Standard Operating Procedure for the Preparation of Spiked Sorbent Samples Using Liquid Spiking onto XAD-2


EPA/600/A-96/122
STANDARD OPERATING PROCEDURE FOR THE PREPARATION OF SPIKED
SORBENT SAMPLES USING LIQUID SPIKING ONTO XAD-2®
1.0 PURPOSE
The purpose of this document is to provide a detailed Standard Operating Procedure
(SOP) for preparing spiked sorbents by spiking selected Title m semivolatile organic
compounds (SVOCs) onto clean, dry XAD-2*8 using a liquid spiking technique.
2.0 SCOPE AND APPLICABILITY
2.1 Scope
This SOP covers the preparation of the standard solution and sorbent media
(XAD-2®) and the procedure for the preparation ana storage of the spiked sorbent samples.
2.2 Applicability
This SOP is applicable to the spiking of selected SVOCs, surrogates, and
internal standards. Recoveries of >60% have been demonstrated in laboratory studies for the
following compounds:
Analytes:
Benzene
Toluene
n-Octane
Chlorooenzene
o-Xylene
Cumene
Bromobenzene
3-Chlorotoluene
Dichloroethyl ether
1,4-Dichlorobenzene
31,41 -Difluoroacetophenone
p-Cresol
Acetophenone
Nitrobenzene
Hexachloroe thane
Isophorone
1,2,4-Trichlorobenzene
Naphthalene
Quinoline

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2-MethyInaphthalene
Biphenyl
4-Nitrophenol
Dibenzofuran
Fluorene
Hexachlorobenzene
Lindane
Internal Standards:
1,4-Dichlorobenzene-d«
Naphthalene-ds
Phenanthrene-d10
Acenaphthene-d,0
Chrysene-dn
PeryIene-dI2
Surrogates:
2-Fluorophenol
Phenoi-
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4.0 INTERFERENCES
Any component used during the preparation of the spiked sorbent may act as a source
of analytical interferents. Organic solvents may contain keepers or radical scavengers (for
example, cyciohexer.e in methylene chloride) which may act as analytical interferents.
Styrene, oxygenates, organic adds, esters, aicehyces and phenolic compounds may be
interferents present in XAD-2*. Exposure of XAD-2® to organic solvent vapors (such as in a
laboratory atmosphere) may cause sorption or* these compounds onto the XAD-2®.
Interferences may be minimized by using only solvents of known purity and using only
precleaned XAD-213.
5.0 SAFETY
The preparation of spiked sorbents may expose the analyst to some chemical and
physical hazards. Material safer/ data sheets (MSDSs) must be obtained, and listed guidelines
should be followed for each analyse and solvent used. Any prepaiarion of standard solutions
should be performed in a hood. Personal protective equipment such as chemical resistant
gloves, laboratory coats and laboratory safety glasses must be used while handling organic
solvents or the chemicals listed above. Gloves must also be abrasion resistant for protection
against broken glassware. The analyst must follow the specific OS HA regulations for benzene
(outlines in 29 CFR Chapter XVH, compound #1910.1028) and other carcinogenic
compounds. Spiking operations shcuid be performed in a hood or other well-ventilated area.
6.0 MATERIALS AND APPARATUS
XAD-2® glass sampling moduies (~0-g size) pre-cleaned glass wool (i.e., Soxhlef®
extracted with methylene chiorice.
Standard syringes with stainless steer5 needles (iO-5CO/xL).
Analytical balance (--piace minimum).
Volumetric flasks.
7.0 CHEMICALS AND REAGENTS
Methylene chloride - Spectrometry or equivalent grade. :
SVOC analyte standards - highest purity available.
Method 8270 internal standards (available commercially in a mixture).
Method 8270 surrogates (available commercially in a mixture).
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8.0 PROCEDURE
8.1 Selection of Compound*
Compounds were selected from the semivolatile organic compounds listed in
Title IH of the Clean Air Act Amendments of 19S0. Compounds were selected on the basis of
the following criteria:
1. They were expected to shew acceptable to excellent recoveries from sorbent
and acceptable to good chromatography.
2. The corresponding isctopicaily-Iabeied surrogates, rluorinated analogs, or
homoiogs had to be commercially available. These iscccpicaily-Iabeied or analogous
compounds could be used in the preparation of spiking mixtures for either dynamic spiking at
a field site or spiking onto sorbents which might contain the native materials upon returning
from field testing.
8.2 P-ep~radon of SnV^nq ^niron
One or more compounds selected for spiking may be chosen from the analvte
list given in Section 2.2. A stock solution containing the anaiytes in methylene chloride at a
concentration of 75C0 ftz/mL may be prepared by weighing the individual compounds on an
analytical balance, adding the compounds to a vein metric flask, and diluting to volume with
methylene chloride. The stock solution should be mixed well using sonication if necessary.
Analytical calibration standards may be prepared from this stock solution by diluting aiiquots
of -he stock solution with methylene chloride. Surrogate standards should be prepared
according to SW-846 Method 35CO (if SW-3-c Method 3270 will be used as the analytical
method). The stock solution should be stored in the refrigerator at 4°C, and should be
replaced after one year.
8.3 Prppp-r.nnn of YAP-?3 for
XAD-2® sorbent should be cleaned as described in SW-846 Method 0010, and
cleanliness must be demonstrated. Analysis by GC/MS may be used to demonstrate
cleanliness.
8.4 Preparation of Syringes for Snr-cnq
New syringes must be used, if possible. The syringes must be rinsed a
minimum of five times with methylene chloride prior to use of the syringe with the spiking
solution in order to minimize contamination and to prevent carryover between samples.
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8.5 Smkiny Procedure
The spiking procedure may be carried out as follows:
1. The XAD-2® glass sampling modules (Figure 1) mus; be prepared by adding
40 g of clean, dry XAD-2® to each sampling module. Prs-extracted glass wool must be added
to hold the XAD-2® in place in the sampling module. Alternatively, if the XAD-2® will be
extracted immediately, the 40 g of XAD-2® may be added directly to the extraction vessel
(using pre-extracted glass wool to keep the XAD-2® in piace if using Soxhler* extraction).
2. Tne desired volume of the 75C0 pg/mL spiking solution should be injected
onto the bed of XAD-2® using a gas tight syringe. Tne needle of the syringe should be
inserted into the bed of XAD-2® and the spiking solution injected in one spot.
It is recommended that the spiking volume not exceed ICO /xL, and that the amount
spiked be near the middle of the analytical calibration range.
3.6 Spiked Sample Preservation
After spiking has been completed, the XAD-2® may be extracted ana analyzed
immediately or stored for up to two weeks ina4JC(±2aG refrigerator that is free of organic
solvents . Prior to refrigerating, the glass sampling modules must be sealed tightly at both
ends, and wrapped securely. Terlon3 tape may be used to aid in sealing the ends.
3.7 * *a?yTic3? Procedure
The spiked XAD-2® may be extracted using Soxhier* extraction as described in
SW-846 Method 3540. The extracts may be applicable to analysis by gas chromatographic and
mass spectrometry methods such as the SW-8-6 Method 32~Q.
9.0 SHORT HAND PROCEDURE
1. Audit compounds must be selected from the list of applicable compounds.
2. The analyte and surrogate stock solutions must be prepared.
5. Tne XAD-2® must be prepared for spiking (SW-846 Method CO 10).
4. Tne syringes must be prepared for injection of the spiking standard.
5. Spiking must be performed onto the XAD-25 using direct liquid injection.
6. The spiked XAD-2® must be either immediately extracted and analyzed or
preserved at 4"C (±2°C) for up to two weeks.
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26/12 Socket Joint
\
Glass Wccl Plug
SorfcentTrap
(40 gram Sorient Capacity)
40 nC Glass
or Teflon® Frit
j 28/12 Socket Joint
XAD-2® Glass Sampling Module
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10.0 CALCULATIONS
Calculation of the volume of stock solution to be spiked
Vf- (C, x Ve>'Cs
•-here:
V, = Volume of the sleek solution :o be spiked (>L)
C, = Total analyte (surrogate) concentration to be spiked onto the X.AD-2® (ng/piL)
V. = Final extract volume (>L)
C, = Concentration of the stock solution (ng/'/xL)
ii.O QUALITY CONTROL
A minimum of three XAD-2® modules must be spiked at a time to allow for statistical
evaluation of reproducibility. The analyst must prepare and analyze an XAD-21* method blank
(with each set of samples extracted) spiked cniy with internal standards in order to monitor
laboratory and instrument contamination. The analyst must ensure that all reagents, solvents
and gases used are of the highest purity available (spectrometric grade or equivalent for
solvents), and that all glassware, syringes, equipment, and sorbent. used are clean. Further,
spiking and preservation must be conducted in areas that are as free of organic vapor as
possible.
12.0 DOCUMENTATION
Laboratory notebooks must be used to record all procedures. Tie notebooks should b-e
siznec and reviewed by the analyst and a supervisor or designated personnel. Chain of
custody forms must be used to track all audit materials once they are generated.
13.0 PUBLISHED REFERENCES
EPA SW-S46 Method CO10
EPA SW-346 Method 35CO
EPA SW-846 Method 3540
EPA SW-846 Method 8270
29 CFR Chapter XVII (7-1-92 Edition), pp 193-217
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TECHNICAL REPORT DATA
1. REPORT NO.
EPA/600/A-96/122
2 .
3.:
4. TITLE AND SUBTITLE
Standard Operating Procedure for the Preparation of
Spiked Sorbent Samples Using Liquid Spiking Onto
XAD-2
5.REPORT DATE
6.PERFORMING ORGANIZATION CODE
7. AUTHOR (S)
J. F. McGaughey, Eastern Research Group
J. T. Bursey, Eastern Research Group
C. M. Morris, U.S. EPA
8.PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Eastern Research Group
P.O. Box 2010
Morrisville, NC 27560
10.PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-D4-0022
12. SPONSORING AGENCY NAME AND ADDRESS
U.S.Environmental Protection Agency
NERL, AMRD, QAD
Research Triangle Park, NC 27711
13.TYPE OF REPORT AND PERIOD COVERED
Standard Operating Procedure
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
This Standard Operating Procedure is a method developed to spike semi-volatile
organic compounds on solid adsorbents by direct liquid injection for use as quality
assurance and performance evaluation standards.
17. KEY WORDS AND DOCUMENT ANALYSIS
a. DESCRIPTORS
b.IDENTIFIERS/ OPEN ENDED
TERMS
c.COSATI
Semi-volatile organic compounds, liquid
injection, solid adsorbent

18. DISTRIBUTION STATEMENT
19. SECURITY CLASS (This
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