Page:NIOSH Manual of Analytical Methods - 9106.pdf/1

 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