6.3 Labware
prevent adsorption of several of the analytes.
1. Microliter syringes if making manual injec-
After several injections of sample extracts, depo-
tions (Hamilton series 701 liquid syringe, or
sition of nonvolatile residues may result in peak
equivalent).
tailing and a decline in the response for HMX. The
2. Disposable cartridge filters: 0.45 micron
injection-port liner must be changed or cleaned
(Millex SR or equivalent).
each time the septum is replaced, at least every 50
3. Pipets: Class A, glass, appropriate sizes.
injections.
4. Pasteur pipets.
5. Autosampler vials.
5.0 SAFETY
6. Disposable syringes: Plastipak, 3 mL (or
equivalent).
Standard precautionary measures used for han-
7. Volumetric flasks: appropriate sizes, with
dling other organic compounds should be suffi-
ground-glass stoppers, Class A.
cient for the safe handling of the analytes targeted
8. Vacuum desiccator: glass.
by this method. The only extra precaution that
9. Graduated cylinders: 5.00 mL.
should be taken is when handling the analytical
standard neat material of the explosives. Follow
6.4 Equipment specific to cartridge SPE
the note for drying the neat materials at ambient
1. Visiprep Solid-Phase Extraction Manifold:
temperatures in Step 10.1.
(Supelco 5-7030 or equivalent).
2. Visiprep large volume sampler (Supelco #5-
7275).
6.0 EQUIPMENT AND SUPPLIES
3. Porapak RDX (divinylbenzene/vinylpyrroli-
6.1 Instrumentation, GC system
done) Sep-Pak Vac Cartridges (one per sam-
1. GC equipped with the following:
ple) (Waters # WATO47220).
a. Heated injection port for 0.53-mm-i.d.
capillary columns.
6.5 Equipment specific to disk SPE
b. Deactivated direct injection liners (Restek
1. Vacuum filter apparatus, glass: 47 mm, with
#20964 or equivalent).
manifold or 1-L vacuum flask.
c. ECD detector (Ni63).
2. Empore SDB-RPS disks: 47-mm (one per
d. Temperature-programmable oven.
sample) (Empore #1214-5026).
2. Recommended primary column: Fused-
silica 100% polydimethylsiloxane, 0.53-mm
i.d., 1.5 m, 6 m (DB-1 or equivalent).
7.0 REAGENTS AND STANDARDS
3. Recommended secondary columns:
Reagent-grade chemicals shall be used in all
a. Fused-silica trifluoropropyl methylpoly-
siloxane, 0.53-mm i.d., 1.5 m, 6 m (Restek
tests. Unless otherwise indicated, all reagents shall
conform to the specifications of the Committee on
RTX-200 or equivalent).
Analytical Reagents of the American Chemi-
b. Fused-silica RTX-225 (50% cyanopropyl-
cal Society, where such specifications are available.
methyl50% phenyl methylpolysiloxane)
0.53-mm i.d., 1 m, 6 m.
Other grades may be used, provided that the re-
agent is of sufficiently high purity to permit its use
4. Data system for peak integration (HP 3365
without lowering the accuracy of the determina-
ChemStation or equivalent).
tion or causing interferences.
5. Hydrogen for carrier gas (99.99999+% pur-
ity), from cylinder or generator (Whatman
Acetonitrile (CH3CN), for HPLC, GC, pesti-
Model 75-32 or equivalent).
cide residue analysis, spectrophotometry.
6. Nitrogen for makeup gas (99.9995% purity,
Acetone (CH3COCH3), for HPLC, GC, pesti-
oxygen- and moisture-free), from cylinder or
cide residue analysis, spectrophotometry.
generator (Whatman 75-92 or equivalent).
7. Autosampler with ability to refrigerate vials
Isopropanol ([CH3]2CHOH), for HPLC, GC,
(HP 6890 or equivalent) (optional).
pesticide residue analysis, spectrophotome-
try.
6.2 Instrumentation, other
Methanol (CH3OH) for HPLC, GC, pesticide
1. Balance plus-minus 0.0001 g.
residue analysis, spectrophotometry.
2. Refrigerated circulating bath (Neslab Endo-
SARMs (Standard Analytical Reference Mate-
cal or equivalent).
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