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'TABLE 4. INFRARED SAMPLING AND ANALYTICAL METHODS FOR CRYSTALLINE SILICA.'

NMAM 7602 NMAM 7603 MSHA P-7 MDHS 37 MDHS 38
Matrix   coal mine dust coal mine dust    
Sampler 10-mm nylon cyclone, 1.7 L/min

Higgins-Dewell cyclone, 2.2 L/min

10-mm nylon cyclone, 1.7 L/min

Higgins-Dewell cyclone, 2.2 L/min

10-mm nylon Dorr-Oliver cyclone, 2.0 L/min Higgins-Dewell cyclone, 1.9 L/min Higgins-Dewell cyclone, 1.9 L/min
Filter 37-mm 0.8 PVC or 5-µm MCE 37-mm 0.8 PVC or 5-µm MCE 37-mm 0.8-µm, 5-µm PVC pre-weighed 37-mm 0.8-µm, 5-µm PVC 37-mm 0.8-µm, 5-µm PVC
Volume 400-800 L
total dust < 2mg
300-1000 L
total dust < 2mg
not stated ≥ 456 L
total dust < 1mg
≥ 456 L
total dust < 0.7mg
Filter Prep RF plasma asher or muffle furnace RF plasma asher or muffle furnace RF plasma asher none muffle furnace
Analytical Sample Prep mix residue with KBr, press 13-mm pellet redeposit on 0.45-µm acrylic copolymer filter redeposit on 0.45-µm acrylic copolymer filter none mix residue with KBr, press 13-mm pellet
Standard polystyrene film polystyrene film polystyrene film polystyrene film polystyrene film
Calibration quartz diluted in KBr suspensions of quartz in 2-propanol suspensions of quartz in 2-propanol sampling from a generated atmosphere of standard quartz dust sampling from a generated atmosphere of standard quartz dust
Proficiency Testing PAT PAT PAT WASP WASP
Range (µg quartz) 10-160 30-250 25-250 10-1000 5-700
LOD (µg quartz) 5 (estimated) 10 (estimated) 10 varies with particle size varies with particle size
Precision* CV < 15 % @ 30µg CV = 9.8 % @ 100 - 500 µg CV = 5-10 % @ 100 - 500 µg CV = 5 % @ 50 µg CV = 5 % @ 50 µg

* Precision is noted in terms of CV (coefficient of variation) for all methods for convenience of comparison. CV is equivalent to (relative standard deviation). In some methods, precision is noted in terms of (pooled relative standard deviation) which is equivalent to

NMAM=NIOSH Manual of Analytical Methods, MSHA=Mine Safety and Health Administration, MDHS=Methods for Determination of Hazardous Substances, PVC=polyvinyl chloride, MCE=methyl cellulose ester, RF=radio frequency, KBr=potassium bromide, PAT=proficiency analytical testing, WASP=workplace analysis scheme for proficiency, LOD=limit of detection, CV=coefficient of variation.

Infrared Methods. IR methods include NMAM 7602, NMAM 7603, MSHA P-7, MDHS 37 and MDHS 38 [63-67]. Details of these methods are listed in Table 4.

3/15/03
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NIOSH Manual of Analytical Methods