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

This page has been proofread, but needs to be validated.
METHAMPHETAMINE and Illicit Drugs, Precursors, and Adulterants on Wipes by Solid Phase Extraction
9109
FORMULA: Table 1
MW: Table 1
CAS: Table 1
RTECS: Table 1
METHOD: 9109, Issue 1
EVALUATION: Partial
Issue 1: 17 October 2011
U.S. regulatory OELS
PROPERTIES: Table 3

OSHA or MSHA: none for surfaces
Other published OELs and guidelines
NIOSH, ACGIH, or AIHA: none for surfaces
States: Table 2

SYNONYMS: Table 4

SAMPLING
MEASUREMENT
SAMPLER: Wipe

SAMPLE AREA: 100 cm2 or 1000 cm2

SHIPMENT: Ship refrigerated preferably, <6 °C

SMAPLE
STABILITY: At least 30 days at <6 °C (See Table 5)

FIELD BLANKS: 2 to 10 field blanks per sample set

MEASUREMENT ACCURACY

LEVEL STUDIED: 3.0 μg/sample

BIAS: Table 10[1]

OVERALL
PRECISION (ŜrT): Surface recovery not performed

ACCURACY: Table 8a and 8b [1]

TECHNIQUE: GAS CHROMATOGRAPHY/MASS SPECTROMETRY

ANALYTES: Table 1

DESORPTION: 0.1 M sulfuric acid

CLEANUP/
EXTRACTION: Solid phase extraction

DERIVATIZATION: MSTFA and MBHFBA

INJECTION VOLUME: 2 µL Splitless

TEMPERATURE Injection: 255 °C

Detector: 285 &degrees;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 standards, See Table 7

RANGE: Table 8a and 8b [1].

ESTIMATED LOD: Table 5

PRECISION (Ŝr): 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 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
This article is issued from Wikisource. The text is available under Creative Commons Attribution-Share Alike 4.0 unless otherwise noted. Additional terms may apply for the media files.