Table 2-1M: US-EPA Method 3031 Standard Method

US-EPA Method 3031 (A13)

Acid Digestion of Oils for Metals Analysis by FLAA or ICP Spectroscopy

Type

Matrix

Analytes

Detection

Control

Microwave Digestion

Oil

Ag, As, Ba, Be, Cd, Co, Cr, Cu, Mo, Ni, Pb, Sb, Se, Tl, V, Zn

FAAS

ICP-AES

Calibration

Condensed Procedure

Method 1: 0.5 g sample and 0.5 g KMnO4

20% for 2 min

add 2 mL H2SO4, 20% for 3 min (to near dryness)

add 10 mL HNO3 and 2 mL HCl, 15% for 5 min,

20% for 3 min (to near dryness), cool for 5 min

add 5 mL HCl, 15% for 5 min

Method 2: 0.5 g sample and 10 mL H2SO4

20% for 5 min, 25% for 5 min, 30% for 5 min, 35% for 5 min, cool for 5 min

add 8 mL H2O2, 50% for 5 min, cool for 5 min

add 8 mL H2O2, 60% for 5 min

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