METHAMPHETAMINE and Illicit Drugs, Precursors and Adulterants on Wipes by Liquid-Liquid Extraction FORMULA: Table 1
MW: Table 1
METHOD: 9106, Issue 1
CAS: Table 1
EVALUATION: Partial
U.S. regulatory OELS OSHA or MSHA: none for surfaces Other published OELs and guidelines NIOSH, ACGIH, or AIHA: none for surfaces States: Table 2
9106
RTECS: Table 1
Issue 1: 17 October 2011
PROPERTIES: Table 3
SYNONYMS: Table 4 SAMPLING SAMPLER:
Wipe
SAMPLE AREA:
100 cm² or 1000 cm²
SHIPMENT:
Preferably ship refrigerated, <6 °C
SAMPLE STABILITY:
30 days at <6 °C (See Table 5)
FIELD BLANKS:
2 to 10 blanks per sample set
MEASUREMENT ACCURACY LEVEL STUDIED:
3 μg/sample on smooth surfaces
BIAS:
Table 11a and 11b
OVERALL PRECISION ( ACCURACY:
):
Table 8a and 8b [1] Table 8a and 8b [1]
MEASUREMENT TECHNIQUE:
GAS CHROMATOGRAPHY/MASS SPECTROMETRY
ANALYTES:
Table 1
DESORPTION:
0.1 M sulfuric acid
CLEANUP/ EXTRACTION:
Hexane cleanup followed by methylene chloride extraction
DERIVATIZATION:
Chlorodifluoroacetic anhydride
INJECTION:
2 µL, splitless
TEMPERATURE - Injection: 265 °C - Detector: 285 °C - Column: 90 °C (2 min), 310 °C (10 °C/ min), hold for 11 min MASS SPECTROMETER: Scan mode (29 – 470 AMU), 2 scan per sec, Selected ion monitoring (SIM) mode Table 6 CARRIER GAS:
Helium, 1.5 mL/min
COLUMN:
Capillary, fused silica, 30 m × 0.32 mm ID; 0.5 μm film DB-5ms or equivalent
CALIBRATION:
Standards from spiked wipes with internal standard, See Table 7
RANGE:
Table 8a and 8b [1]
ESTIMATED LOD:
Table 5
PRECISION ( ):
Table 8a and 8b [1]
APPLICABILITY: For methamphetamine, the range is 0.05 to 60 μg/sample (sample = 100 cm2 or 1000 cm2). This method was developed for the analysis of selected drugs and precursors on surfaces in clandestine drug labs. [1, 2] Sampling methodology was tested using wipes on smooth, non-porous surfaces. The APPENDIX contains sampling information for other types of surfaces. INTERFERENCES: No chromatographic interferences detected. Water, surfactants and polyols inhibit derivatization. OTHER WIPE METHODS: NIOSH 9109 uses solid-phase extraction and gas chromatography/mass spectrometry (GC/MS) to measure multiple drugs [3]. NIOSH 9111 uses liquid chromatography/mass spectrometry (LC/MS) to measure methamphetamine [4]. NIOSH Manual of Analytical Methods (NMAM), Fifth Edition
Method rev. 1.1.1
