METHAMPHETAMINE and Illicit Drugs, Precursors, and Adulterants on Wipes by Solid Phase Extraction FORMULA: Table 1
MW: Table 1
METHOD: 9109, Issue 1
CAS: Table 1
RTECS: 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
9109
Issue 1: 17 October 2011
PROPERTIES: Table 3
SYNONYMS: Table 4 SAMPLING SAMPLER:
MEASUREMENT
Wipe
TECHNIQUE:
GAS CHROMATOGRAPHY/MASS SPECTROMETRY
SAMPLE AREA:
100 cm² or 1000 cm²
ANALYTES:
Table 1
SHIPMENT:
Ship refrigerated preferably, <6 °C
DESORPTION:
0.1 M sulfuric acid
CLEANUP/ EXTRACTION:
Solid phase extraction
SAMPLE STABILITY:
At least 30 days at <6 °C (See Table 5)
FIELD BLANKS:
2 to 10 blanks per sample set
MEASUREMENT ACCURACY LEVEL STUDIED: 3.0 μg/sample BIAS:
OVERALL PRECISION ( ACCURACY:
Table 10 [1]
): Surface recovery not performed Table 8a and 8b [1]
DERIVATIZATION: MSTFA and MBHFBA INJECTION VOLUME:
2 µL Splitless
TEMPERATURE Injection: 255 °C. Detector: 285 °C Column: 90 °C (2 min), to 310 °C (10 °C/ min), hold 6 min MASS SPECTROMETER: Scan mode (29 – 470 AMU), 2 scan/sec or selected ion monitoring (SIM) mode (Table 6) CARRIER GAS:
Helium, 1.5 mL/min
COLUMN:
Capillary, fused silica, 30 m x 0.32 mm i.d., 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. [2, 3] 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 9106 uses liquid-liquid extraction and gas chromatography/mass spectrometry (GC/MS) to measure multiple drugs [4]. NIOSH 9111 uses liquid chromatography/mass spectrometry (LC/MS) to measure methamphetamine [5].
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition
Method rev. 1.1.1
