Page:NIOSH Manual of Analytical Methods - 7301.pdf/1

 ELEMENTS by ICP (Aqua Regia Ashing) MW: Table 1 METHOD: 7301, Issue 1

CAS: Table 2

RTECS: Table 2

EVALUATION: PARTIAL

Issue 1: 15 March 2003

PROPERTIES: Table 1

OSHA : Table 2 NIOSH: Table 2 ACGIH: Table 2 ELEMENTS:

7301

aluminum* antimony* arsenic barium beryllium cadmium

calcium chromium* cobalt copper iron* lanthanum

lead* lithium magnesium manganese molybdenum nickel

phosphorus potassium selenium silver strontium tellurium

thallium tin titanium tungsten* vanadium yttrium

zinc zirconium*

SAMPLING
 * Some compounds of those elements require special sample treatment.

MEASUREMENT

SAMPLER:

FILTER (0.8-µm, cellulose ester membrane, or 5.0-µm, polyvinyl chloride membrane)

TECHNIQUE:

INDUCTIVELY COUPLED ARGON PLASMA, ATOMIC EMISSION SPECTROSCOPY (ICP-AES)

FLOW RATE:

1 to 4 L/min

ANALYTE:

Elements above

VOL-MIN: -MAX:

Table 1 Table 1

ASHING REAGENTS:

Aqua regia (1 HNO3 : 3 HCl)

SHIPMENT:

Routine

CONDITIONS:

SAMPLE STABILITY:

Stable

FINAL SOLUTION:

5% aqua regia, 25 mL

BLANKS:

2 to 10 field blanks per set WAVELENGTH:

Depends upon element, Table 3

BACKGROUND CORRECTION:

Spectral wavelength shift

CALIBRATION:

Elements in 5% aqua regia

RANGE:

Varies with element [1]

ESTIMATED LOD:

Tables 3 and 4

PRECISION ( þ r ):

Tables 3 and 4

ACCURACY RANGE STUDIED:

Not determined

BIAS:

Not determined

OVERALL PRECISION (Ö r T ):

Not determined

ACCURACY:

Not determined

Room temperature, 30 min; 150 °C to near dryness

APPLICABILITY: The working range of this method is 0.005 to 2.0 mg/m3 for each element in a 500-L air sample. This is simultaneous elemental analysis, not compound specific. Verify that the types of compounds in the samples are soluble with the ashing procedure selected. This method does not digest PVC filters completely.

INTERFERENCES: Spectral interferences are the primary interferences encountered in ICP-AES analysis. These are minimized by judicious wavelength selection, interelement correction factors and background correction [1-4].

OTHER METHODS: Flame atomic absorption spectroscopy (e.g., Methods 70XX) is an alternate analytical technique for many of these elements. Graphite furnace AAS (e.g., 7102 for Be, 7105 for Pb) is more sensitive. NIOSH Methods 7300 & 7302 are alternative digestion procedures.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition