Page:NIOSH Manual of Analytical Methods - 1025.pdf/2

 1- and 2-BR OM OP RO PAN E: ME TH OD 1025, Issue 1, dated 1 5 Ma rch 2003 - Page 2 of 4 REAGENTS:

EQUIPMENT:

1. 2. 3. 4. 5. 6. 7.

1. Sam pler: glass tu be, 7 cm long, 4-m m ID, flam e-sealed en ds w ith plastic cap s, containing two sections of Anasorb® CSC or equivalent (100/50 m g) separated b y a 2-mm urethane plug. A silylated glass wool plug precede s the front section and a 3-m m urethane foam plug follows the back section. 2. Alternative sampler: glass tube, 7 cm long, 4mm ID, flame-sealed ends with plastic caps, containing two sections of Anasorb® CMS or equivalent (150/75 m g) separated b y a 2-mm urethane plug. A silylated glass wool plug precede s the front section and a 3-m m urethane foam plug follows the back section. 3. Personal sampling pump, 0.01 to 0.2 L/min, connected with flexible tubing. 4. Ga s ch rom atog raph equ ipped with F ID, integrator and capillary column (see page 2552-1). 5. Autosampler vials, 2-mL, glass, with PTFElined crimp caps. 6. Syringes, 10-:L, 25-:L, and 1-mL. 7. Pipettes, 3-mL and 5-mL. 8. Volumetric flasks, 10-mL.

1-Bromopropane, GC grade. 2-Bromopropane, GC grade. Carbon disulfide, GC grade. Helium, prepurified and filtered. Hydrogen, prepurified and filtered. Air, compressed, purified, filtered. Calibration stock solution: Add known amounts of analytes to carbon disulfide in 10m L volum etric flas k.


 * See SPECIAL PRECAUTIONS

SPECIAL PRECAUTIONS: Carbon d isulfide is toxic, explosive, and a fire hazard (FP= -30°C). W ork with carbo n disu lfide in a w ell ventilated ho od.

SAMPLING: 1. Ca librate each sam pling pum p with a represe ntative sam pler in line. 2. Break the ends of sampling tube imm ediately before sampling. Attach sampling tube to personal sam pling pum p with flexible tu bing. 3. Sam ple at an accurately known flow rate between 0.01 and 0.2 L/min for a total sample size of 12 L. 4. Ca p the sam plers with plastic ca ps a nd p ack sec urely for shipm ent.

SAMPLE PREPARATION: 5. Place the front and back sorbent sec tions of the sampler tube in separate vials. Place the glass wool preceding the front section into the vial containing the front sorbent section. Discard the urethane foam plugs. 6. Ad d 1.0 m L of carbon disulfide into each vial. Attach crim p caps to each vial. 7. Allow to stand fo r 30 m inutes with oc cas ional agitation.

CALIBRATION AND QUALITY CONTRO L: 8. Calibrate daily with at least six working standards from below the LOD to 10 times the LO Q. If necess ary, add itional standa rds m ay be a dde d to exten d the calibra tion cu rve. a. Add kn ow n am ounts of a nalytes to carbon disulfide solvent in a 10-mL volumetric flask and dilute to the mark. Prepare additional standards by serial dilution in 10-mL volumetric flasks. b. Analyze together with samp les and blanks (steps 11 and 12). c. Prepare calibration graph (peak area vs :g analyte). NIOSH Manual of Analytical Methods (NMAM), Fourth Edition