Page:NIOSH Manual of Analytical Methods - 9109.pdf/2

 METHAMPHETAMINE. . . on Wipes by SPE: METHOD 9109, Issue 1, dated 17 October 2011 - Page 2 of 33

REAGENTS:

EQUIPMENT:

NOTE: See APPENDIX A for special instructions on reagents. 1.	 Analytes listed in Table 1* 2.	 Internal standards from those listed in Table 9 3.	 Solvents, residue free analytical grades a.	 Isopropanol (IPA)* b.	 Methanol* c.	 Methylene chloride (CH2Cl2)* d.	 Acetonitrile* 4.	 Concentrated sulfuric and hydrochloric acids (AR or trace metals analysis grades)* 5.	 Ammonium hydroxide (NH4OH), 28-30%, A.C.S. grade* 6.	 Bromothymol blue, ≥95%, A.C.S.; crystal violet (Gentian Violet), ≥95%, A.C.S. 7.	 Purified gases: helium for carrier gas, nitrogen for drying 8.	 MSTFA (N-methyl-N-trimethylsilyl-trifluoro-acetamide) derivatizing agent* 9.	 MBHFBA (N-methyl-N,N-bisheptafluorobutyramide) derivatizing agent* 10.	 4,4’-Dibromooctafluorobiphenyl, 99% 11.	 Deionized water (ASTM type II)

NOTE: See APPENDIX B for special instructions on equipment. 1.	 Wipe, cotton gauze, (7.6 cm × 7.6 cm) 12-ply or equivalent. 2.	 Sample storage and shipping container: 50-mL polypropylene centrifuge tubes with PTFE-lined caps or equivalent. 3.	 Gas chromatograph/mass spectrometer detector, with column and integrator, See p. 9109-1. 4.	 Solid phase extraction (SPE) columns: Any of the following or other equivalent mixed phase cation exchange hydrophilic solid phase extraction columns: a.	 Waters Oasis® MCX, 60 mg/3 cc (Waters Corp. Milford, MA.) b.	 Clean Screen®, 300 mg/3 mL (United Chemical Technologies, Inc., Bristol, PA, Cat. no. #CSDAU303.) c.	 Speedisk® H2O-Philic SC-DVB (J.T.Baker, Center Valley, PA). d.	 BOND ELUT-CERTIFY®, 200 mg/3mL (Agilent Technologies, Santa Clara, CA). 5.	 Collection tubes and GC vials: a.	 Glass test tubes (13 mm x 100 mm) with PTFE-lined caps b.	 GC autosampler vials, 2-mL Limited-volume, 300-500 μL (amber vials recommended), and caps. 6.	 Volumetric flasks: 10-, 100-, and 250-mL. 7.	 Reagent bottle, 4-L. 8.	 Liquid Transfer: a.	 Syringes: 10-, 25-, and 100-μL. b.	 Mechanical pipette with disposable tips, 5-mL. c.	 Repeating dispensers: 1 to 5-mL. d.	 Syringe or repeating dispenser: 100-μL. e.	 Syringes: 250-μL. 9.	 Forceps. 10.	 Gloves: latex or nitrile. Avoid vinyl gloves (see 9109-3, Sampling, step 1, NOTE 2). 11.	 Rotating mixer capable of 10-30 rpm. 12.	 Vacuum manifold box with 12 to 36 vacuum ports, and adjustable flow rates. 13.	 Nitrogen blow-down apparatus with water bath capable of maintaining 35 ºC. 14.	 Vortex mixer. 15.	 Pasteur pipettes. 16.	 pH paper. 17.	 Template: 10 cm x 10 cm (or 1 foot x 1 foot) opening made of relatively rigid disposable cardstock or sheet of PTFE. 18.	 Ice or other cold media for shipping.

SOLUTIONS: NOTE: See APPENDIX A for special instructions on solutions. 1.	 Prepare solutions of analytes of interest (Table 1). Calculate concentrations as the free base. Keep solutions refrigerated (<6 °C). Protect solutions from light. a.	 Stock solutions are prepared at about 1-2 mg/mL in methanol. b.	 Analyte spiking solutions are prepared by diluting the stock solutions to about 200 μg/mL each in methanol. 2.	 Prepare internal standard spiking solution in methanol at about 200 μg/mL. NOTE: Add about 2 mg of crystal violet per 20 mL of internal standard spiking solution to help indicate which samples have been spiked. 3.	 Desorption solution: 0.1 M sulfuric acid. Add 22 mL conc. sulfuric acid to 4 liters deionized water. 4.	 Bromothymol blue pH indicator solution: 1 mg/mL in 4:1 isopropanol:deionized water. 5.	 Crystal violet indicator: 2-3 mg/mL in isopropanol. 6.	 Solid phase extraction (SPE) wash solution: Aqueous 0.1 M hydrochloric acid: Dilute 8.3 mL concentrated hydrochloric acid in about 800 mL water, dilute to 1 liter with ASTM Type II water. 7.	 SPE elution solution: 80:20:2 CH2Cl2:IPA:NH4OH v/v. Prepare fresh daily. 8.	 0.3 M hydrochloric acid in methanol: Dilute 2.5 mL conc. hydrochloric acid in about 80 mL methanol; dilute to 100 mL with methanol. 9.	 Derivatization diluent solvent: acetonitrile containing 4 μg/mL of 4,4’-dibromo-octafluorobiphenyl (optional).


 * See SPECIAL PRECAUTIONS

Method rev. 1.1.1

NIOSH Manual of Analytical Methods (NMAM), Fifth Edition