Page:NIOSH Manual of Analytical Methods - 9109.pdf/1

 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