8 Hour Stability

Application Note:
AN_E0637
Key Words
• ICP-AES
• Environmental
Analysis
• SW-846 Method
6010B
• US EPA
• SW-846 Method
3050B
US EPA SW-846 Method 6010B using the IRIS
Intrepid II ICP-AES
1. Introduction
This Application Note describes the use of the Thermo
Electron Corporation IRIS Intrepid II ICP-AES to carry
out SW-846 Method 6010B compliant analysis. The
method is suitable for the determination of 31 elements
in ground waters, TCLP and EP extracts, industrial and
organic wastes, soils, sludges and sediments. This note
provides data showing compliance with each of the
requirements and highlights the integrated system tools
specifically designed to aid compliance.
2. Background
EPA Historical Facts
In 1970, the United States government established the
Environmental Protection Agency (EPA) in response to
growing public demand for cleaner water, air and land.
Prior to this, the national government was not structured
to deal with pollution that caused harm to human health
and degraded the environment. The EPA was tasked with
repairing the damage already done and moving towards
a cleaner environment. Its mission is to protect human
health and to safeguard the natural environment. The
Agency provides leadership in the nation's
environmental science, research, education and
assessment efforts and works closely with other federal
agencies and local government to develop and enforce
regulations under existing environmental law. The
Agency is responsible for researching and setting national
standards for a variety of environmental programs and
delegates the responsibility for issuing permits, and
monitoring and enforcing compliance, to local
government. Where national standards are not met, the
EPA can issue sanctions and take other steps to assist
local government in reaching the desired levels of
environmental quality. The Agency also works with
industries and all levels of government in a wide variety
of voluntary pollution prevention programs and energy
conservation efforts. Its protocols have also been
adopted as the basis for national or local standards in
many countries around the world.
Office of Solid Waste
The EPA's Office of Solid Waste (OSW) regulates all waste
under the Resource Conservation and Recovery Act
(RCRA). The RCRA's goals are to:
1. Protect the public from the hazards of waste disposal
2. Conserve energy and natural resources by recycling and
recovery
3. Reduce or eliminate waste, and
4. Clean up waste, which may have spilled, leaked, or
been improperly disposed of.
The RCRA tightly regulates all hazardous waste from
production to disposal. The RCRA also controls domestic
and industrial waste. Industrial waste is process waste that
comes from a broad range of operations. Some wastes are
managed by other federal agencies or state laws. Examples
of such wastes are animal waste, radioactive waste, and
medical waste.
The EPA publication SW-846, entitled Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods, is the
OSW's official compendium of over 200 analytical and
sampling methods that have been evaluated and approved
for use for analysis relating to the RCRA regulations. SW-
846 functions primarily as a guidance document setting
forth acceptable, although not required, methods for the
regulated and regulatory communities to use in responding
to RCRA-related sampling and analysis requirements. SW-
846 is a multi-volume document that changes over time as
new information and data are developed. It was first issued
by the EPA in 1980 and is currently in its fourth edition.
Advances in analytical instrumentation and techniques are
continually reviewed by the OSW and incorporated into
periodic updates to SW-846 to support changes in the
regulatory program and to improve method performance
and cost effectiveness. To date, the EPA has finalized
Updates I through IIIA of the SW-846 manual, and the
updated and fully integrated manual contains approximately
3500 pages. The Methods Team of OSW has also made
Draft Updates IVA and IVB available for public discussion.
The SW-846 Method 6010B describes the use of ICP-
AES instrumentation for determining a variety of metallic
elements in aqueous and solid media. In draft edition IVA of
November 2000, updated Method 6010C is under
consideration.

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.

Blanks
Two types of blanks are required for the analysis of
samples prepared by any method other than EPA Method
3050B. The calibration blank is used in establishing the
analytical curve and the method blank is used to identify
possible contamination resulting from either the reagents
(acids) or the equipment used during sample processing
including filtration.
The calibration blank is prepared by acidifying
reagent water to the same concentrations of the acids
found in the standards and samples. A sufficient quantity
must be prepared to flush the system between standards
and samples. The calibration blank will also be used for
all initial (ICB) and continuing calibration blank (CCB)
determinations.
The method blank must contain all of the reagents in
the same volumes as used in the processing of the samples.
The method blank must be carried through the complete
preparation procedure and contain the same acid
concentration in the final solution as the sample solution
used for analysis
Check Solutions
The initial calibration verification (ICV) standard is
prepared by combining compatible elements from a
standard source different from that used to prepare the
calibration standard, and at concentration near the
midpoint of the calibration curve. This standard may also
be purchased commercially.
The continuing calibration verification (CCV)
standard is prepared in the same acid matrix using the
same standards used for calibration, at a concentration
near the mid-point of the calibration curve.
The interference check solution (ICS) is prepared to
contain known concentrations of interfering elements that
will provide an adequate test of the correction factors.
The sample is spiked with the elements of interest,
particularly those with known interferences at the 0.5 to 1
mg/L level.
3.3 Method Development
Interelement Corrections
Due to the complex nature of the matrix experienced with
these types of samples, significant interferences from
spectral overlaps can be observed. As part of the method
development process, high purity solutions of the major
matrix elements, such as Al, Ca, Fe, Mg, Si and P, were
checked for their contribution to the signals of other
analyte elements. After the interfering elements were
identified, their solutions were measured and the
instrument software was used to automatically calculate
the appropriate interference correction factors.
Table 3 lists the major interferences found during this
procedure. A dash indicates that no significant interference
was encountered at the wavelength concerned.
ELEMENT WAVELENGTH (nm) INTERFERING ELEMENT
Ag 328.289 Ca, Fe
Al 308.215 -
As 189.042 -
B 208.959 Al, Fe
Ba 455.403 -
Be 313.107 -
Ca 315.887 -
Cd 214.438 Fe
Co 228.616 Fe
Cr 205.552 Fe
Cu 324.754 Ca, Fe
Fe 271.441 -
In 230.606 -
K 766.491 -
Li 670.784 -
Mg 279.079 -
Mn 257.610 Al, Mg
Mo 202.030 -
Na 589.592 -
Ni 231.604 Al, Fe
P 178.287 -
Pb 220.353 Al, Fe
Sb 206.833 Al, Fe
Se 196.090 Al, Fe
Si 251.612 -
Sn 189.989 -
Ti 334.941 -
Tl 190.864 Mg
V 292.402 Fe
Y 224.306 -
Y 360.073 -
Y 361.105 -
Zn 206.200 Fe, Mg
Table 3. Interelement interferences.
Method 6010B states that interference effects must be
evaluated for each individual instrument and the
interelement corrections should be verified daily by
running an ICS. The measured values must be within 20%
for five consecutive days. They must also be verified and
updated every six months or when changes to the
instrumentation have been made (i.e. changing torch or
nebuliser or plasma conditions).
Method Detection Limits (MDL)
Method Detection Limits were established by measuring a
solution containing all the analytes at concentration levels
which are 3 - 5x the published Instrument Detection
Limits for the IRIS Intrepid II. The solution was analysed
ten times on three separate days and the mean of the three
sigma values from all runs was calculated. Table 4 lists the
MDL’s in mg/L measured in the test and Method 6010B
calls for them to be re-confirmed on a quarterly basis.

ELEMENT WAVELENGTH MDL MAXIMUM
(nm) (µg/L) LINEAR RANGE (mg/L)
Ag 328.289 0.5 10
Al 308.215 11.4 1000
As 189.042 2.1 50
B 208.959 2.2 10
Ba 455.403 0.7 50
Be 313.107 0.1 10
Ca 317.933 2.6 1000
Cd 214.438 0.1 20
Co 228.616 0.2 100
Cr 205.552 0.3 50
Cu 324.754 0.5 50
Fe 271.441 52 1000
K 766.491 30 500
Li 670.784 1.0 50
Mg 279.079 40 1000
Mn 257.610 0.1 20
Mo 202.030 0.5 20
Na 589.592 10 200
Ni 231.604 0.4 50
P 178.287 3.2 20
Pb 220.353 2.1 50
Sb 206.833 2.4 50
Se 196.090 2.8 50
Si 251.612 7.2 50
Sn 189.989 1.8 50
Ti 334.941 0.2 20
Tl 190.864 1.6 100
V 292.402 0.6 50
Zn 206.200 0.2 20
Table 4. Wavelengths, Method Detection Limits and Maximum Linear Range.
Linear Concentration Range
The upper limit of the linear dynamic range must be
established for each analyte and instrument configuration.
The upper range limit should result in an observed signal
no more than 10% below the level extrapolated from the
normal calibration curve. This check should be carried
out whenever instrument changes occur and at six
monthly intervals as a minimum.
This evaluation is very important when using interelement
correction since, if the linear range is exceeded for
the interfering element measurement, the calculated
correction factor will be incorrect and the analytical result
will be in error.
For some elements the plasma is viewed in radial
mode using a weaker line to improve the linear range.
This results in less chance of some samples being overrange
so that more accurate data is achieved. Table 4
shows the maximum linear range figures in mg/L.
Background Correction Points
Method 6010B requires that off-peak background
correction is used for trace element determinations. The
background was measured simultaneously by monitoring
the signal in pixels adjacent to the analyte peak position.
The ideal position of background correction points was
determined by examining spectra in subarrays for a
calibration blank, calibration standard and spiked matrix
solution. The points selected for analysis should take into
account any spectral interferences that may be present.
The documented data for all decisions related to
wavelength choice (where different to the EPArecommended
lines), background correction points,
interelement corrections and MDL’s must be kept on file
and be available for review by the data user or auditor.
4. Results and Discussion
4.1 Initial (ICV) and Continuing (CCV) Calibration
Verification
Method 6010B requires that a very strict quality control
procedure is followed to ensure validity of sample data.
Quality control checks are carried out following
instrument calibration, during sample analysis and at the
end of the analytical run. For the sample data to be
acceptable all checks must meet the required criteria.
The instrument was set up using the parameters shown in
Table 1 and allowed to stabilise for 30 minutes prior to
calibration.
Immediately after calibration, an Initial Calibration
Verification (ICV) solution, calibration blank and
Continuing Calibration Verification (CCV) solution were
run. The calibration blank value must be within 3 times
the Method Detection Limit (MDL) while the calibration
verification solution results must be within 10% of their
calibrated value. In addition, the standard deviation for a
minimum of 2 resamples must be less than 5% for the
data to be acceptable. Typical results are shown in Table 5
below.
Analysis of the CCV solution and calibration blank
was then repeated every 10 samples to ensure that the
instrument remained in calibration.
4.2 Interference Check Solutions
Prior to the start of each sample analysis, interference
check solutions were run to verify that the inter-element
correction factors and background correction points were
still valid.
Interference Check Sample A (ICSA) was prepared
containing 500mg/L Al, Ca, Mg and 200mg/L Fe.
Interference Check Solution AB was then prepared by
spiking this solution at concentrations of 0.05 to 1mg/L
for the analyte elements. The values measured for ICSAB
must be within 20% of the true value for the data to be
acceptable. Data is shown in Table 6 below.

ELEMENT ICV (µg/g) CCV (µg/g)
ACTUAL MEASURED ACTUAL MEASURED
Ag 1 0.96 0.5 0.51
Al 200 202 100 99.7
As 1 0.99 0.5 0.48
B 1 0.99 0.5 0.5
Ba 10 10.3 5 4.97
Be 1 1.02 0.5 0.52
Ca 200 201 100 98.8
Cd 1 1.03 0.5 0.49
Co 10 10.5 5 5.02
Cr 10 10.2 5 5.05
Cu 10 9.80 5 4.98
Fe 200 203 100 101
K 100 98.7 50 49.9
Mg 100 101 50 50.5
Mn 10 9.85 5 4.92
Mo 1 1.02 0.5 0.48
Na 100 102 50 51.2
Ni 10 10.1 5 5.10
P 10 10.2 5 5.07
Pb 10 9.93 5 5.04
Sb 1 0.98 0.5 0.48
Se 1 1.05 0.5 0.53
Ti 10 10.1 5 5.02
Tl 1 0.97 0.5 0.48
V 10 10.4 5 4.89
Zn 10 10.1 5 5.02
Table 5. Calibration QC Checks.
4.3 Correction Factor Stability Evaluation
The IRIS Intrepid II XDL spectrometer has a highly
regulated temperature controlled optical system. This
ensures that peak analytical performance is maintained
over extended time periods, despite any fluctuations in the
general laboratory conditions.
An interference correction was set up for Fe on Cd
and then a high purity iron solution was measured over
an 8 hour period in order to assess the amount of drift on
the Cd signal in this time frame. A plot of the data is
shown in Figure 1.
To provide additional evidence of the instrument
stability, a nominal 100 ppb multielement standard was
analysed over an 8 hour period, without any calibration
updates. The plots are shown in Figure 2 and illustrate the
inherent stability of the system.
ELEMENT ICSA ICSAB TARGET VALUE %
(µg/L) (µg/L) (µg/L) RECOVERY
Ag < 0.5 98.7 100 98.7
As -1.3 100.7 100 100.7
B < 2 499 500 99.8
Ba < 0.7 486 500 97.2
Be < 0.1 495 500 99.0
Cd < 0.1 103 100 103
Co < 0.2 489 500 97.8
Cr < 0.3 476 500 95.2
Cu < 0.5 478 500 95.6
Mn < 0.1 512 500 102
Mo < 0.5 478 500 95.6
Ni < 0.4 952 1000 95.2
P < 3 475 500 95
Pb < 2 48.9 50 97.8
Sb < 2 503 500 101
Se < 3 58 50 116
Si < 7 47 50 94
Ti < 0.2 507 500 101
Tl < 2 88.5 100 88.5
V < 0.6 487 500 97.4
Zn < 0.2 1012 1000 101
Table 6. Results for Interference Check Solutions.
4.4 Sample Results
After the successful analysis of the specified quality
control solutions, the actual sample analysis sequence can
begin. With the exception of groundwater samples, all
aqueous and solid matrices require acid digestion prior to
analysis. Recommended dissolution procedures for real
samples are given in EPA Method 3050B or 3051A (the
latter being a microwave-assisted version of the former).
Groundwater samples that have been pre-filtered and
acidified do not need acid digestion.
It is general practice to include at least one Laboratory
Control Sample (LCS) in each run, the LCS normally
being a Standard Reference Material with a similar matrix
to the samples being analysed. In this particular analysis, a
sample of Buffalo River Sediment (NBS SRM2704) was
prepared and used as the LCS.
This sample can also be prepared and analysed in
duplicate, at least once per analysis, in order to check for
contamination problems. The sample was also spiked and
analysed to monitor spike recoveries.
Method 6010B states that duplicate samples must
agree within 20% of each other and spiked samples must
be recovered within 25% of the actual value.

Concentration (ug/L)
110
105
100
95
90
85
80
10:38
11:15
11:44
8 Hour Run, drift of Corrected Cadmium with Iron IEC
12:16
12:48
13:14
13:40
EPA Acceptable Range
EPA Acceptable Range
13:57
8 Hour Stability
1 21 41 61 81 101 121
Sample number
ELEMENT MEASURED CONCENTRATION CERTIFIED VALUE
As 23.1µg/g 23.4+/- 0.8
Ba 407µg/g 414 +/- 12
Ca 2.55% 2.60 +/- 0.03
Cd 3.50µg/g 3.45 +/- 0.22
Co 14.3µg/g 14 +/- 0.6
Cr 132µg/g 135 +/- 5
Cu 100.2µg/g 98.6 +/- 5.0
Fe 4.03% 4.11 +/- 0.10
K 2.02% 2.00 +/- 0.04
Mg 1.21% 1.20 +/- 0.02
Mn 547µg/g 555 +/- 19
Na 0.53% 0.547 +/- 0.014
Ni 43.8µg/g 44.1 +/- 3.0
Pb 163µg/g 161 +/- 17
Sb 3.61µg/g 3.79 +/- 0.15
Ti 0.46% 0.457 +/- 0.018
V 93µg/g 95 +/- 4
Zn 440µg/g 438 +/- 12
Table 7. NBS 2704 Buffalo River Sediment Data
14:25
15:12
15:40
15:55
16:25
16:50
17:18
17:42
18:00
2
1.5
1
0.5
0
-0.5 -
-1 -
-1.5 -
-2 -
PPB
As1890
Ba4554
Cd2288
Pb2203
Se1960
Zn2138
Figure 1. Stability of
the Fe interelement
correction factor for
Cd
Figure 2. Stability of a
100ppb multielement
standard over an 8
hour period
Table 7 compares the measured and certified results
for the SRM2704 Buffalo River Sediment sample,
demonstrating the excellent agreement between them.

Table 8 shows the results for a duplicate analysis test
with the LCS sample. Agreement between duplicates is
generally within 1%, well within the EPA limit of 20%.
ELEMENT ANALYSIS 1 ANALYSIS 2 % DIFFERENCE
As 23.1µg/g 23.3µg/g 0.8
Ba 407µg/g 403µg/g 1.0
Ca 2.55% 2.54% 0.4
Cd 3.50µg/g 3.46µg/g 1.1
Co 14.3µg/g 14.4µg/g 0.7
Cr 132µg/g 131µg/g 0.8
Cu 100.2µg/g 101µg/g 0.8
Fe 4.03% 4.04% 0.3
K 2.02% 2.03% 0.6
Mg 1.21% 1.20% 0.3
Mn 547µg/g 543µg/g 0.8
Na 0.53% 0.54% 1.8
Ni 43.8µg/g 44.1µg/g 0.7
Pb 163µg/g 163µg/g 0.2
Sb 3.61µg/g 3.65µg/g 1.1
Ti 0.46% 0.46% 0.4
V 93.0µg/g 92.3µg/g 0.8
Zn 440µg/g 435µg/g 1.1
Table 8. NBS 2704 Buffalo River Sediment Duplicate Analysis Test
Table 9 shows the recoveries from spiked samples of
the LCS, again all well within the EPA 25% limit.
ELEMENT CERTIFIED VALUE SPIKE CONC MEASURED VALUE % REC
www.thermo.com/elemental
µg/L µg/L µg/L
As 230 50 276 92
Ba 4140 100 4234 94
Cd 34.5 10 43.6 91
Co 140 10 151 110
Cr 1350 50 1402 104
Cu 986 50 1033 94
Mn 5550 100 5652 102
Ni 441 10 450 90
Pb 1610 50 1656 92
Sb 37.9 10 47.0 91
V 950 50 1004 108
Zn 4380 100 4482 102
Table 9. NBS 2704 Buffalo River Sediment Spike Sample Recovery Data
In order to check that the method works for different
sample matrices, a reference sample of a sewage sludge
(BCR146) was analysed using exactly the same procedure.
Table 10 compares the measured and certified results for
the sediment sample, demonstrating the excellent
agreement. Values in brackets are advisory figures only.
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ELEMENT MEASURED CONCENTRATION CERTIFIED VALUE
Ca 10.2% (10.14%)
Cd 75.8µg/g 77.7 +/- 2.6
Co 11.9µg/g 11.8 +/- 0.7
Cu 928µg/g 934 +/- 24
Fe 1.80% (1.86%)
K 0.49% (0.48%)
Mg 2.01% (1.99%)
Mn 570µg/g 588 +/- 24
Na 0.21% (0.22%)
Ni 276µg/g 280 +/- 18
P 2.52% (2.58%)
Pb 1260µg/g 1270 +/- 28
Zn 4040µg/g 4059 +/- 90
Table 10. BCR146 Sewage Sludge Data
5. Conclusions
The IRIS Intrepid II demonstrates SW-846 Method 6010B
compliant analysis for a range of sample types and easily
copes with the stringent interference checks and AQC
requirements stipulated for use in this method.
The IRIS Intrepid II is the latest generation of IRIS
ICP Spectrometers from Thermo Electron. It incorporates
a new design of the exclusive charge injection device
(CID) detector housed in a highly regulated optical
system. The result of these product developments is an
instrument that is capable of providing extremely low
detection limits and excellent long term stability. This
makes the IRIS Intrepid II ideally suited for cost-effective
elemental analysis in the environmental field.
References
USEPA SW-846 Method 3050B, Revision 2, December 1996.
USEPA SW-846 Method 3051A, Revision 1, January 1998.
USEPA SW-846 Method 6010B, Revision 2, December 1996.
USEPA SW-846 Method 6010C, Revision 3, November 2000.
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AN_E0637 06/03