Page:NIOSH Manual of Analytical Methods - 7074.pdf/1

From Wikisource
Jump to navigation Jump to search
This page needs to be proofread.

TUNGSTEN (soluble and insoluble)

W

MW:

183.85

METHOD: 7074, Issue 2

OSHA : no PEL NIOSH: 1 mg/m 3 5 mg/m 3 ACGIH: 1 mg/m 3 5 mg/m 3

CAS: 7440-33-7

7074

RTECS: Y07175000

EVALUATION: FULL

Issue 1: 15 February 1984 Issue 2: 15 August 1994

PROPERTIES: brittle metal; MP 3410 °C; valence 2,3,4,5,6 solubles; STEL 3 mg/m 3 insolubles; STEL 10 mg/m 3 solubles, STEL 3 mg/m 3 insolubles, STEL 10 mg/m 3

SYNONYMS: wolfram.

SAMPLING SAMPLER:

FILTER (0.8-µm cellulose ester membrane)

FLOW RATE:

1 to 4 L/min

VOL-MIN: -MAX:

200 L @ 1 mg/m 3 1000 L

SHIPMENT:

routine

SAMPLE STABILITY:

stable at least 2 weeks @ 25 °C

BLANKS:

2 to 10 field blanks per set

MEASUREMENT TECHNIQUE:

ATOMIC ABSORPTION, FLAME

ANALYTE:

tungsten

EXTRACTION:

H 2O; 6 min, 25 °C (soluble)

ASHING:

1:1 HF:HNO 3, 10 mL; 6 h, 150 °C (insoluble)

FINAL SOLUTION:

0.05 M NaOH/2% Na 2SO 4; 25 mL

FLAME:

nitrous oxide-acetylene, reducing

WAVELENGTH:

255.1 nm

BACKGROUND CORRECTION:

none used

CALIBRATION:

W in 0.05 M NaOH and 2% Na 2SO 4

RANGE:

0.1 to 0.5 mg per sample (soluble); 0.25 to 12 mg per sample (insoluble)

ACCURACY RANGE STUDIED: BIAS:

0.42 to 2.0 mg/m 3 (soluble) [1]; 0.84 to 19.7 mg/m 3 (insoluble) [1] + 0.015

ˆ ): 0.055 (soluble) [1]; OVERALL PRECISION (S rT 0.056 (insoluble) [1] ACCURACY:

± 12.5%

ESTIMATED LOD: 50 µg soluble W per sample; 125 µg insoluble W per sample [2] PRECISION (Sr):

0.029 [1]

APPLICABILITY: The working range of this method is 0.25 to 5 mg/m 3 (soluble) and 0.6 to 5 mg/m 3 (insoluble) for a 400-L air sample. This is an elemental analysis and not compound-specific. For cemented tungsten carbide samples, cobalt can be quantitatively determined from the HCl extract used to remove interferences.

INTERFERENCES: None known. Ni, Mo, V, Mn, Cr, Co and Fe do not interfere at concentrations up to 50 times the tungsten concentration [3].

OTHER METHODS: This revises P&CAM 271 [1,3]. Method 7300 (ICP-AES) is an alternate measurement method; however, the extraction and ashing procedures described in this method must be followed.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94