoO
MoO
ZrO
MoO, ZrO
ArO
CIO
SO
MoOH
MoOH
MoOH
GeS
SeS, GeS
MoN, ZrN
MoN, ZrN
ZrOH
CIOH
ArOH
CaO
TiO, PO2
TiO
--"WOW-.
WOH ^
WOH
TaOH
December, 1991
Page D-100
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-10 (Continued)
Analyte
Oxygen
Inter.
I li •ri«jM«m«l
nyoroxyi
Inter.
Nitrogen
Inter.
Chlorine
Inter.
Sulfur
Inter.
'\Carbon
Tnter.
Other
61
Ni
*
76Se
^Se
74Se
Ag
Ag
107
109
si
"zn
66zn
70Zn
CaO
CaO
TiO
ScO
TiO
ZnO
NiO
ZnO
NiO
NiO
NiO
ZrO
CIO
SO
TiO
TiO
CrO
VO
FeO
KOH
CaOH
ScOH
CaOH
TK)H
CuOH
NiOH
CuOH
CoOH
NiOH
FeOH
ZrOH
MoOH
WOH
SOH
TiOH
TiOH
VOH
TiOH, CrOH
CrOH
WN
CaN
TIN
TIN
TIN
TiN,CrN
ZnN
ZnN
ZnN
NiN
CuN
NiN
MoN
NaCI
MgCI, NaCI
AJCI, MgCI
MgCI
Sid, AICI
Sea,
CaCI,
TiCI,
Mo"1
Be"*
Ba"1
NOTE: The information p:
described interferences
for informational p
e does, riot indicate that all of the
**ever, the table can be consulted
encountered.
December, 1991
Page D-101
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-ll
MASS CHOICES FOR ANALYTES WHICH MOST BE MONITORED
EITHER DURING THE ANALYTICAL RUN OR IN A SEPARATExSCANsFQR ICP-MS
Analytes
of
Interest
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Cerium
Chlorine
/
Chromium
Cobalt
/ /
Copper/
Gallium
Germanium
Lfon
Kryp
ton
/Lan
thanum
Lekd
121, 123
/ /
138, 137, 136, 135,
114.
42, 43,
, 4^ /
140
V
63/6S/
s56,
, 206. 204
/24/21, 26
, 108
December, 1991
Page D-102
-------
Exhibit D
Metal Analysis of Ambient Air
TABLE D-ll (Continued)
Analytes
of
Interest
Manganese
Mercury
Molybdenum
Nickel
Palladium
Potassium
Selenium
Silver
Sodium
Tellurium
Thallium
Tin
Titanium ^
Vanadium /
Xenon / /
Zinc / /
Mass / /~"\ ^\
55
202, 200. 199,
£ / "\ ^
201 / Y
98, 96, 92, 97, 9/ /
58, 60, 62, QL, §4 / /
105 /
^ //
12 '"X^ ^\/ /
80, 21, 82, 2i, 22^>< <\
1S2, 122 "\ "'N
13 /^^^^ -__ ^^
125 \ \^~-— -^ •_ ^~~~^7
205, 203\ \ / / ^^
m \ v/
^^ \ \
^*>\ \\
129 } ^^
x- v
e^.yk/C^TO/
NOTE: The^aasses vmich must be monitored are indicated by
underlining, rt^is sbcongly recommended that the other
elejaents-bemonitoxed to^ndicate other potential
:ular infefcrferen^fefi which could affect the data
:t^-\ X ^x/
December, 1991
Page D-103
-------
Exhibit D
Metal Analysis of Ambient Air
FIGURE D-l
TEMPLATE FOR CUTTING GLASS-FIBER FI
MMwM m FCWHT
To PfWMit FUfttf
FfwnStfcUnatD
PUctfc
Wldltiof
QraoMlem
foUtod (UniitfmlM) hi Hrtf
December, 1991
Page D-104
-------
Exhibit D
Metal Analysis of Ambient Air
FIGURE D-2
MICROWAVE DIGESTION SYSTEM
December, 1991
Page D-105
-------
Exhibit D
Metal Analysis of Ambient Air
FIGURE D-3
FURNACE ATOMIC ABSORPTION ANALYSES SC
Prepare and Analyze
Sample and One Spike
at 2 times the CRQL
(Double Injections Required)
Analyses within
Calibration Range
NO
Dilate Sample
YES
Recovery of Spike
Less than 40Z
NO
Sample Absorbance or
Cone. Less than SOX of
Spike Absorbance or Cone.
NO
^
YES \
^\
Spike Recovery
Greater than 85X/an(
Less than USX
\Report Results
Down to MQL
Report Results
Down to MQL
Flag with a "W"
Quantitate by MSA withx3
Spikes at 50%^_lfiO%, and
150Z of/Sample Ca
(Only
Quantitate from
Calibration Curve
and Report Down
to MQL
NO
If YES, repeat only once
Coefficient
0.995
NO
Flag Data with "S^k
If still YES
Flag Data
with a "+"
December, 1991
Page D-106
-------
EXHIBIT E
QUALITY ASSURANCE REQUIREMENTS
December, 1991
-------
EXHIBIT E
QUALITY ASSURANCE REQU
TABLE OF CONTENTS / /^
/ / / / PAGE NO.
SECTION 1 INTRODUCTION >x. . . / E-l
SECTION 2 QUALITY ASSURANCE PLANS "^X^ '^^V E"3
SECTION 3 STANDARD OPERATING PROCflJURES-^^.. . . . . >x/ .... E-6
SECTION 4 CHAIN-OF-CUSTODY . . \. ""^vT-T-T-^ . . 7^"~T~77 E-13
DOCUMENT CONTROL . . . . \ . \ . / ./ E-16
SECTION 6 ANALYTICAL STANDARDS REQUIREMENTS ./ E-20
SECTION 7 METHOD SPECIF^TQC REQUIREMENTS\.\ E-24
SECTION 8 REGIONAL D/
SECTION 9 LABORATORY EVALUATION/SAl
SECTION 10 ON-SITEsLABOttA^ORY/EVALUATIONS
SECTION 11 DATA MANAGI
SECTION 12
E-37
E-38
E-40
E-43
E-45
December, 1991
-------
SECTION 1
INTRODUCTION
Quality assurance (QA) and quality control (QC)
EPA's Contract Laboratory Program (CLP). The CLP QA
management review and oversight at the planning, imp
completion stages of environmental data generation
data provided are of the quality required. The C
activities required as part of data generation t
known and documented quality.
During the planning of an environmental
activities focus on defining data quality
designing a QC system to measure and doc
generated. During the implementation of
activities ensure that the QC system is f
deficiencies are identified and corrected.
generated, QA activities focus on assessing the
determine their suitability to support enforcement o
integral parts of
The purpose of this Exhibit
CLP meets the quality objectives d^efir
activities which represent the min:
the analytical requirements associated with the/d
method analytes. These operations are\desi^ne/l t
comparable data from all Contractors.
laboratory from maintaining its own QC checks
performance.
on program, QA
teria, and
data that will be
effort, QA
tively, and that
'onmental data are
data obtained to
decisions.
by which the
requires a variety of
ations necessary to satisfy
i of the different
ensure the generation of
iirements do not release the
method and instrument
Ln
Appropriate use of/da
conditions encountered
procedures and criteri
contract have been vali
laboratories participa
methods does not guajrante"
collected under actua
such as sampling artifact'
Therefore, the QC component
The
analytical
corrective /ac
include
accuracy,
activit
known and
Necessary
criteria that demons
QA review. External revl
ted under ^she ^reat range of analytical
fses r^qvures reliance on the QC
orporated into tfeesmetnods. The methods in this
ted on s^mpleT^typical~i5f those received by the
in the CpP. HoweVec/ the validation of these
y perform equally well for all samples
tions. Inaccuracies can result from causes
equipment malfunctions, and human error.
is indispensable.
|C procedures are used to estimate and evaluate
ine the necessity for or the effect of
ed for evaluating the analytical results
.ve indicators of quality such as precision,
addition, QC data give an overview of the
ed program to generate environmental data of
red to meet defined objectives.
Sf at complete QA/QC program include internal QC
eptable levels of performance, as determined by
data and procedures is accomplished by the
December, 1991
Page E-l
-------
Exhibit E
Metal Analysis of Ambient Air
monitoring activities of the National Program Office, Regi
SMO, NEIC, and EMSL/LV. Each external review accomplish
purpose. These reviews are described in specific secti
Performance evaluation samples provide an external QA
program. A laboratory on-site evaluation system is a
QA monitoring. A feedback loop provides the results
functions to the contract laboratories through dire
APOs and TPOs.
This Exhibit is not a guide to construct!}
plans, quality control systems, or a quality a?
however, an explanation of the QA requirement^
minimum standards for QA/QC programs. It
are required in a QA Plan, and the QA/QC dc
contract. Delivery of this documentation^
data package which will stand alone, and
Contractor or with an analyst, at a later
is questioned.
To ensure that the product delivered by the
requirements of the contract and to/tmpi5evfi__ inter -
the Agency requires the following £rom
• Development and implementatio
the key elements of that QA pro]
described in Section 2 of this
• Preparation of and
(SOPs) as describe
data users,
/different
if this Exhibit.
':ence for the
of the external
review
with the
• Adherence to the.
documentat ion
• Verification
of referenc
solutions obta:
• Participation_in the
s ample s .xlnclud
nee to wri
on 3 of
ect
ince organization. It is,
It outlines some
ific items that
red by this
;ency with a complete
for contact with the
aspect of the analysis
ts the
ta comparison,
ocumentation of
a written QA Plan, as
Operating Procedures
ciated QC and
contract.
Subraiss
during s
documentation of the purity
ifals and the purity and accuracy of
fvate chemical houses.
>f laboratory performance evaluation
arrective action procedures.
site\laboratory evaluations, including adherence
rondures.
and pertinent documentation for Regional
of all original documentation generated
December, 1991
Page E-2
-------
Exhibit E
Metal
Analysi
sis of Ambient Air
SECTION 2
QUALITY ASSURANCE FLANS
The Contractor shall establish a quality assui;
objective of providing sound analytical chemical m^
shall incorporate the quality control procedures,
and all documentation required during data colle^
assessment measures performed by management to
production.
As evidence of such a program, the
Quality Assurance Plan (QAP) which descri
implemented to achieve the following:
• Maintain data integrity, validity,
• Ensure that analytical measurement systems
acceptable state of stability^ and
• Detect problems through da
action procedures to ensure
.ed in an
corrective
ss is reliable.
epare a. written
that are
• Document all aspects of the me
data that are technically sound
The QAP must present
objectives, and specific
quality requirements in
each element shall be
be available during 01
the APO. Additional/in;
found in EPA and AS,
icess in order to provide
defensible.
policies, organization,
id to achieve the data
able, SOPs pertaining to
t' of the QAP. The QAP must
and upon written request by
preparation of a QAP can be
2.1 ELEMENTS OF A
The folio-
address in th<
SICE PLAN
Contractors quality program shall be
and Objectives
lei
of QC and QA responsibilities; and
December, 1991
Page E-3
-------
Exhibit E
Metal Analysis of Ambient Air
Reporting relationships.
Personnel;
Staff resumes;
Education and experience requir^
Contract; and
Training progress.
Facilities and Equipment;
Instrumentation and bacl
Maintenance activitie
Document Control;
Laboratory notebook policy;
Sample and dat
documentation
Logbook maintenance and arch:
procedures and
dures;
Case file organizati
procedures; and
.ration, and review
roval, review, revision,
•'frequency;
f
handling and storage procedures;
^extraction procedures;
Lysis procedures; and
saration procedures.
i!on procedures;
fion procedures;
December, 1991
Page E-4
-------
Exhibit E
Metal Analysis of Ambient Air
adsor
Data review procedures;
Data reporting and authorization
Data management procedures.
Quality Control Program; and
Solvent, reagent, and
Reference material analys
Internal QC checks;
Corrective action and
Procedures.
Quality Assurance Program Assessment^
Data audits;
Systems audits;
Performance audits;1
Corrective action
QA re
December, 1991
Page E-5
-------
Exhibit E
Metal Analysis of Ambient Air
SECTION 3
STANDARD OPERATING PROCEDURES
In order to obtain reliable results, adherence
methodology is imperative. In any operation that
basis, reproducibility is best accomplished through
Operating Procedures (SOPs). As defined by the
document that provides directions for the step-bv-step
operation, analysis, or action which is commonly accepted as the
performing certain routine or repetitive tasl
analytical
a repetitive
d
execution
SOPs prepared by the Contractor must
comprehensive, up-to-date, and sufficiently
results by qualified analysts. All SOPs,/as
reflect activities as they are currently pfc
addition, all SOPs must:
• Be consistent with current EPA regulations,
contract's requirements.
• Be consistent with inst:
manuals.
• Be available to the EPA during
complete set of SOPs shall be
inspection at such evaluations.
laboratory personnel,.
the SOPs.
e. , clear,
rmit duplication of
the Agency, must
laboratory. In
and the CLP
ic instruction
aboratory evaluation. A
.er and available for
-site evaluations,
trate the application of
Provide for the
complete to re
protocol.
Describe the'
by the Contract^
results.
Describ
analy
that is sufficiently
tasks required by the
monstrating the validity of data reported
the cause of missing or inconsistent
ind feedback mechanism used when
rotocol requirements.
\updated as necessary when contract,
pcedural modifications are made.
rence in usability or evidentiary
work stations as appropriate.
December, 1991
Page E-6
-------
Exhibit E
Metal Analysis of Ambient Air
• Be subject to a document control procedure which
outdated or inappropriate SOPs.
3.1 SOP SPECIFICATIONS AND FORMAT
udes the use of
on
3.1.1 An SOP is defined as a written narrati-
of laboratory operating procedures including
documentation. The SOPs must accurately de
used in the laboratory, and copies of the written SOPs shall be available
to the appropriate laboratory personnel. /The^se procedures are necessary
to ensure that analytical data produced
acceptable for use in EPA enforcement c/se/prepara
The Contractor's SOPs shall provide me;
each of the following specifications
basis for laboratory evidence audits.
3.1.2 The format for SOPs may vary dependingxupon
for which they are prepared. However, at a min:
sections must be included:
3.1.2.1 Title page.
3.1.2.2 Scope and application
3.1.2.3 Definitions.
umentation to meet
d by EPA as the
,e kind of activity
thVxfollowing
3.1.2.4
3.1.2.5
Procedures.
QC ace
3.1.2.6 Corr
secondary revi
.eluding procedures for
'rated.
3.1.2.7
3.1.2.8
3.1.2.9
3.2 REQ
3.2.
sample
procedures
Contractor:
ription and example forms.
and precautions.
lop and use adequate written SOPs to ensure
Evidentiary SOPs shall include specific
processes as they are performed by the
3.2.1.1 Sample re^sejlpt and logging
December, 1991
Page E-7
-------
Exhibit E
Metal Analysis of Ambient Air
3.2.1.1.1 The Contractor shall have written SOPs
logging in the samples. The procedures shall i]t
of the following information:
• Presence or absence of EPA chain-of-<
• Presence or absence of airbills or/
• Presence or absence of EPA Traff
lists;
• Presence or absence of custo;;
sample containers and their/
• Custody seal numbers, whe
Presence or absence of samp]
• Sample tag ID numbers;
• Condition of the
• Condition of the
receiving and
documentation
Verification of agre
receiving documents am
Resolution
The def j
upon
.greement of information on
3.2.1.1.2
responsib
his/her dl
.epancies with SMO; and
'describe sample condition
signated sample custodian
have written SOPs describing
3.2.1.2
3.2
sample
definitions
have written SOPs for maintaining
.roughout the laboratory.
assigns unique laboratory identifiers,
ade a description of the method used to
tory identifier and cross-reference to the
sntiractor uses prefixes or suffixes in addition to
numbers, the written SOPs shall include their
December, 1991
Page E-8
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Exhibit E
Metal Analysis of Ambient Air
3.2.1.3 Sample security
The Contractor shall have written SOPs fo
security of samples after log-in and shall demi
sample storage and laboratory areas. The SOP,
include descriptions of all storage areas fo
laboratory, and steps taken to prevent samp
shall include a list of authorized perso:
storage areas.
3.2.1.4 Internal chain-of-custody o
The Contractor shall have wril
consisting of sample identificatiot
receiving procedures, and sample trafc
information concerning the chain-of-cust
this Exhibit.
3.2.1.5 Internal tracking
3.2.1.5.1 The Contracto
work performed on any par
include the following:
itenance of the
of the
sically
A description of the
receipt, sample storage)v
tion used to record sample
transfers, sample
es;
ta.
chain-of-custody
procedures, sample
For more
dures see Section 4 of
for tracking the
ing SOP shall
3.2.1.6
3.2.2
used to record instrument
ities; and
and laboratory
)le receipt, sample storage,
Eer/ and sample analyses.
and information control
The jConfcractor shall develop and use adequeate written SOPs to ensure
that a4lydata generatedNforNthe CLP are of known, documented, and
acceptable quality. Analytical SOPs shall include specific procedures
for/theCfollowing processes s\s they are performed by the Contractor:
Contractor ^hall have written SOPs for preventing sample
pn, our ing/sample preparation, cleaning of glassware,
December, 1991
Page E-9
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Exhibit E
Metal Analysis of Ambient Air
3.2.2.2 The Contractor shall have SOPs to ensure
standards used in sample analysis QA/QC.
3.2.3 Quality Management SOPs
3.2.3.1 The Contractor shall have written
managerial review of laboratory operation and/
laboratory data review/laboratory self inspe/
procedures shall include but not be limited^^/documenting
information:
3.2.3.1.1 Data flow and chain-of-
3.2.3.1.2 Procedures for measuri
3.2.3.1.3 Evaluation of paramet
errors.
eability of
3.2.3.1.4 Procedures to assure that hardc
complete and compliant with the requirements
3.2.3.1.5 Demons tration
(demonstrated by supervis1
internal PE samples, etc.)^
ction
3.2.3.1.6 Frequency and type df i:
quarterly, spot checks, perceived
3.2.3.1.7 Demo:
and resumption
internal audi
3.2.3.1.8 D,
response,
Arables are
t B.
procedure
lotebooks,
doc
3.2.3.2 The
assembly of all
and manageria]^_review.
basis. Th€~"procecItiZfis mus
pages
audi ts (e.g., random,
le areas).
denazification-corrective actions
Sequence resulting from
s, (internal and external),
11 have written SOPs for organization and
ating to each EPA Case, including technical
shall be filed on a Case-specific
that all documents including logbook
omatographic charts, computer
3.2.3.3
management
include but
ecords
ies, correspondence, and any other written
inceVto the Case are compiled in one location for
ysrem must include a document numbering and
mare information concerning document control
ee Section 5 of this Exhibit.
r £hall have written SOPs for sample analysis,
g,/and reporting of data. The procedures shall
to documenting the following information:
December, 1991
Page E-10
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Exhibit E
Metal
AnalYsi
•sis of Ambient Air
3.2.3.3.1 Procedures for controlling and est
errors.
3.2.3.3.2 Procedures for reviewing changes
and ensuring traceability of updates.
3.2.3.3.3 Life cycle management proce
and implementing changes to existing c
hardware, software, and documentation
3.2.3.3.4 Database security, bac
including recovery from system fa:
3.2.3.3.5 System maintenance pr
3.2.3.3.6 Individual(s) responsible
maintenance, data integrity and security^
installing new systc
procedures
3.2.3.3.7 Specifications
3.2.3.4 The Contractor stia.ll
3.3 HANDLING OF CONFIDENTIAL INFO]
staff training
written
dure
x7
laboratory safety.
3.3.1 A Contractor conducting work
designated confidential information
information must be hand£etihsReparately
under this contract. /To accomplish this ,NN
the handling of confidejrt6Ial\inrV)rmation
3.3.2 All confidential docv
designated Document/Control
is contract may receive EPA-
Agency. Confidential
ther documentation developed
.the\following procedures for
en established.
jr the supervision of a
3.3.3 Any samples or^info£ma£ion received with a request of
confidentiality sh£il be nandled as "confidential." A separate locked
file shall be maintained to V&ore this information and shall be
segregated fjpoa-ather non&onfideht^al information. Data generated from
confidential samplessball be^treate)d as confidential. Upon receipt of
gs these documents into a
The information is then made available to
after it has been signed out to that person
documents^ shkll be returned to the locked file at the
working] day. Confidential information may not be
upon apjjro-^l by the EPA Contracting Officer. The DCO
.e document control system. In addition,
ion may noy. be/disposed of except upon approval by the EPA
Confi
autho:
by
C1
rep
will eft
this infoj
Contracting 6f£ieer?Vv<3hey^CO shall remove and retain the cover page of
any confidential information disposed of for one year and shall keep a
record of the disposition in the Confidential Inventory Log.
December, 1991
Page E-ll
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Exhibit E
Metal Analysis of Ambient Air
3.4 SOPS DELIVERY REQUIREMENTS
Within forty-five (45) days of contract receipt, a comniete set of SOPs
relevant to this contract shall be sent to the TPO, SHO/an^ EMSL/LV. Also,
during the term of performance of the contract, copies'of SOBs which have been
amended or new SOPs which have been written shall be/sen€x° thVx^PO, EMSL/LV
(quality assurance SOPs) and NEIC (evidentiary SOPs!
December, 1991
Page E-12
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Exhibit E
Metal Analysis of Ambient Air
from the
ffort is
lowing
labora
ession of the
od for maintaining
laboratory.
iner shall be labeled
.tifier. If a
;eferenced to the
SECTION 4
CHAIN-OF-CUSTODY
A sample is physical evidence collected from a
environment. An essential part of hazardous waste
that the evidence gathered be controlled. To accoi
sample identification, chain-of-custody, sample r
procedures have been established.
4.1 SAMPLE IDENTIFICATION
4.1.1 To ensure traceability of sampl
Contractor, the Contractor shall have
identification and tracking of sampl
4.1.2 Each air sample and sample prepar
with the EPA sample number or a unique
unique laboratory identifier is used, it shall
EPA sample number.
4.2 CHAIN-OF-CUSTODY PROCEDURES
4.2.1 Because of the nature of^che>data b4ing collected, the custody of
EPA samples must be traceable from\the\time tme samples are collected
\ X / / *
until the associated data are introduceovas/evidence in legal
proceedings. The Contractor shall turoe procedures ensuring that EPA
sample and data custod^-are-naintained\nd alocumented. A sample is under
custody if the followi
.n your possession, or
and you locked it up, or
secure area (secure areas shall be
1 only).
4.3
/ / \ \
signate a sample custodian responsible for
4.2.1.4
accessible
4.37
samples
4.3.3 The
inspected upon reel
signate a representative to receive
ample custodian is not available.
shipping containers and canisters shall be
the sample custodian or his/her representative.
December, 1991
Page E-13
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Exhibit E
Metal Analysis of Ambient Air
4.3.4 The condition of the custody seals (intact/r
inspected upon receipt by the sample custodian or hj
4.3.5 The sample custodian or his/her represent
the presence or absence of the following documei;
sample shipment:
tact) shall be
r representative.
check for
the
4.3.5.1
4.3.5.2
4.3.5.3
4.3.5.4
4.3.5.5
Airbills or airbill stickers.
Custody seals.
EPA custody records.
EPA traffic reports or
Sample tags.
4.3.6 The. sample custodian or his/her
date all forms (e.g., custody records, traffic
and airbills) accompanying they
4.3.7 The Contractor shall co;
problems such as absent document
custody seals, and unsatisfactory
bottle).
11 sign and
tacking lists,
e receipt.
repancies and
ion, broken
tion (e.g., leaking sample
4.3.8 The Contractor
problems on Telep
4.3.9 The follo<
AADC-1 by the s
received and ins;
4.3.9.1
4.3.9.2
shipping
.ution of discrepancies and
rded on appropriate Form
resentative as samples are
Lpping container.
and condition of custody seals on
•present.
ysample canisters.
:e of airbills or airbill stickers.
Ll sticker numbers.
/sence of EPA custody records.
December, 1991
Page E-14
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Exhibit E
Metal Analysis of Ambient Air
4.3.9.8
lists.
Presence or absence of EFA traffic report
SAS packing
4.3.9.9 Presence or absence of sample tags.
4.3.9.10 Sample tag identification numbers c
sample numbers.
4.3.9.11 Verification of agreement or n
recorded on shipping documents and sample
4.3.9.12 Problems or discrepancies.
4.4 SAMPLE TRACKING PROCEDURES
The Contractor shall maintain recor
handling from receipt to final analysis.
documentation of the movement of samples and
out of designated laboratory storage areas.
to the EPA
all phases of sample
shall include
^samples into and
December, 1991
Page E-15
-------
Exhibit E
Metal Analysis of Ambient Air
SECTION 5
DOCUMENT CONTROL
The goal of the laboratory document control prpgramvis to assure that
all documents for a specified SDG are accountable upon/completion ofxtlie
project. Accountable documents used by contract laboratories shkil include
but not be limited to logbooks, chain-of-custody
bench sheets, and other documents relating to tl
.The following document control procedures have
all laboratory records are assembled and stored
available upon request from the EPA prior to/
5.1 PREPRINTED LABORATORY FORMS AND LOG!
prds, sample worfc^sheets,
mple or sample analysers'.
established to assure that
>r deliygisy to the EPA or are
delivery schedule.
5.1.1 All documents produced by the Contactor wi(ich are directly
related to the preparation and analysis of EPAx^ampIfes shall become the
property of the EPA and shall be placed in the cotBpletes&le delivery
group file (CSF). All observations and results recorded bV the
laboratory but not on preprint^alaBSrafeoog^fprms shall^fee entered into
permanent laboratory logbooks,\ Wh«n_^ll data^rTToTB^an^SDG are compiled,
all original laboratory forms atal coj>ies"Trf--all_J>DG- related logbook
entries shall be included in thextocumentatioi
5.1.2 The Contractor shall identif
laboratory documents which is directlj
analysis of EPA samples^
5.1.3 Pre-printed
laboratory and be dkte,
responsible for
performed.
in the name of the
jned by the person
e time an activity is
t
ivity recorded on all
:ed to the preparation and
5.1.4
person responsible
performed.
dated (month/day/year) and signed by the
ing the activity at the time an activity is
5.1.5 Logbook entrifessshalfsbe in^fchronological order. Entries in
logbooks/wrph—the-^xcepbion of £nsjmnnent run logs and extraction logs,
shall include only ones^DG^er page.
unbound logbooks shall be sequentially
5.1.7 ^Instrument run lo^s shall be maintained so as to enable a
reconstrucfckm of^the run sequence of individual instruments. Because
the laboratory^ajust provide copies of the instrument run logs to the EPA,
the laboratory ma^exercise the option of using only laboratory or EPA
sample identifications-numbers in the logs for sample ID rather than
December, 1991
Page E-16
-------
Exhibit E
Metal Analysis of Ambient Air
government agency or commercial client names to prese
confidentiality of commercial clients.
5.1.8 Corrections to supporting documents and raW data shall be made by
drawing a single line through the error and entering the^Qorrect
information. Corrections and additions to supportin^documeixts and raw
data shall be dated and initialed. No informatior/shall>be obliterated
or rendered unreadable. All notations shall fee recorded insink. onused
portions of documents shall be "crossed"
5.2 CONSISTENCY OF DOCUMENTATION
5.2.1 The Contractor shall assign a
responsible for the organization and
5.2.2 All copies of laboratory doc
5.2.3 Original documents what include info
one SDG shall be filled in the CSF of the lowest:
shall be placed in the other CSF(s) and the
following information on the c/pyts")—ia-cgd ink:
"COPY"
5 . 3
Contrac
DOCUMENT
5.3.1 In order to p
analysis
serialize
complete and legible.
lating to more than
The copy(s)
1 record the
"ORIGINAL IS FILED IN CSF
The Contractor shall sign and date thN
5.2.4 Before releasing analytical
shall assemble and oros^cfteck t|he
records, laboratory bench sheiftsl<^pe1
relevant data to erasure that aata pertait
sample delivery group is con/is^entoitouf
ition to the copy(s).
e document control officer
sample tags, custody
instrument logs, and other
to each particular sample or
>ut the CSF.
pre
analys
inventorie
ument accountability of the completed
in asCSF shall be inventoried and assigned a
in Efcjiibit B, Section 2.
£zed number (For example: 75-2-0240).
:- to each SDG, including logbook pages,
.romatograms, screening records, re-
is records, records of failed or attempted
brary research results, etc., shall be
December, 1991
Page E-17
-------
Exhibit E
Metal Analysis of Ambient Air
5.3.3 The DCO shall be responsible for ensuring
generated are placed in the CSF for inventory and
EPA. The DCO shall place the sample tags in plas
Figure E-l is an example of a document inventory
documents
livered to the
the file.
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
etc.
0001
0002
0003
0004
0005
0006
0007
0008
*This number is to be re
Case File Document I
Chain-of-Custody Records
Shipping Manifests
Sample Tags
SMO Inor{
Inorganic
Analysts' I
ICP, ICP-MS
etc.
on each
5.4 STORAGE OF EPA
The Contract<
location.
5.5 SHIPPING DATA
5.5.1 The
the recipi
placed s
seal.
the me
5.5.
EPA
5.5.3 A
and SMO.
tory documents in a secure
it shipment of deliverables packages to
re custody seals on'the containers
without damaging or breaking the
cument what was sent, to whom, the date, and
ge the CSF deliverable to the appropriate
eport submission.
•Lttal letter for the CSF will be sent to NEIC
December, 1991
Page E-18
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Exhibit E
Metal Analysis of Ambient Air
5.5.4 The Document Control Form is used to document/
inspection of shipping containers and samples. The
one (1) original FORM AADC-1 for each shipping conta
5.5.5 The Contractor shall sign and date the
examine the shipping containers, and record the
custody seals and their conditions.
5.5.6 The Contractor shall note any proble
the instructions explained in Exhibit B, Si
5.5.7 The Contractor shall submit a coq
each SDG package.
receipt and
ctor shall submit
of
ow
t Control Form with
December, 1991
Page E-19
-------
Exhibit E
Mecal Analysis of Ambient Air
SECTION 6
ANALYTICAL STANDARDS REQUIREMENT?
The U.S. Environmental Protection Agency will not y^Jpjjly analytical
reference standards either for direct analytical meafsurementi^xjr forxthe
purpose of traceability. All Contractors will be acquired to prepare
reference standards from traceable National InstiJfb«r of Standards at
Technology Standard Reference Materials or NIST/EPA/approved certified"
reference material. If the NIST/EPA reference >fetajf{dards are not available"
the Contractor can purchase them from private/chejaical supply houses or
venders, those standards necessary to successfully and accurately perform the
analyses required in this protocol.
6.1 PREPARATION OF CHEMICAL STANDARDS FROKTHE
CTY BULK MATERIAL
6.1.1 A Contractor may prepare its chemicar^s^andatds from high purtiy
materials. Contractor laboratories should obtainthe highest purity
possible when purchasing chemical standards; standardsxmirch^sed at less
than 97H purity must be document^oT~a2~~t»-^whv^a higher purity could not be
obtained.
6.1.2 Proper storage of chemical
safeguard them from decomposition.
indarc
fcal in order to
6.1.3 The weight of material to be weighed out for a specified volume
should be calculated by taking^into account tbe purity of the analyte and
the desired concentration. Thei&alculatioiv. should be verify by a second
person for accuracy.
balance to the nearest (V.I mg
weights and verified by a seco
solute should be compatible
be used; the solute should
solvent. In theSsase
not react with each oQier.
should be\
person.
« prsi^pcoJ
soluble, ste
performed on an analytical
adardized using standard
solvent used to dissolve the
in which the standard is to
and nonreactive with the
Ltl'-component solution, the components must
6.1.4
Transfe
soluteoco a>wolumetric flask and dilute to the
specified solution volume with^s^lvenTs after ensuring dissolution of the
solute in luie solvent^ SohicationNxir/warming may be performed to promote
dissolution tfz the solutse. ibis solution is to be called the primary
standard'an/1 all subsequent dilutions must be traceable back to the primary
standard.
6.1.5X. Log^-notebooks are tfo hfe kept for all weighing and dilutions. All
subsequeitesdilubions from tme .primary standard and the calculations for
determining cbeircttncentirations are to be recorded and verified by a
second person. ^k\l solution; standards are to be refrigerated when not in
use. All solutions
-------
Exhibit E
Metal Analysis of Ambient Air
of the compound or compounds, concentration, date prep
initials of the preparer.
6.2 PURCHASE OF CHEMICAL STANDARDS IN SOLUTION
Solutions of analytical reference standards
Contractors provided they meet the following crite
6.2.1 Contractor laboratories must maintaii
to verify the integrity of the standard solut
6.2.1.1 Purity confirmation of the /tanaard
6.2.1.2 Chromatographic and quantatalfive docv
solution standard was QC checked acoordrag to tlae
solvent, and
ition that the
>llowing:
6.2.1.2.1 The Contractor must purchase standards for which the
quality is demonstrated statistically ano^analycically by a method of
the supplier's choice. One way this can be demonstr-ated is to
prepare and analyze three solutions; a. high standard,^ low standard,
and a standard at the targercoTteefttration (see beltiwy. The
Contractor must then demonstrate that the~~aTialvtical results for the
high standard and low stani
theoretical concentrations. \his\ is
part 6.2.1.2.2 which follows.
must then demonstrate that the cfcmcet
lies midway between the concentrations
This is done by the
to be within 10 percent o
6.2.1.2.2
document that
targe
le/followine have be«
with ^he difference in
t-test in
'achieved, the Contractor
:ion of the target standard
)f the low and high standards.
the standard is certified
ventration.
>
is\j4sed, the supplier must
achieved:
of idc
om
Two soluo
indepenoently
solution muse be
"target standard^)
and diluted
tim thev--§e/cond solution and diluted to a
ent less that the target standard. This is
rd";
of each standard (a total of 18 analyses)
e following sequence: low standard, target
low standard, target standard, high
December, 1991
Page E-21
-------
Exhibit E
Metal Analysis of Ambient Air
The mean and variance of the six results for
calculated using the following equations:
solution must be
Variance
Mean
'12
Yt + Ys
+ na
y» * ysa
Eq. E-l
The values Ylt Y2, Y3
analyses of each standard. Ttv
standards are designated M1(
variances of the low, target,
vi> vz« and V3, respectively.
Vp, is calculated using the following
Vk
If the square root of Vp
/10.000 is to be used as the^
calculations.
The test sta
If the tes
demonstrate a
In s
of the six
, target, and high
Actively. The
.rds are designated
pooled variance,
Eq. E-3
one percent of M2, then M22
Vp in all subsequent
the following equation:
Eq. E-4
exceeds 2.13 then the supplier has failed to
rcent difference between the high and low
the standards are not acceptable.
Iculated using the following
Eq. E-5
If theXest
demons trabs^that
exceeds 2.13, the supplier has failed to
target standard concentration is midway
December, 1991
Page E-22
-------
Exhibit E
Metal Analysis of Ambient Air
between the high and low standards. In such
are not acceptable.
The 95 percent confidence intervals for tto
standard must be calculated using the fol
INTERVAL FOR LOW STANDARD
INTERVAL FOR TARGET STANDARD =
INTERVAL FOR HIGH STt
E-7
Eq. E-8
These intervals must not overlap. If^eyerla^Kis observed, then
the supplier has failed to demonstrate th^abirtty to discriminate
the 10 percent difference in concentrations/X^n si^h a case, the
standards are not accep/table"1:—In^any event, theXkaboratory is
responsible for the qu^lit^of^thestSnttaEd&^gmployed for analyses
under this contract.
6.3 REQUESTING STANDARDS FROM THE EPl
Solutions of analytical reference
EPA Chemical Standards Reposife*^. depending, on"*
can place an order for standards on^y after
are not available from cfnmne^rcT&k vendors in
6.4 DOCUMENTATION OF/
VERIFIC
'REPOSITORY
can be ordered from the U.S.
availability. The Contractor
grating that these standards
an.
OF CHEMICAL STANDARDS
It is the Contractor' s responsibility Bo^maintain the necessary
documentation to showxthafcx£heycheaiical standards they have used in the
performance of CLP analysis coniform to the requirements previously listed.
Weighing logbooks, calculabions, chromatograms, mass spectra, whether produced
by the Contractorgz-purchase^from chemical supply houses, must be maintained
by the Contractor and may^be subject toOoeview during on-site inspection
visits. DocumentatroTV~o_f standards preparation may be required to be sent to
EPA for verification of contract compliance. In those cases where the
documentation a.s supportive 6f the analytical results of data packages sent to
EPA, such/documentation is to l^e ^ept on file by the Contractors for a period
of one
December, 1991
Page E-23
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Exhibit E
Metal Analysis of Ambient Air
SECTION 7
METHOD SPECIFIC QC REQUIREMENTS
rations that
in
The purpose of this section is to outline the
are an integral part of the analytical requirements/
determination of target analytes listed in Exhibit*
Exhibit D, Section 3 for metals collected on
inductively coupled plasma (ICP) spectrometry, inductively coupled
spectrometry (ICP-MS), and graphite furnace atomic/absorption (GFAA)
spectrometry. This section is not intended a/ a/eompreheftsdve quality control
document, rather as a guide to the specific QC roeratiotfs that must be
considered for inorganic analyses. At a m}
to address these operations in preparing
this Exhibit, and the SOPs discussed in SeJ
7.1 These operations include the following:
Instrument Calibration;
atory is expected
in Section 2 of
Initial Calibration Verific
Verification (CCV);
CRQL Standards;
• Linear Range Standard (LRS)
Initial Calibration/Blank
Preparation Blank/PB
• ICP and ICP-MS
• Spike Sample
• Duplicate Sample
• Laboratory Cjmfral
Calibration
erial Dilution Analv
dxQuantitation Limit
nal Standards K
alibration Blank (CCB), and
)
CS) Analyses;
lyses;
Analyses;
)L) Determination; and
pfc ICP and ICP-MS;
iP-MS; and
December, 1991
Page E-24
-------
Exhibit E
Metal Analysis of Ambient Air
Furnace AA QC Analyses (Method of Standard Additions/.
7.1.1 Ins trument Galibrat ion
7.1.1.1 Guidelines for instrument calibration
D, Inorganics, Section 3.7.1 for ICP, Section
Section 5.6.1 for GFAA. Each instrument shal
once every 24 hours and each time the inst
7.1.1.2 The calibration standards shall
of matrix and at the same concentration
following the procedures outlined in Exrfib
Section 4.6 for ICP-MS, and Section 5.
:ype
!ie preparation blank,
D, Sec>cion 3.6 for ICP,
GFAA.
7.1.2
Initial Calibration Verificat:
IC.V)
7.1.2.1 Immediately after each of the ^T€P. ICP-1&, and GFAA systems
have been calibrated, the accuracy of the ihitial^alibration shall be
verified and documented for each analyte by the^-analys-is of EPA ICV
solution(s). When resulting measurements exceed theconfcrol limits in
Exhibit D, Section 3, Table n/Tl^3-r-the^analysis shallSbyfe terminated,
the problem corrected, the instrument recaTlbrate4Jl__and the calibration
reverified. For ICP, ICP-MS XandCGFSrrH&e ICV shall>e run and
reported at each wavelength
7.1.2.2 If the ICVs are not avail*
of an analyte is not available fronT
conducted on an
used for regular
range. An indepe
analytes from a d
the instrument c
indepe:
7.1.3
Conti
7.1.3.1 To ensi
required in Exhibit^
and Section 5.6.3 for
either prepared
mass useft foj
analyticaVsample.
or
the
EPA, or a certified solution
analyses shall be
oncentration other than that
within the calibration
standard composed of the
ed in the standards for
(CCV)
accuracy during each analysis run as
3.713 for ICP, Section 4.7.3 for ICP-MS,
shall analyze a CCV solution,
:-prepared, for every wavelength or
Ing of the run and after the last
7.1./3.2/ Each CCV analyzed s^hall reflect the conditions of analysis of
all/associated analytical] samples (the preceding 10 analytical samples
pt€iceding analytical samples up to the previous CCV). The
durat3*m of^analysis, rinse^, and other related operations that may
affect thB^CCV mftasured/re/ult may not apply to the CCV to a greater
extent thanche exfctont? applied to the associated analytical samples.
December, 1991
Page E-25
-------
Exhibit E
Metal Ai
.nalys:
sis of Ambient Air
7.1.3.3 If the deviation of the CCV is greater than ttfe control limits
specified in Exhibit D, Section 3, Table D/IN-3, tzne Analysis shall be
terminated, the problem corrected, and the CCV reanalyzed only once. If
the reanalysis yields a CCV value within centre/ limitsV^then the
preceding 10 analytical samples or all analytical/saTHDles^aoalyzed since
the last acceptable calibration verification /shaYL be ahalyzeEKfor the
analytes affected. Otherwise the instrumencCsh/ll be recalibrate^ the
calibration verified, and the affected
ana}
7.1.4
CRQL Standards
for 1C!
7.1.4.1 To verify linearity near the
analysis, the 'Contractor shall analy:
two times the CRQL or two times the
standard shall be analyzed at the be
analysis run or a minimum of twice per
whichever is more frequent, but not before
D, Section 3.7.4 for ICP, Section 4.7.4 for 1C
'CRQL sty
liche
t hoi
P-MS, and AA
(CRI and CRA) at
•er/is greater. The CRQL
d of each sample
working shift,
ijitlined in Exhibit
6.4 for AA.
This standard must be run for every wavelength or Iftass used for
analysis, except those for A3/TBa7"^eat-r--Ee_, MR, Na, andN/for ICP.
7.1.4.2 Results for the anal}
15 percent of the true value fo*
not, the analysis shall be termii
analytical samples since the last
7.1.5 Linear Range Standard Analysis
7.1.5.1 For all
check standard (L^S)/shall
three calendar montps) for e/ach
Exhibit D, Sectfion/3.7.5
standard must/be orn for
naly
.QL standard" must be within ±
way/e^e/ngl:hT~Tls«d for analysis. If
roblem corrected, and the
e CRI or CRA reanalyzed.
:erly)
ses,\a Mnear range verification
and\g^ported quarterly (every
FORM III-AAIN as outlined in
>ectibn 4.7.5 for ICP-MS. This
wavelengtn or mass used for analysis.
7.1.5.2 Results^for th¥ analysis of the LRS must be within ± 5 percent
of the true value foixeach wavelength or mass used for analysis. If
not, the anjj^tsismust Dfesterminated and successive dilutions of the
standard/must be re^ttjalyzedsuntii>the control limits are met. The
concentzratj^n^crf-^his fftandard^tshyt meets the control limits is the
upper/1 imd/t of the rHstrvbnent linear range beyond which results cannot
be repop:ed under this^concract without dilution of the analytical
sample/
il and Conti
Calibration Blanks Analyses
7.1.6.1 ~v&^alibxation/blank must be analyzed at each wavelength or mass
used for analysis iimnediately after every initial and continuing
calibration veri&tcatiqji, at a frequency of 10 -percent of every two
December, 1991
Page E-26
-------
Exhibit E
Metal Analysis of Ambient Air
hours during the run, whichever is more frequent, as/outlined in Exhibit
D, Sections 3.7.6 and 3.7.7 for ICP, Sections 4.7.6/an/4.7.7 for ICP-
MS, and Sections 5.6.5 and 5.6.6 for GFAA. The blank/must be analyzed
at the beginning of the run and after the last analytical sample.
7.1.6.2 If the absolute value of the blank result
CRQL
(Exhibit C), analysis must be terminated, th
continuing calibration blank (CCB) reanalyz
a CCB with an absolute value below the CRQ!
analyzed since the last acceptable calibr
Otherwise, the instrument must be recall
verified, and the affected analytical
7.1.6.3 Each analytical sample must
CCBs that have been analyzed within
than 10 analytical samples run betwe
each analyte in these two CCBs must
7.1.7 Preparation Blank (PB) Analysis
7.1.7.1 At least one PB (or
processed through each sampl^
prepared and analyzed with evfe
digested, (whichever is more
Section 3.7.8 for ICP, Section 4"
GFAA.
rect
prcfblem cs
If the
1 analytical samles
blank must be re
d, the calibration
and the
ed.
two consecutive
;h other with no more
e absolute value for
e CRQL.
consisting^xaf reagent water
ij; procedure must be
of samples
Exhibit D,
MS, and Section 5.6.7 for
7.1.7.2 The first ba
one, the second bat
contain the result
in that SDG.
7.1.7.3 The
to ascertain
following man;
DG shall to be assigned to PB
vetc. Each package must
ociated with the samples
SDG and used in all analyses
reflect contamination in the
7.1.7.3.1
less than
result
negative CRQL,
value of the concentration of the PB is
(Exhibit C), no correction of sample
concentration in the PB is above the CRQL,
taining less than ten times the blank
ested and reanalyzed for that analyte.
re not to be corrected for the blank
concentration in the PB is below the
Les with reported analyte values below ten
December, 1991
Page E-27
-------
Exhibit E
Metal Analysis of Ambient Air
times CRQL and associated with the blank must be/redigested and
reanalyzed.
7.1.7.3.4 The values for the PB must be recorded li
7.1.8 ICP and ICP-MS Interference Check Samp]
7.1.8.1 To verify interelement and backgrduh^correction fac£c
Contractor must analyze and report the re/ultts for an ICP and
Interference Check Sample (ICS). The ICS im/st be analyzed at the
beginning and end of each analysis run jor A minimunf^af twice per eight
hour working shift, whichever is more/frequent, b/t itt>t before the ICV
(see Exhibit D, Section 3.7.9 for ICP^and Sectiofi 4/7.9 for ICP-MS).
The ICP and ICP-MS ICS must be obtained<£rom EEA (^MSL-LV), if
available, and analyzed according to'ttje ins-tyucl^Lons supplied with the
ICS.
7.1.8.2 The ICS consists of Solutions A and AJT^hat
analytes and potential interferents. An ICS analyS
analyzing the solution for a^il wavSlenRttis or masses
analyte reported by ICP.
7.1.9
t contain both
consists of
d for each
7.1.8.3 Results for the ICP
analytical runs must be within
analytes included in the ICS. If
the problem, recalibrate the inst
samples analyzed since--ti«-4.ast
analytes contained
supplied with
determined by in
repetitively fo
be made during
supplied EPA
result of thi
value for the li
exhausted).
and AB during the
of the true value for the
nate the analysis, correct
reanalyze the analytical
ICS. If true values for
ICP and ICP-MS are not
for each analyte must be
least five times
This mean determination must
results for the previously
'cations. Additionally, the
termination is to be used as the true
t solution (i.e., until the solution is
7.1.9
abou;
met]
Exhib
Section
analysis is designed to provide information
le matrix on the digestion and measurement
dded before the sample preparation (i.e.,
|on). At least one spike sample analysis
oup of samples for each SDG, according to
or ICP, Section 4.7.10 for ICP-MS, and
Exhibit D, Table D/IN-3.
December, 1991
Page E-28
-------
Exhibit E
Metal Analysis of Ambient Air
7.1.9.2 If the spike analysis is performed on the
chosen for the duplicate sample analysis, spike ca
performed using the results of the sample designa
sample" (see Duplicate Sample Analysis). The avi
results cannot be used for the purpose of dete
Samples identified as field blanks cannot be
analysis.
7.1.9.3 If two analytical methods are uset
values for the same analyte within an SDG,
each method used.
?sample that is
itions must be
the "original
of the duplicate
^rcent recovery.
>ike sample
Lke samples must
Lm^ts of 75-125
iociated with that
nethod must be
/entration is more than
7.1.9.4 If the spike recovery is not ;^itb/in the
percent, the data for all of the samples/receive^
spike sample and determined by the
flagged with the letter "N", unles the. samp~K 7~-Section 3.7.11 for ICP,
Section 4.7.11 for ICP-MS, anb\ S^tioiT-5^6,, 9 for GFAA? Duplicates
cannot be averaged in reporting\resuits.
7.1.10.2 Samples identified as fie\d Blanks' cannot be used for duplicate
sample analysis. EPA may require tttat a specific sample be used for
duplicate sample analvsis^^If two analytical methods are used to obtain
the reported values/for the siame elemen\foka SDG (e.g., ICP and GFAA),
duplicate samples must/ttr^cun b^y each mett)od\ised.
7.1.11 Laboratory,
7.1.11.1 The
analyte using
procedures emplo
D, Section 3.7.12
for GFAA.
7.1.11.3
established
corrected, and
S) must be analyzed for each
preparation, analytical methods and QA/QC
samples received, as outlined in Exhibit
4.7.12 for ICP-MS, and Section 5.6.10
LCS mu^5/be prepared and analyzed using each
£0 the samples received. If the EPA LCS is
ty assurance check samples or other
ed. One LCS must be prepared and analyzed
a SDG or for each batch of samples
requent.
the LCS are not within the control limits
alyses must be terminated, the problem
s associated with the LCS prepared again and
December, 1991
Page E-29
-------
Exhibit E
Metal Analysis of Ambient Air
reanalyzed. A control limit of ± 20 percent of the;
used if no control limits are provided with the
7.1.12 Performance Evaluation Sample (FES)
7.1.12.1 The Performance Evaluation Sample (P.
in monitoring Contractor performance. The Igbo
informed in advance of the analytes in the
value must be
ution.
Agency
and report the results of
jibit D, Section 3.
d in the sample
e the PES using
7.1.12.2 The Contractor must prepare,
one PES per each SDG, if available, as
7.1.12.3 Prepare the PES using the p
preparation section of Exhibit D, S
the methods described in Exhibit D
samples. All contract required QC must
7.1.12.4 The Contractor must demonstrate acceptable p^cformance for
analyte identification and quantification. If the^ContraJetor achieves a
score of less than 75 percent^~tKe~T&genevmay take bub^i/ not limited to
the following actions: Show<^ausje^a^/orC^ir^--Ke4^ce, reduction of the
number of samples shipped to che \aborate^, suspension of sample
shipment, a. site visit, a full «lata\audit/ aj
-------
Exhibit E
Metal Analysis of Ambient Air
Llution must be
Indicated in
7.1.13.4 The values for the initial sample and seri*
recorded on FORM XI-AAIN for all analysis systems,/as
Exhibit B, Section 3.
7.1.14 Method Quant it at ion Limit Determination
7.1.14.1 The Method Quantitation Limit (MQL) Ain/pg/L)"
determined for each instrument used, within ^0 /days prior "bo. the"xsfart
of any contract analysis and at least quarterly (every 3 calendar
months), as outlined in Exhibit D, Sectiojl 3/7.14 for ICP, Sectiot
4.7.15 for ICP-MS, and Section 5.6.13 fo/GFAA. The MQL must be equal
to or less than CRQLs (0g/L) specified /in Exhibit
7.1.14.2 The MQLs must be determined/by i6ultiply/ng/t>y three the average
of the standard deviations obtained/on three noncoiPisecutive days (each
analyte in reagent water) at a conceh^raticJia^JinreiB times the MQL, with
seven consecutive measurements. Each me^uremen^ must be performed as
though it were a separate analytical sampleXi-e.T^each measurement must
be followed by a rinse and/or any other procedure normally performed
between the analysis of separate samples). MQLs mint be/determined and
reported for each wave length /orma"Ss—used in the analysis of the
samples.
7.1.14.3 The quarterly determined MQL for/ai
used as the MQL for that inst
instrument is adjusted in any way
that instrument must be redetermine
as the established MQL--€o*
-------
Exhibit E
Metal Analysis of Ambient Air
7.1.15.2 The correction factors must be determined lender the same
instrument conditions used for sample analysis. Ir fae instrument was
adjusted in any way that may affect the ICP and ICP-l^S interelement
correction factors, the factors must be redetermined ahcl the results
submitted for use. The interelement factors dexerzfirnationNijust be
reported for all ICP and 1CP-MS analytes, for/each insCtumenc%ised to
generate data in the SDG.
7.1.16 Internal Standard for ICP-MS
7.1.16.1 The internal standard analyses/is
presence of physical interferences and/coi
performed by ICP-MS.
lerformadxto check for the
•ect for/thjcm for analyses
7.1.16.2 A minimum of three internal>s^andatd^/ lifted in Table D/IN-7,
Exhibit D, bracketing the mass range mushxbe used^ The intensity level
of an internal standard for each sample, dui>i4xjate>vspike analysis, and
PES must agree within ± 50 percent of the intenS-ity level of the
internal standard of the initial calibration blank^s^anda^d solution
(SO). If not, the sample
fold (1:4) dilution. If the(intensity leve
remains greater than 50 percent, \jpnyl
suspected, and the data on FORMXXV^AIN
The analytes affected by the interference
section on the appropriate FORMs I
AAIN.
ed after performing a five
£_difference, %T>,
interference must be
with an "E."
t be listed in the comment
-AAIN, VII-AAIN, and VIII-
level
thi-
7.1.16.3 The intensify
CCB solutions must
the internal standard of the\ i:
(SO). If not
and the CCV/CCB/rej
CCV/CCB ZD va
samples or al
calibration veriflc^ati
Otherwise, the inst
and the aff.ec
of the in
ilysis
ilyzed
± 20 percent
st be tei
Lthin control limits
standards for the CCV and
the intensity level of
.on blank standard solution
jiated, the problem corrected
first reanalysis yields a
ten the preceding 10 analytical
les analyzed since the last compliant
be reanalyzed for the analytes affected.
.t be recalibrated, the calibration verified
.es rerun in the context of a new run.
onc
7.1.
must be
in Exhibit
jevel of^hy^ internal standards for the ICV and
ithin ± 20 percent of the intensity level of
initial calibration blank standard solution
t be terminated, the problem corrected,
be started.
Internal Standard Percent Difference (ZD)
CP-MS analysis on FORM XV-AAIN as indicated
December, 1991
Page E-32
-------
Exhibit E
Metal Analysis of Ambient Air
7.1.17 Furnace AA QC Analyses (Method of Standard Additi
is)
7.1.17.1 Because of the nature of the GFAA tec
procedures summarized in Figure E-2 will be requ
(These procedures do not replace those in Exhib
this document, but supplement the guidance proyl
ies, the special
(for quantitation.
:ion 5.6.12 of
7.1.17.1.1 All analyses must fall within
addition, all analyses, except during fu
Additions (MSA), will require duplicate/in
raw data as well as the average intens
A maximum of 10 full sample analyses
may be performed between each conse
and blank. The raw data package
concentration values for both inj
relative standard deviation (RSD)
For concentrations greater than CRQL,
readings must agree within 15 percent
In
calibration
|ethod of Standai
ction must be repofbed/in
id concentration values.
maximunf'iaf 20 injections
calibration verification
ity and
_e value and the
of variation (CV).
duplicate injection
the analytical
ontain
the
sample must be rerun once (i.e., two additionalinjee^ions). If the
readings are still out, flagthe value reported on^FOR^ I-AAIN with
an "M." The "M" flag is requTreTr--for^the analytical>®pike as well as
the sample. If the analytacal^-sgike fora~^an^le_requires an "M"
flag, the flag must be reportea\on~TDRM~I-AAIN fortihat sample.
If the preparation blank analyica
85-115 percent, the spiking solution"1
and rerunning the preparation blank one
analytical spike recove*yis still out
problem, respike aricl reanalye all an
that blank.
.yt:
'recovery is out of control
be verified by respiking
If the preparation blank
control, correct the
:al samples associated with
M" £
je if t
Lines
7.1.17.1.2
those requiring
spike to determ
analytical s-pj-ke
sample) of two
/jg/L). This requr
and the pre_uar_ation b
calibr,
accortfr
blai
bl
maly^
pro
with
digestion
or eadb^analytical sample, including
reouire at least an analytical
MSA will be~~required for quantitation. The
r/quired to be at a concentration (in the
L (except for lead which must be at 20
mt "£
-------
Exhibit E
Metal Analysis of Ambient Air
7.1.17.1.3 The analytical spike of a sample must/ be/run immediately
after that sample. The percent recovery (%R) of the. spike,
calculated by the same formula as Spike Sample/Anaiyses (see Spike
Sample Analysis, this Exhibit), will then determine fte^ the sample
will be quantitated, as follows:
7.1.17.1.3.1 If the spike recovery is
must be diluted by a factor of five
spike. This step must only be perf/
dilution the spike recovery is sti
from the initial undiluted analys
indicate interference problems.
) percent, ^Bt^e sample
»n and rerun withxanothpr
once. If after
40 percent, report data
id flag/Wsth an "E" to
zovei
,50
7.1.17.1.3.2 If the spike re
absorbance or concentration is
the sample results to the MQL. I
percent or greater than 115 percent,
is > >+0 Percent and the sample
:nt/of the spike, report
spi^e is less than 85
esult with a "W."
7.1.17.1.3.3 If the sample absorbance or concentration is < 50
' * ^s^ /
percent of the spike arid theSpike^Eecpvery is ats/or between 85
percent and 115 percem:, tAfiL^samle mus^~1re—quantitated directly
from the calibration curye apd repoijted^own to/the MQL.
7.1.17.1.3.4 If the sample\ab^orb4no4 or concentration is < 50
percent of the spike and the\spikB recovery is < 85 percent or
greater than 115 percent, the^amp^s must be quantitated by MSA.
7.1.17.1.3.5
MSA analyse
e following proceHurek will be incorporated into
/alcuLations^snust be within the linear range
y ;dhe ca^45rat:ion curve generated at the
analyticaT^run.
The ""feample^and: three spikes must be analyzed consecutively
for MSASmantibaj^ion (the "initial" spike run data is
U-f icalty-sexclvWed from use in the MSA quantitation) .
le infcctioM are required for MSA quantitation.
counts as two analytical samples towards
percent QC frequency (i.e., five full MSAs
d between calibration verifications) .
runs containing only MSAs, single injections
QC samples during that run.
be prepared such that:
December, 1991
Page E-34
-------
Exhibit E
Metal Analysis of Ambient Air
Figure E-2
Furnace Atomic Absorption Analyses Sc
Prepare and Analyze
Sample and One Spike
at 2 times the CRQL
(Double Injections Required)
Analyses within
Calibration Range
YES
NO
If YES, repea^ only once
Recovery of Spike
Less than 402
If still,
/Flag Data
an "E"
NO
NO
Report Results
\jfown to MQL
Sample Absorbance or
Cone. Less than 50Z of
Spike Absorbance or Cone.
NO
Spike Recovery /
Greater than 852 and /
Less than 1153/ /
Quantitate by MSA
Spikes at 50%, 100X,
150X of Sample—Cone.
{Only Single Injections Required)
Report Results
Down to MQL
Flag with a "W"
Quantitate from
Calibration Curve
and Report Down
to MQL
If YES, repeat only once
Coefficient \
0.995
If still YES
Flag Data
with a "+"
December, 1991
Page E-35
-------
Exhibit E
Metal Analysis of Ambient Air
Oys
1) Spike 1 is approximately 50 perce
concentration.
2) Spike 2 is approximately 100 percent
concentration.
3) Spike 3 is approximately 1
concentration.
the sample
the sample
The data for each MSA analy/sis/
in the raw data documentat
measured intensities or
intercept and correlati$
be reported on FORM
MSA must be flagged on
the correlation coefficient
0.995.
If the correlation coefficient
analysis is les
repeated once.
less than 0.995,"
run with the bestir
FORM X-AAIN report\he\esuits/of both MSA analysis and
flag with a "+" for a^y MSA nfesult that yields a
correlation coefficient\lesj/than 0.995.
t be clearly identified
entrations
intercept, y-
The results shall
Values obtained by
th the letter "S" if
;reater than or equal to
icular
is must be
fficient is still
iRM I-IN from the
with a "+.'
On
December, 1991
Page E-36
-------
Exhibit E
Metal Analysis of Ambient Air
SECTION 8
REGIONAL DATA REVIEW
Contract laboratory data are generated to meet ;dhe specific needs of the
Regions. In order to verify the usability of data for t!h«L intended purpose,
each Region reviews data from the perspective of the eiid-useis- basfedupon
functional aspects of data quality. General guidelines for dataxrevie^have
been developed jointly by the Regions and the Natffcobal Program Offi*
Region uses these guidelines as the basis for data/evaluation. Indivi
Regions may augment the basic guideline review/process with additional review
based on Region-specific or site-specific concerns. Regional reviews, like
the sites under investigation, vary based on the nature/of /the problems under
investigation and the Regional response appropriate to/ thjt specific
circumstances.
Regional data reviews relating usabilifcy^of the Aata to a specific site
are part of the. collective assessment process. They complement the review
done at the SMO, which is designed to identify contr^QtuaP^screpancies, and
the review done at EMSL/LV, which is designed to evaluate Contractor and
method performance. These individufiT^&roluations are integ^ajted into a
collective review that is necessary forprogram^attd--4a]joratory administration
and management and may be used to oakevipp?Op*ia,te actiontjo correct
deficiencies in the Contractor's
December, 1991
Page E-37
-------
Exhibit E
Metal Analysis of Ambient Air
SECTION 9
LABORATORY EVALUATION SAMPLES
Although intra-laboratory QC may demonstrate
performance that can be tracked over time, an exte
program is an essential feature of a QA program
Contractor and method performance, Contractors
comparison studies conducted by the EPA. Resu
laboratory evaluation samples will be used by
Contractor's continuing ability to produce
results are also used to assess the precisi
methods for specific analytes.
rom the analysis oi
,PA to verify the
ical data. The
/of the analytical
the/
ep£able an
id accur.
Sample sets may be provided to participating^Obnt^actors as frequently
as on an SDG-by-SDG basis as a recognizable QC sample of known composition; as
a recognizable QC sample of unknown composition; orxnpt recognizable as a QC
material. The laboratory evaluation samples may be senteitfeer by the
Regional client or the National ProgeanL_Off ice, and may beNusepY for contract
action.
ed
return the data
iround time.
Contractors are required to arialyze the
package and all raw data within the coptrVct r
At a minimum, the results are evalOtated' fdr parameter identification,
quantification, and sample contamination. NConi&dence intervals for the
quantification of target comp~6ufiasNv are based\pn \eported values using
population statistics. 'EPA mavadjust the scoresxm any given laboratory
evaluation sample to compensate ror unanticipated difficulties with a
particular sample. Normally, a fraction o£\the compounds spiked into the
sample are not specifically listed^ in^-fcfee^ contract.
The Contracte
laboratory evaluation
provide^score of 90 or above.
For a score of 89 to
F
orEPO co
Contra
reduction
of sample
data audit; analylsj.s o
such as a Cure Notic?
, the^Spjitr^ctor shall describe the
action(s) taken in a letter to the
wi^shin 14 days of receipt of notification from
75, the Contractor shall be notified by the APO
edy for their unacceptable performance. A
>ut/EPA is not limited to, the following actions:
of. samples sent under the contract; suspension
Contractor; a follow-up site visit; a full
remedial PE samples; and/or contract sanction,
December, 1991
Page E-38
-------
Exhibit E
Metal Analysis of Ambient Air
MOTE: A Contractor's prompt response demonstrating /hat corrective
action has been taken to ensure the Contractor's capability to meet
contract requirements will facilitate continuatior/of/full sample
delivery.
December, 1991
Page E-39
-------
Exhibit E
Metal
Analys:
sis of Ambient Air
SECTION 10
ON-SITE LABORATORY EVALUATIONS
At a frequency dictated by a contract laboratoy
TPO, or their authorized representative will conduc,
evaluations. On-site laboratory evaluations are c
Contractor's ability to meet selected terms and
contract. The evaluation process incorporates
Quality Assurance Evaluation and an Evidentia:
the APO,
10.1
QUALITY ASSURANCE ON-SITE EVALDATIO;
10.1.1 Quality assurance evaluators ^
to verify the adequacy and maintenance
of personnel meeting experience or educatia
acceptable performance of analytical and QC
should expect items to be monitored will include
following items:
ractor's facilities
Station, the continuity
and the
The Contractor
limited to the
10.1.1.1
Size and appea
10.1.1.2 Quantity, age, avaN
performance of instrumentation.
10.1.1.3
10.1.1.4
programs.
10.1.1.5
10.1.1.6
10.1.1.7
10.1.1.8
inspect!
Availability,
/-
Staff oualifica
maintenance, and
and utilization of SOPs.
and personnel training
Re
.e storage facilities.
and raw data.
analytical logbook maintenance and review.
ictor's sample analysis/data package
evaluation, various documentation pertaining
Contractor is integrated in a profile
& evaluation. Items that may be included
laboratory evaluation sample scores, Regional
erials, and data trend reports.
December, 1991
Page E-40
-------
Exhibit E
Metal Analysis of Ambient Air
10.2 EVIDENTIARY AUDIT
Evidence auditors conduct an on-site laboratory evaluation to determine
if laboratory policies and procedures are in place to satisfy evidence
handling requirements as stated. The evidence audit jis completes the
following three activities.
10.2.1 Procedural Audit
The procedural audit consists of review/anc
SOPs and accompanying documentation for the
operations:
• Sample receiving;
• Sample storage;
• Sample.identification;
Sample security;
• Sample tracking (from re
• Analytical project file org<
10.2.2 Written SOPs Audit
The written SOPs
written SOPs to
following laboratory
identification, samp;
completion of analyy
assembly.
10.2.3 Analyti
The analytical pr
examination of theanalyt£
review the filestoBt&feermineT
ile Evidence Audit
analysis); and
and examination of the
and complete for the
ig, sample storage, sample
(from receipt to
ec£ file organization and
evidence audit consists of review and
set file documentation. The auditors
Trace.
Identificati
it inventory;
the document numbering system;
e Activity;
ivity recorded on the documents; and
December, 1991
Page E-41
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Exhibit E
Metal Analysis of Ambient Air
10.3
Error correction methods.
DISCUSSION OF THE ON-SITE TEAM'S FINDINGS
The quality assurance and evidentiary auditors
with the APO/TPO prior to debriefing the Contractor
the auditors present their findings and recommenda
necessary to the Contractor personnel.
10.4 CORRECTIVE ACTION REPORTS IN RESPONSE
EVIDENTIARY AUDIT REPORTS
10.4.1 Following an on-site evaluatio
audit reports which discuss deficienci
evaluation will be forwarded to the Con
discuss the corrective actions taken to res"
during the on-site visit and discussed in the
fALITY ASSURANCE AND
.ce and evidentiary
on-site
ontractor must
'deficiencies discussed
siteXeports in a letter
to the APO, TPO, EMSL/LV (response to the quality a^suraitse report) and
NEIC (response to the evidentiary report) within 14 d&ys orVeceipt of the
finding or within the time agreeaupon~-be£Heen the APO/TPQs^and the
Contractor. If SOPs are required tML_b_e^witteiTlsr--SQE§are required to be
amended, the Contractor must proVideXtnTTjWs;, to the TP07 EMSL/LV (quality
assurance/technical SOPs) and NEIC\(e^dentlary/SoP2>--wiThin 30 days of
receipt of the finding or within the\tiihf a^re/6d upon between the APO/TPO
and the Contractor.
10.4.2 If the Contract
resolve the deficienci
expect, but the Agenc
of the number of s
shipment to the Co
analysis of remed
Notice.
Ls to takeNappfcopriate corrective action to
discussed in the on-site reports, a Contractor may
.im\ted to, ttte following actions: reduction
suspension of sample
>llowrup srtfe visit: a full data audit;
ict sanction, such as a Cure
December, 1991
Page E-42
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Exhibit E
Metal Analysis of Ambient Air
(^specifying the
id security of
ritten form
yierate or
Lpn
SECTION 11
DATA MANAGEMENT
Data management procedures are defined as proce
acquisition or entry, update, correction, deletion,
computer readable data and files. These procedures
and contain a clear definition for all databases
resubmit deliverables. Key areas of concern incl
(including personnel and security), documentation,
and quality control.
11.1 DATA ENTRY
Data manually entered from hard copy irfust/be checlced/for accuracy and
the error rates estimated. Systems should/present entry of. incorrect or
out-of-range data and alert data entry persqnnel>af errors. In addition, data
entry error rates must be estimated and recorded^ on a monthly basis by
reentering a statistical sample of the data
discrepancy rates by data element.
11.2 CORRECTIONS AND UPDATES
The record of changes in the
originally generated, submitted, and,
allow traceability of updates. Docume
each change:
11.2.1 Justification or
11.2.2 Initials of
must be implemented
source generating t
11.2.3 Change
the original del
11.2.4 Resubmitted di:
a part of the laboratory
resubmiss ionx""The entice
inspected.
11.2.5
submit
dates to data
documented to
include the following for
or changes. Data changes
;roup independent of the
d according to the schedule of
11.2.
auditors^
r other deliverables must be reinspected as
inspection process prior to
not just the changes, must be
must approve changes to originally
hanges may be requested by laboratory
December, 1991
Page E-43
-------
Exhibit E
Metal Analysis of Ambient Air
software
edit contract
ed prior to
11.3 LIFE CYCLE MANAGEMENT
Life cycle management procedures must be appliedx
systems developed by the laboratory to be used to gene
deliverables. Such systems must be thoroughly testej
utilization:
11.3.1 A software test and acceptance plan
test results and acceptance criteria must
available in written form.
11.3.2 System changes must not be made
generating deliverables. Changes must
system and tested prior to implementation.
11.3.3 Each version of the production
identification number, date of installation,
archived.
11.3.4 System and operations
maintained for each system.
an operations and maintenance
11.4 PERSONNEL IDENTIFICATION REQU
will/be given an
operation and
ed and
ie a user's manual and
uction systems
a development
Individual(s) responsible for the
identified:
functions must be
11.4.1 System opera
training.
11.4.2 Data bas
quality control.
11.4.3
f.ng documentation and
£ntry, data updating and
r, backup and archiving.
December, 1991
Page E-44
-------
Exhibit E
Metal Analysis of Ambient Air
SECTION 12
REFERENCES
Office of Monitoring Systems and Quality Assurance
Protection Agency, "Interim Guidelines and Specif ij
Quality Assurance Project Plans", QAMS-005/80, De
Office of Solid Waste and Emergency Response, tf. S ./Environmental Protect
Agency, Test Methods for Evaluating Solid Vas/e, ,Third Edition, SW-846,
November 1986.
Laidlaw, R.H., "Document Control and Chain/of/Custody,
National Contract Laboratory Program," Qu^lityXJontrc
Investigations: Hazardous and Industrial Ss^id Wksxe
ASTM STP 925, C.L. Perket, ed. , American Society for
Philadelphia, 1986.
Environmental Protection Agency,
the Analysis of Pollutants Under
Final Rule and Proposed Rule", 40
209., pp 43234-43442, October 26,
American Chemical Society Committee on
Subcommittee on Environmental Analytical\Che
Acquisition and Data Quality Evaluation ii
Analytical Chemistry, Volx
EstablishingX^es t/ Procedures for
Act; FinalRule and Interim
ster, Vol. 49, No.
Improvement, and
Guidelines for Data
Chemistry",
er 1980.
iderations for the
Remedial Site
testing, Fifth Volume,
sting and Materials,
Moore, J.M. and Pearson/J.
Contract Laboratory Pr
Hazardous and Industrial /Solid
Perket, ed., Americ
emedial
>port for the Superfund
Site Investigation:
th Volume, ASTM STP 925, C.L.
terials, Philadelphia, 1986.
December, 1991
Page E-45
-------
EXHIBIT F
December, 1991
-------
EXHIBIT F
EVIDENTIARY REQUIREMENTS
TABLE OF CONTENTS
SECTION 1 SAMPLE CHAIN OF CUSTODY
1.1 SAMPLE IDENTIFICATION /./..././. F-1
1.2 CHAIN-OF-CUSTODY PROCEDURES , .A . S\. . /•/ F-1
1.3 SAMPLE RECEIVING PROCEDURES . . —\- • • / F-1
1.4 SAMPLE TRACKING PROCEDURES />\, . >x. F-3
SECTION 2 DOCUMENT CONTROL PROCED1
2.1 PREPRINTED LABORATORY F
2.2 CONSISTENCY OF DOCUMENTATI'
2.3 DOCUMENT NUMBERING AND
SECTION 3 STANDARD OP!
2.4 STORAGE OF EPA FILES . . . . . . / ............ F-5
2.5 SHIPPING DATA PA
3 . 1 SPECIFICATI
3 . 2 HANDLING
December, 1991
-------
Exhibit F
Metals in Ambient Air
SECTION 1
SAMPLE CHAIN-OF-CUSTODY
A sample is physical evidence collected from
environment. An essential part of hazardous waste
that the evidence gathered be controlled. To accoi
sample identification, chain-of-custody, sample r
procedures have been established.
1.1 SAMPLE IDENTIFICATION
1.1.1 To assure traceability of sampl
Contractor, the Contractor shall have
identification of samples throughout
1.1.2 Each sample and sample preparati
with the EPA sample number or a unique labo
unique laboratory identifier is used, it shall
EPA sample number.
1.2 CHAIN-OF-CUSTODY PROCEDURES
1.2.1 Because of the nature of\th£
EPA samples must be traceable frofc
until they are introduced as evidence
Contractor shall have procedures ensi
maintained and documented
1.2.2 A sample is
1.2.2.1 It is
1.2.2.2 It
1.2.2.3 1
1.2.2.4 It i
accessible to autho
or from the
effort is
following
acking
ssion of the
for maintaining
shall be labeled
intifier. If a
referenced to the
1.3 SAMPLE
:ed, the custody of
& samples are collected
proceedings. The
'hat EPA sample custody is
rng applies:
Ln your possession.
Jyou locked it up.
ited secure area (secure areas shall be
only).
1 designate a sample custodian responsible for
esignate a representative to receive
sample custodian is not available. The
tainers and sample bottles shall be
sample custodian or his/her representative.
December, 1991
Page F-l
-------
Exhibit F
Metals in Ambient Air
1.3.3 The condition of the custody seals (intact/
inspected upon receipt by the sample custodian or h
1.3.4 The sample custodian or his/her represent
the presence or absence of the following docume
sample shipment:
1.3.4.1 Airbills or airbill stickers.
1.3.4.2 Custody seals.
1.3.4.3 EPA custody records.
1.3.4.4 EPA traffic reports or S,
1.3.4.5 Sample tags.
shall be
representative.
1 check for
the
1.3.5 The sample custodian or his/her representative
date all forms (e.g., custody records, traffic repor
and airbills) accompanying the/sample^~-*t_^the time of
1.3.6 The Contractor shall cot
problems such as absent document
custody seals, and unsatisfactory
bottle).
1.3.7 The Contractor
problems on Telephone/
1.3.8 The follow
AADC-1 by the s
received and ins
1.3.8.1
11 sign and
.eking lists,
receipt.
repancies and
ion, broken
•ndition (e.g., leaking sample
1.3.8.2 Presence c>
shipping an<
•ecord the\resolution of discrepancies and
rded on appropriate Form
>resentative as samples are
ipping container.
and condition of custody seals on
ien present.
sample bottles.
:e of airbills or airbill stickers.
Ll sticker numbers.
Xsence of EPA custody records.
'absence of EPA traffic reports or SAS packing lists.
December, 1991
Page F-2
-------
Exhibit F
Metals in Ambient Air
1.4
1.3.8.9 Presence or absence of sample tags.
1.3.8.10 Sample tag identification numbers cross,
sample numbers.
1.3.8.11 Verification of agreement or non-a
recorded on shipping documents and sample c<
1.3.8.12 Problems or discrepancies.
SAMPLE TRACKING PROCEDURES
to the EPA
The Contractor shall maintain records
handling from receipt to final analysis.
documentation of the movement of samples
designated laboratory storage areas.
phases of sample
include
les into and out of
December, 1991
Page F-3
-------
Exhibit F
Metals in Ambient Air
SECTION 2
DOCUMENT CONTROL PROCEDURES
The goal of the laboratory document control prgrafiHs to^assure that
all documents for a specified SDG will be accounted/foir when^fche pr&ject is
completed. Accountable documents used by contract^laoratories sfaall raclude
but not be limited to logbooks, chain-of- custody
bench sheets , and other documents relating to tWe
The following document control procedures have/been established to assure that
all laboratory records are assembled and stored for deliyferv to the EPA or are
available upon request from the EPA prior to/ the delivery schedule.
2.1 PREPRINTED LABORATORY FORMS AND L06|
2.1.1 All documents produced by the Contractor wtfich are directly
related to the preparation and analysis of EPAssampl'a
-------
Exhibit F
Metals in Ambient Air
2.4
government agency or commercial client names to prese
confidentiality of commercial clients.
2.1.8 Corrections to supporting documents and ra1
drawing a single line through the error and enter
information. Corrections and additions to support!
data shall be dated and initialed. No informa
or rendered unreadable. All notations shall
portions of documents shall be "crossed"
2.2 CONSISTENCY OF DOCUMENTATION
2.2.1 The Contractor shall assign a
responsible for the organization and a;
2.2.2 All copies of laboratory doc
:he
shall be made by
correct
and raw
Literated
jsed
2.2.3 Before releasing analytical results^
shall assemble and cross-check the information^
records, laboratory bench sheets, personal and inst
relevant data to ensure that dafta-pej^aining to
sample delivery group is consistent thfoughoutsjthe CSF.
fficer
be/complete and legible.
control officer
tags, custody
ogs, and other
'cular sample or
2.3 DOCUMENT NUMBERING AND
3EDI
2.3.1 In order to provide document
analysis records, each item in a CSF\shally
serialized number as described in ExhO
CSF # - Region -
2.3.2 All documi
bench sheets,
preparation record?
analysis, custody
inventoried.
jer (For
ability of the completed
ae inventoried and assigned a
Section 2.
lie: 75-2-0240).
to each
trams,
^ ^V /
2.3.3 The Document Control
ensuring thatTHTTttecuments
and are d^livgxedto tha EPA.
plastic/ba^sin the^i^leN^ Figure
documi
Including logbook pages,
Screening records, re-
^ecords of failed or attempted
rary research results, etc., shall be
recorc
The
location.
^cer (DCO) shall be responsible for
I are placed in the CSF for inventory
10 shall place the sample tags in
of Exhibit E is an example of a
.n EPA laboratory documents in a secure
December, 1991
Page F-5
-------
Exhibit F
Metals in Ambient Air
Arables packages
the
ging or
to whom,
2.5 SHIPPING DATA PACKAGES AND CSF
2.5.1 The Contractor shall document shipment of
to the recipients. These shipments require custoj
containers placed such that they cannot be opene^
breaking the seal. The Contractor shall documej
the date, and the method (carrier) used.
2.5.2 The Contractor shall purge the CSF
EPA Region 180 days after the report submitsic
2.5.3 A copy of the transmittal letter/foi/the CSF/wi^l be sent to NEIC
and SMO.
2.5.4 The Document Control form is used to^dpcK&nenfc the receipt and
inspection of shipping containers and samples. Th£ Contractor shall
submit one original FORM AADC-1 for each ship>ing container.
2.5.5 The Contractor shall sign and date the airbi
examine the shipping containersC~rSCo*d^the presence
custody seals and their conditdor
resent),
ence of
2.5.6 The Contractor shall note\anV problems/wittr-£kuf samples and
follow the instructions explained \n Exhibit,0, Sample Log-In Sheet.
2.5.7 The Contractor shall submit a\omp^«ted Document Control Form
with each SDG package.
December, 1991
Page F-6
-------
Exhibit F
Metals in Ambient Air
SECTION 3
STANDARD OPERATING PROCEDURES
The Contractor must have written standard opera
for receipt of samples, maintenance of custody, samp
storage, tracking the analysis of samples, and ass
3.1 SPECIFICATIONS FOR WRITTEN STANDARD OPERAT
3.1.1 An SOP is defined as a written nar,
of laboratory operating procedures incl
documentation. The SOPs must accurate1
used in the laboratory, and copies
to the appropriate laboratory perso:
to ensure that analytical data produc
acceptable for use in EPA enforcement ca
edures (SOPs)
, sample
data.
Ictual
of
3.1.2 The Contractor's SOPs shall provide meet
to meet each of the following specifications and si
the basis for laboratory evidey£e~~aadits_. The Contract
written standard operating pro
re step-by-step description
laboratory
procedures
shall be available
dures are necessary
ontract are
ion and litigation.
Sample receipt and
Sample storage.
Preventing sample contain!
Security fo
Trace/bijaty of s,
Ma
documentation
ed by EPA as
must have
3.1.2.1
3.1.2.2
3.1.2.3
3.1.2.4
3.1.2.5
3.1.2.6
3.1.2.7
3.1.2.8
and logbooks.
[nd data control systems.
review of laboratory operation and
contractually-required quality assurance
each individual data package.
data handling, and reporting.
December, 1991
Page F-7
-------
Exhibit F
Metals in Ambient Air
3.1.2.13 Document control, including Case file pr<
3.1.3 The Contractor shall have a designated sample Custodian
responsible for receipt of samples and have writtpn SOPs"Ndescribing
his/her duties and responsibilities.
3.1.4 The Contractor shall have written SOPs
in of the samples. The procedures shall inc^l
documenting the following information:
3.1.4.1
3.1.4.2
3.1.4.3
lists.
Presence or absence of EPA c\
Presence or absence of air)!
Presence or absence of El
3.1.4.4 Presence or absence of custody seals
sample containers and their condition.
forms.
stickers.
or SAS packing
shipping and/or
3.1.4.5
3.1.4.6
3.1.4.7
3.1.4.8
3.1.4.9
Custody seal numb
Presence or'absence
Sample tag ID numbers.
Condition
Conditi
3.1.4.10 Veri
receiving doc
3.1.4.11 Re
3.1.4.12 The defin
upon recei
tonagreement of information on
3.1.6 The
performed on any
following:
jlems or discrepancies with the SMO.
f terms used to describe sample condition
ill havV-jgrltten SOPs for maintenance of the
I-in and shall demonstrate security of the
areas. The SOPs shall specifically include
reas for EPA samples in the laboratory, and
Icontamination. The SOPs shall include a
10 have access or keys to secure storage
11 have written SOPs for tracking the work
sample. The tracking SOP shall include the
December, 1991
Page F-8
-------
Exhibit F
Metals in Ambient Air
3.1.6.1 A description of the documentation used
receipt, sample storage, sample transfers, sample
sample analyses.
3.1.6.2 A description of the documentation
calibration and other QA/QC activities.
3.1.6.3 Examples of the document formats
used in the sample receipt, sample storage
analyses.
3.1.7 The Contractor shall have written/SO:
identification of EPA samples throughou
3.1.8 If the Contractor assigns uni
SOPs shall include a description of
laboratory identifier and cross-referenc
3.1.9 If the Contractor uses prefixes or suf f
identification numbers, the written SOPs shall
The Contractor shall have writ
laboratory maintains samples
ord sample
ations, and
cord instrument
aboratoryxdocumfentation
le transfer, and sample
\7
intaining
.entifiers, written
to assign the unique
sample number.
incl
scribing the
lition to sample
definitions.
ad by which the
ier custody;
3.1.10 The Contractor shall hav^i written S&Ps
assembly of all documents relating\toNeacb/E
and managerial review. Documents shall\b4 $
basis. The procedures must ensure tn^t al]
pages, sample tracking records, chroma
printouts, raw data summaries
documents having referei
submission to EPA./The' syste
inventory procedu
^correspond
Case are\coi
iclude
ization and
Case, including technical
led on a Case-specific
documents including logbook
charts, computer
and any other written
iled in one location for
cument numbering and
ihic
3.1.11 The Contractor shall
3.1.12 The Contra
used in preparing
r st
3.1.13 The-'Contr actos^ shal F
in sanrple/analy6is^QA/C
3.2
HANDI
'OF CONFIDENT]
writte^i-^SOPs for laboratory safety.
iave written SOPs for cleaning of glassware
samples under this contract.
's for traceability of standards used
3RMATION
3.2./1 A Contractor conduttiig work under this contract may receive EPA-
desl>gnatebVxConfidential information from the Agency. Confidential
information must be handled ^separately from other documentation developed
under thisxcontrkct. To/ac/omplish this, the following procedures for
the handling of^conlfidj^nti/il information have been established.
December, 1991
Page F-9
-------
Exhibit F
Metals in Ambient Air
3.2.2 All confidential documents shall be voider th
designated Document Control Officer (DCO).
ervision of a
3.2.3 Any samples or information received with
confidentiality shall be handled as "confidently
file shall be maintained to store this informal;
segregated from other nonconfidential informal
confidential samples shall be treated as coi
confidential information, the DCO logs thesi
Confidential Inventory Log. The information is then made available to
authorized personnel but only after it has b^en signefikout to that person
by the DCO. The documents shall be returneio to the/looked file at the
conclusion of each working day. Confidential info^ataon may not be
reproduced except upon approval by th/EPAxContractiWg Officer. The DCO
will enter all copies into the documenSv^ontfcal/sys/em. In addition,
this information may not be disposed of ekcept upon approval by the EPA
Contracting Officer. The DCO shall remove aiMkretaiivthe cover page of
any confidential information disposed of for one^year ahd^ shall keep a
record of the disposition in the Confidential Invent
December, 1991
Page F-10
-------
-------
Exhibit G
Metal Analysis of Ambient Air
EXHIBIT G
GLOSSARY OF TEEMS
Absorbance - A measure of the decrease in incident li
sample into the detector. It is defined mathematica
A =
•* solvent _
I solution
where:
.ng through a
I - Radiation intens
Aliquot - A measured portion of a field s
Analysis Date/Time - The date and milita:
introduction of the sample, standard, or bl
Analysis Group - An analysis group is a set of no mote thahx^wenty analytical
samples (as defined below) for the purpose of method Qua^ty Assurance/Quality
Control (QA/QC), such that the QA/QJTreqwLcgdby Exhibit fiS>sy at a minimum,
prepared and analyzed at a frequency of^onceper"Twen^r_analytical samples.
G-l
lysis.
clock) of the
analysis system.
Analysis Replicate - A single analyti^al\sample/prj]
preparation method and analyzed in
rough the analytical
Analysis Run - The actual instrumental
from the time of instrument calibration th;
All sample preparation analyses dihs^ng the
protocols set forth in Ejuiib>t-E^of
in the individual metho/
Analysis Spike Sampl
preparation method
Analyte - The element
interest.
Analytical
preparation
Analytical
fusion, etc
from its/ma
suitabl6.for
ly
contra
of the sample preparations
,the running of the final CCV.
s run are subject to the QC
less otherwise specified
:n through the analytical
ysis.
lysis seeks to determine; the element of
le taken through the analytical
preparation or sample preparation.
method (digestion, dilution, extraction,
orVotherwise release the analyte(s) of interest
inal solution containing the analyte which is
er analysis methods.
December, 1991
Page G - 2
-------
Exhibit G
Metal Analysis of Ambient Air
Analytical Sample - Any solution or media introduced into
which an analysis is performed excluding instrument cali
calibration verification, initial calibration blank, coj^ti:
verification and continuing calibration blank. Note
defined as analytical samples: undiluted and dilute
EPA), predigestion spike samples, duplicate samples
analytical spike samples, post-digestion spike s
samples (ICS), CRQL standard for AA (CRA), CRQL s
laboratory control sample (LCS), preparation bl
analysis sample (LRS).
'an ^instrument on
initial
ing calibration
are all
and non-
following
s (
^i
interfer
d for ICP ((
B) and linear rang*
Analytical Spike - A post -digestion spike to
adding a known quantity of the analyte to
The unspiked sample aliquot must compensa
samples by addition of ASTM Type II water x^the
volume of the spiking solution added must not
sample volume.
repared/pribr
quot
any v
ASTM Type II Water - Distilled water with a conductivi
/anno/cm at 25°C. For additional sp/
"Standard Specification for Reagera
Autozero - Zeroing the instrument atv
to running a standard blank with the
Average Intensity - The average of two dij
/•" "*•
Background Correction - A/techniquey to
contribution to the inst
to analysis by
prepared sample.
change in the spike
sample aliquot. The
of the analytical
than 1.0
L193-77,
It is equivalent
at zero.
injections (exposures).
or variable background
.nation of trace elements.
Batch - A group of s
Calibration - The e
absorbance, emissi
standards. Calibratibl
this SOW. Refer to the
method.
Calibration B,
acidified
reagents
preparati
produced
Calibration^
analyst for
curve based on the
measured characteristic of known
differ for the various methods included in
nterest for a definition specific to that
Lume of deionized distilled water
rochlorlc acid, and containing all of the
ition as those used in the analytical sample
ejected to the preparation method but is
f known standard solutions used by the
trument (i.e., preparation of the analytical
December, 1991
Page G - 3
-------
Exhibit G
Metal Analysis of Ambient Air
curve). The solutions are not subjected to the preparatic
the same matrix as the sample preparations to be analyzec
Calibration Verification (CCV) - A single element or
solution prepared by the analyst to be used to
instrument calibration with time and the instrument,
analysis of samples. The CCV can either be one or,
standards and/or an ICV. However, all analyte elf
particular system must be represented in this st
have the same matrix as the samples. The CCV
the middle of the calibrated range. Analytic
analytical samples or every 2 hours, whichevf
calibration of the analytical system.
Case - A finite, usually predetermined n
given time period from a particular site.'
Sample Management Office. A Case consists
Groups.
Coefficient of Variation (CV) - The standard deviation"
arithmetic mean.
Continuing Calibration - Analytica>
verify the calibration of the analy
thod but contain
-element standard
Ability of the
^during the
quent, to verify the
collected over a
are assigned by the
Sample Delivery
cent of the
Control Limits - A ra;
to be compliant.
if exceeded, or advi
Correlation Coeffi
dependence between
dependent they are the
least squares line.
•ery 12 hours to
Contract Required Quantitation Limit (
acceptable under the contract Statement
more) times the standard deviation of seve
blank.
mmum level of quantitation
Generally defined as 3.3 (or
icate analyses of the method
Con
urement results must fall
requiring corrective action
liant data be flagged.
(r) which indicates the degree of
/(e.g., concentration - absorbance). The more
to one. Determine on the basis of the
11 mean calendar day.
of the sample preparation (digestion).
December, 1991
Page G - 4
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Exhibit G
Metal Analysis of Ambient Air
Dissolved Metals - Analyte elements which have not been d^ges-ted prior to
analysis and which will pass through a 0.45 fan filter.
e weight after
Dry Weight - The weight of a sample based on percent solids
drying in an oven.
Duplicate - A second aliquot of a sample that is t
original sample in order to determine the precis
EBCDIC - Extended Binary Coded Decimal Interc]
Exposure - A full measurement of an emission
concentration of the analyte can be determ:
manner that meets the systems detection 1
peak scan.
External Standards - Target analytes analyzed at as^nownx^ncentration prior
to sample analysis, to determine response factors.
Field Blank - Any sample submitted i?rom~the—field identified
.yte from which the
ation system in a
referred to as a
Field Sample - A portion of material
in single or multiple containers and
Flame Atomic Absorption (AA) - Atomic
excitation.
Graphite Furnace Atomic Al
graphite cell for excita;
Holding Time - The el
the sample by the Co'
a blank.
that is contained
EPA Sample Number.
which utilizes flame for
absorption which utilizes a
from the date of receipt of
s analysis.
Independent Standar'
composed of analytes
for the initial calibratio
Inductively
sequential
the method
technique.
excitatio:
In-Hous
prepared standard solution that is
ent source than those used in the standards
que for the simultaneous or
elements in solution. The basis of
atomic emission by an optical spectroscopic
line emission spectra are produced by
p frequency inductively coupled plasma.
December, 1991
Page G - 5
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Exhibit G
Metal Analysis of Ambient Air
Initial Calibration - Analysis of analytical standards for/aperies of
different specified concentrations; used to define the liriearlty and dynamic
range of the response of the analytical instrument to ttye target analytes.
Initial Calibration Verification (ICV) - Solution(s) obtaineU.from the EPA or
prepared from stock standard solutions, metals or sa^ts xSktaine^Kfrom a source
separate from that (those) utilized to prepare the (/alteration^:starJdajrds, and
that have known concentration values. The ICV is jasea to verifyx^he
concentration of the calibration standards and thex^dequacy of theinstruijient
calibration of the calibration standards and the/adequacy of the instrument;
calibration. The ICV is not restricted to preparations made by official
agencies when EPA sources are not available bur should be/traceable to an NBS
or other certified standard.
Instrument Blank - For inorganics, acidifi
whether carry-over from a previous sample'
sd to determine
Instrument Detection Limit (IDL) - Determined by'multiply^ng by three the
standard deviation obtained for the analysis of a. stkadardsolution (each
analyte in reagent water) at a concentration of 3x-5x ibi^on three
nonconsecutive days with seven consyecuTrxveuegasurements per"
Interference Check Sample - Solution^s;\co"ttt»iniiig both interfering and
analyte elements of known concentratrpnsNthat c«i be~^»ed^j!o verify background
and interelement correction factors. This\soli/ti«to must also contain the same
matrix as the analytical preparations. \ \/ /
Interferents - Substances whii
interest.
iffeet the analysis for the element of
Internal Standards -
known concentration,
basis for quantitatic
Laboratory - Synony
ftyt
to analysis. Int
the t
sta^daird, blank, and sample at a
standards are used as the
.Aliq*
Laboratory Control Sample
specific analytes and subj ec£
monitor method yatSoT contifac^pr pe
/ ^- ~^
Laboratory
Contractor
sample Tr
receipt)
to
:tor as used herein.
spiked with known concentration of
entire analytical procedure in order to
te on which a sample is received at the
d on the shipper's delivery receipt and
red to as VTSR (validated time of sample
December, 1991
Page G - 6
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Exhibit G
Metal
Analysi
.sis of Ambient Air
Linear Range - The concentration range over which the a:
linear. The range of the instrument for a specific ana
using calibration standards. The upper limit of this
at each analysis) is the highest concentration calibr
determined value within 10% of the known value.
Mass Spectral Interference - Defined as the inabil
standard quantification ion due to presence of h
"noise" at the same mass.
Matrix - The predominant material of which
composed.
Matrix Modifier - Salts used in AA to les
interferents, viscosity, and surface tensic?
Matrix Spike - Aliquot of a sample fortified (spi
specific analytes and subjected to the entire analytf
indicate the appropriateness of the jnethod for the matri
recovery.
cal curve remains
as determined
range (determined
dard that has a
known quantities of
dure in order to
suring
Method Blank - A solution produced
method without the addition of a sample. \The s
concentrations of reagents as all othe
impurities derived from the preparation process.
reagents of variable concentrations, the m^tho
reagent concentration used in—the^ sample pr
the^jmalyt^cal preparation
contains the same
preparations plus any
For preparations containing
blank should match the maximum
ion(s).
d af tec* eachaddit
Method of Standard Addi
standard solution (spikes)/to sample
are made on the origi
y- intercept are determined by
concentration is determined by
Ideally, the spike Wlume
10% of the volume).
spectral effects. Also re
-\The addit£toi of 3 increments of a
of\:he same size. Measurements
The slope, x-intercept and
s. The analyte
bsolute vSJfcfae of the x-intercept.
to the sample volume (approximately
eract matrix effects; it will not counteract
as Standard Addition.
Method Detectij
signal, due
standard deyla
method blaj
higher than
metals is t
Of coursfes. all
integration
- TheXchemibal concentration that produces a
ich is e*mal to the student t 99 times the
es qf measurements on at least seven separate
rnkthod detection limit will be substantially
;ecrion limit. The method detection limit for
d aeviation of seven method blank analyses.
iunffl techniques must be operative and the same
izerd as when actual samples are analyzed.
December, 1991
Page G - 7
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Exhibit G
Metal Analysis of Ambient Air
MS-SCAN - The ICP is coupled to a mass selective detector/^H^re the instrument
is programmed to acquire all mass for target analytes anf to/disregard all
others.
Performance Evaluation (PE) Sample - A sample of knowA composition provided by
EPA for Contractor analysis. Used by EPA to evaluates CeSn^ractbi^performance.
Preparation Blank (also reagent, procedure, and meXhoa blank) -
inorganics, an analytical control that contains •distilled, deionizl
reagents, which is carried through the entire analytical procedure
and analyzed).
watetand
Preparation Log - An official record of the/sample preparation (digestion) .
Protocol - A compilation of the procedures tcCbe fol
sample receipt and handling, analytical
deliverables, and document control. Used s
(SOW).
with respect to
:ing and
LymouslVwith Statement of Work
Qualitative Accuracy - The ability of an analytical sysl
identify compounds.
to^correctly
itaining
Quality Control (QC) Check Sample
of analytes that is analyzed by a 1
acceptable identifications and measurements w^th/procedures
analyze environmental samples contain!
Analyte concentrations are known by the
ilys;
concentrations
that it can obtain
to be used to
or similar analytes.
Preparation of the QC check
sample by a laboratory or s
performing the analysis
Quality Control Set -
that bracket those s
Quantitative Accur.
measure the concen
Recovery - A determination
comparing measured__values
spike values. /'Recovery^
rd supplies, other than the laboratory
ical
jles plus the CCVs and CCBs
dete
tical system to correctly
intified compound.
accuracy of the analytical procedure made by
fied (spiked) sample against the known
the following equation:
zovery
'Measured value
spiked value
x 100%
Eq. G-2
Relative7 Response Factor (RRFjl - |A measure of the relative mass spectral
responses'of atKanalyte compared oo its internal standard. Relative Response
Factors a^e^deter«j.ned by analyses of standards and are used in the
December, 1991
Page G - 8
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Exhibit G
Metal Analysis of Ambient Air
calculation of concentrations of analytes in samples.
the following equation:
RRF = —2- X -I*
A,, CL
where:
A - Area of the characteristi
C = Concentration;
is — Internal standard; and;
x = Analyte of interest.
Resolution - Also termed separation, the s<£paj;
chromatogram, calculated by dividing the neif
peaks by the peak height of the smaller p«
100.
teen peaks on a
illey between the
tved, multiplied by
Retention Time (RT) - The time to elute a specific chemicalNErom a
chromatographic column for a specific carrier gas flow r*se, measured from the
time the chemical is injected into/the~^sts-*£r.eam until its^awcimum
concentration appears at the dete<(tor,
Retention Time Window - Retention tin
of interest and is the time from inj<
from a chromatographic column. The wine
of a single component standard over a 24-1
times the standard deviatiojv-of-4;he absolut
Rounding Rules - If the
the figure is dropped,
example, 11.443 is royto
If the figur
figure is drd
example, 11.446
re*
res
for each analyte
/tion of a specific chemical
^termined by three injections
Period as plus or minus three
mention time for that analyte.
retained is less than 5,
kept unchanged. As an
ned is greater than 5, the
retained figure is raised by 1. As an
'off to 11.45.
If the figure—fallowingxthose"1'fco be retained is 5, and if there are no
figures crf-her than^aeros be>ond the five, the figure 5 is dropped, and
the lasr-place-figure retaineo^i^/increased by one if it is an odd
numbe/or/ it is kep^unchanged if an even number. As an example, 11.435
is r/un^ied off to 11.4
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Exhibit G
Metal Analysis of Ambient Air
NOTE: See forms instructions (Exhibit B) for except
Run - A continuous analytical sequence consisting of pr
associated quality assurance measurements as required
Statement of Work.
Sample - A portion of material to be analyzed that
multiple containers and identified by a unique s
td samples and all
contract
Sample Delivery Group (SDG) - A unit within a
identify a group of samples for delivery. An
samples within a Case, received over a period/of
from all samples in an SDG are due concurre
the following, whichever occurs first:
• Case ; or
Each 20 samples within a Case; or
Each 14 -day calendar period during which samp}
beginning with receipt of the first sample in
NOTE: Samples may be assigned to
Tenax® tubes in one SDG, all canis
e or
Sensitivity - The slo
between emission inti
Serial Dilution -
by the dilution facto
undiluted sample within s
influence of interferents
Standard Anal;
target comp
Stock Sol
standard:
Case that is
s a group of 20 or fewer
alendar days. Data
fined by one of
[ase are received,
SDG.
method (i.e., all
Sample Number (EPA Sample Number) - A
by EPA for each sample. The EPA Sampl
Report which documents information on tha
Sample Recovery (SR) - Ttv
compared to a known quantity
ification number designated
on the sample Traffic
measured in a sample as
)
.e., functional relationship
sample by a known factor. When corrected
sample must agree with the original
Limits. Serial dilution may reflect the
.nation made with known quantities of
line response factors.
.on which can be diluted to derive other
December, 1991
Page G - 10
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Exhibit G
Metal Analysis of Ambient Air
Time - When required to record time on any deliverable
expressed as Military Time, i.e., a 24-hour clock.
Total Metals - Analyte elements which have been diges
Traffic Report (TR) - An EPA sample identification
sampler, which accompanies the sample during shipi
which is used for documenting sample condition
Twelve-Hour Time Period - The twelve (12) hour,
tuning, standards calibration (initial or con$
the moment of injection of the BFB analysis
documentation of compliant tune. The time
elapsed according to the system clock.
Validated Time of Sample Receipt (VTSR) -
received at the Contractor's facility, as
receipt and Sample Traffic Report.
Viewing Area Adjustment Standard:
strong atom line (i.e., Cu) and a
proper adjustment of the observatio'
by ICP (see Method 200.62-B for deta
ime shall be
to analysis.
period for GC/MS system
ition) begins at
:ory submits as
r 12 hours has
ich a sample is
.shipper's delivery
rd of a
used to verify the
metals analysis
10% Frequency - A frequency specification
allowing for no more than 10 analytical se
verification measurements, as—spe^cified
an analytical sequence
between required calibration
Statement of Work.
December, 1991
Page G - 11
U.S. Environmental Protection Agency
Region 5, Library, PL-12J)
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