8 Hour Stability

Method 6010B (and draft 6010C)
Both methods are broadly similar and provide guidelines
on general laboratory practices such as sample
preparation, instrument setup, calibration of analytes,
and interference correction equations. They also provide
specific rules on various analytical practices that must be
followed, including elements covered, quality control
practices and instrument validation. Since both methods
are well established and readily available in the public
domain they have become widely adopted as templates
for methodologies used by a host of laboratories
undertaking environmental analysis world-wide. The
aim of the protocol is to ensure a consistently high
quality of analytical data by enforcing compliance with a
variety of stringent instrument and analytical
performance checks.
NOTE: Method 6010C, along with all Draft Update IVA SW-846 methods,
may be downloaded from the EPA OSW website:
http://www.epa.gov/epaoswer/hazwaste/test/up4a.htm
3. Experimental
3.1 Equipment
An IRIS Intrepid II Model XDL ICP-AES (Thermo
Electron Corporation, Franklin, Mass., USA) was used
for the analysis of soil and sludge samples. It was fitted
with a dual view optical design - axial view was used for
elements expected at low concentration where the best
sensitivity is required while radial view was used for
elements at higher concentration or for those elements
that suffer from EIE (Easily Ionised Element) interference.
Internal standards were added on-line using the Internal
Standard Mixing Kit (P/N 13670800).
The instrument conditions used for the analysis are
shown in Table 1 below.
PARAMETER VALUE
RF Forward power 1200 watts
Torch Orientation Dual View
Torch Gas Flow 16 L/min
Auxiliary Gas Flow 0.5 L/min
Mixing Chamber Glass Cyclone
Nebulizer Glass Concentric
Nebulizer Gas 0.65 L/min
Sample Pump Winding 3-stop Orange Tygon
Sample Uptake 1.7 mL/min
Purge Gas Argon
Tank Flow 4 L/min
Nozzle Flow 4 L/min
Camera Flow 1 L/min
Table 1. Intrepid II XDL Parameters
Details of the wavelengths and plasma view
orientations used, as well as the internal standards
employed, are shown in Table 2.
ELEMENT WAVELENGTH PLASMA INTERNAL
(nm) VIEW STANDARD
Ag 328.289 Axial Y 361
Al 308.215 Radial Y360
As 189.042 Axial Y224
B 208.959 Axial Y224
Ba 455.403 Radial Y360
Be 313.107 Radial Y360
Ca 317.933 Radial Y360
Cd 214.438 Axial In230
Co 228.616 Axial In230
Cr 205.552 Axial Y224
Cu 324.754 Axial Y361
Fe 271.441 Radial Y360
In 230.606 Axial Int Std
K 766.491 Radial Y360
Li 670.784 Radial Y360
Mg 279.079 Radial Y360
Mn 257.610 Axial Y361
Mo 202.030 Axial Y224
Na 589.592 Radial Y360
Ni 231.604 Axial In230
P 178.287 Axial In230
Pb 220.353 Axial In230
Sb 206.833 Axial Y224
Se 196.090 Axial Y224
Si 251.612 Radial Y360
Sn 189.989 Axial In230
Ti 334.941 Axial Y361
Tl 190.864 Axial In230
V 292.402 Axial Y361
Y 224.306 Axial Int Std
Y 360.073 Radial Int Std
Y 361.105 Axial Int Std
Zn 206.200 Axial In230
Table 2. Wavelengths and Plasma View used.
3.2 Calibration Solutions
Calibration Solutions
High purity reagents were used throughout. Calibration
standards were prepared in 5%v/v HCl and 1%v/v HNO3
from a range of SPEX ICP standards at concentrations
selected to cover the linear range for each element.
Mixed calibration standards were prepared according
to the conditions laid down in Method 6010B.
SOLUTION ELEMENTS
I Be, Cd, Mn, Pb, Se and Zn
II Ba, Co, Cu, Fe and V
III As and Mo
IV Al, Ca, Cr, K, Na, Ni, Li and Sr
V Ag, Mg, Sb and Tl
VI P
A mixture of 20ppm In and 10ppm Y was used as the
internal standard.