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
