United States
Environmental Protection
Agency
Environmental Monitoring
Systems Laboratory
Cincinnati, OH 45268
Research and Development
EPA/600/S4-89/011 Sept. 1989
Project Summary
USEPA Method Study 38
SW-846 Method 3010
Acid Digestion of Aqueous
Samples and Extracts for Total
Metals for Analysis by Flame
Atomic Absorption
Spectroscopy
K.W. Edged and D.M. Wilbers
An interlaboratory method
validation study was conducted on
SW-846 Method 3010, "Acid Digestion
of Aqueous Samples and Extracts for
Total Metals for Analysis by Flame
Atomic Absorption Spectroscopy," to
determine the mean recovery and
precision for analyses of 21 trace
metals in surface and wastewaters.
SW-846 Method 3010 includes
instructions for quality control,
sample preparation, and analysis of
samples by flame atomic absorption
Spectroscopy (FLAA).
The study design was based upon
Youden's non-replicate plan for
collaborative tests of analytical
methods. Four water matrices were
spiked with 21 trace metals at six
concentration levels, as three
Youden pairs. Nine laboratories
digested and refluxed the spiked
water matrices with concentrated
nitric acid, brought them to volume
with dilute hydrochloric acid, and
analyzed each for 21 trace metals by
FLAA. The primary objective of the
study was to analyze the results
using USEPA computer programs
entitled "Interlaboratory Method
Validation Study" (IMVS) which
produced measures of recovery and
precision for the 21 trace metals and
compared the performance of the
method between water types.
Two additional studies were also
conducted on Method 3010. One
study compared minimum detection
limits (MDLs) reported in the SW-846
method manual to MDLs determined
using Method 3010. Another study
was conducted to verify that the
lowest concentration levels of the
optimum range given in the SW-846
method manual are valid. Comparison
between the samples at the lowest
concentration level specified in SW-
846 and another sample at 50% that
value were performed for mean
recovery, overall precision, and
single-analyst precision.
The studies were conducted by The
Bionetics Corporation under the
direction of the Quality Assurance
Research Division, Environmental
Monitoring Systems Laboratory,
Cincinnati, OH under Contract No. 68-
03-3254. Analytical work was
completed as of November 30, 1987.
The report covers a period from
September 10, 1986 to February 28,
1988.
This Project Summary was
developed by EPA's Environmental
-------
Monitoring Systems Laboratory,
Cincinnati, OH, to announce key
findings of the research project that is
fully documented in a separate report
of the same title (see Project Report
ordering information at back).
Introduction
The Hazardous Waste Management
Facility Permit Regulations were promul-
gated in July, 1982 (40 CFR 265) and
provide performance standards for the
monitoring of ground waters, wastewaters
and solid wastes at hazardous waste
sites. To facilitate these standards,
certain analytical methodology are
required to assess the degree of contam-
ination at and around the area of the site.
The Manual: Test Methods for Evaluating
Solid Waste, Physical and Chemical
Methods, (SW-846), November 1986,
Third Edition, provides a unified, up-to-
date source of information on sampling
and analyses related to compliance with
Resource Conservation and Recovery Act
(RCRA) regulations. The success of
these pollution control activities,
particularly when legal action is involved,
depends upon the reliability of the data
provided by the laboratories. Therefore, it
is important to evaluate the methodology
through interlaboratory method validation
studies.
The Environmental Monitoring Systems
Laboratory, Cincinnati, OH (EMSL-
Cincinnati) develops or selects analytical
methods and provides quality assurance
(QA) support for Agency programs
involving water and wastewater
regulations. In EMSL-Cincinnati the
responsibility for providing support is
assigned to the Quality Assurance
Research Division (QARD). Its program is
designed to provide the QA support
needed to establish the reliability and
legal defensibility of water and
wastewater data collected by the Agency,
the state regulating authorities, the
private sector, and commercial
laboratories performing compliance
analyses. One of QARD's QA activities is
to conduct interlaboratory method
validation studies to evaluate analytical
methods selected for the Agency's
operating programs such as the Office of
Solid Waste.
This report describes an interlaboratory
method validation study for SW-846
Method 3010, "Acid Digestion of
Aqueous Samples and Extracts for Total
Metals for Analysis by Flame Atomic
Absorption Spectroscopy." The
elements: aluminum, antimony, barium,
beryllium, calcium, cadmium, chromium,
cobalt, copper, iron, lead, magnesium,
manganese, molybdenum, nickel,
potassium, silver, sodium, thallium,
vanadium, and zinc were analyzed using
Method 3010.
The primary objective of the study was
to characterize the behavior of Method
3010 in terms of recovery, overall and
single-analyst precision, and the effect of
water type on recovery and precision.
The study was conducted with the
cooperation of nine participating
laboratories under the direction of the
Quality Assurance Research Division,
EMSL-Cincinnati. The Bionetics
Corporation, as primary contractor to
QARD, was responsible for the collection
and characterization of the water
matrices, preparation of analyte spiking
solutions, preparation of user instructions
and report forms, distribution of samples,
and screening the returned data for gross
errors. The raw data were evaluated
statistically by the QARD using a series
of computer programs entitled, "Inter-
laboratory Method Validation Studies"
(IMVS). Upon review of the draft report
by EMSL-Cincinnati, The Bionetics
Corporation prepared the final report.
A second objective of the study was to
compare the minimum detection limits
(MDLs) reported in the SW-846 method
manual to the MDLs determined for the
21 elements using Method 3010. The
MDL for each element was obtained by
measuring the noise level response for
seven reagent water digestates with no
detectable background. The mean and
standard deviation of the noise level
responses were then calculated. Then,
each of the four water matrices was
digested and used to prepare a 5 point
calibration curve by the Method of
Standard Additions. The MDLs were
calculated using the following relation-
ship:
MDL = 3(SD)/m
where,
m = (y-i)/x = slope of the
calibration curve
x = concentration (ug/mL)
y = signal at concentration x
i = intercept of the calibration
curve
SD = standard deviation of the
noise level responses
A third study objective was to verify
that the lowest concentration levels of the
optimum range specified in the SW-846
method manual are valid. Comparison
between the samples at the lowest
concentration level and another sample at
50% that value was performed for mean
recovery, overall precision and single-
analyst precision.
Description of Study
Method Summary
In SW-846 Method 3010, 100 mL
sample is digested with 3 mL
concentrated nitric acid, evaporated
about 5 mL on a hot plate, then cor
bined with 3 mL concentrated nitric ac
and refluxed. After cooling, 1:1 hydr
chloric acid is added. The sample is thi
diluted to 100 mL with Type II water. Tl
sample is then ready for analyses f
aluminum, antimony, barium, berylliui
cadmium, calcium, chromium, coba
copper, iron, lead, magnesium, ma
ganese, molybdenum, nickel, potassiui
silver, sodium, thallium, vanadium, ai
zinc by flame atomic absorption spe
troscopy (FLAA).
Study Design
The study design was based <
Youden's non-replicate design f
collaborative evaluation of an analytic
method at several concentration leve
over its linear range. According
Youden's design, two similar yet differs
samples are analyzed in pairs such ti-
the concentration of the pairs vari
between 5 and 20 percent of the mean
the pairs. For this study, six concentrati
levels, as three Youden pairs, were us
(designated samples 1 - 6). The anal^
was directed to do a single analysis
each sample and report one value 1
each element. Analyses in reagent wa
evaluated the proficiency of the meth
on a sample free of interference
analyses in the other matrix waters we
intended to reveal the effects
interferences on the method.
The primary contractor prepared t
study samples by spiking measur
amounts of standard solutions into t
matrix waters being tested. Each spik
matrix water was then dispensed ir
replicate 120 mL bottles for distribution
participants. The analysts were instruct
to quantitatively remove a 100 mL aliqi
from each sample bottle for digestion a
analysis. A matrix blank and a qual
control sample, included in the stuc
were digested with six samples for ea
water type. Background concentrati
levels found in the matrix blanks we
subtracted from the total concentrati
found in each sample. Acceptance lirr
were provided for the quality cont
samples to verify that the analytii
system was in control. If not in conti
the problem was to be corrected a
fresh aliquots of the samples, associal
-------
with that QC sample, had to be digested
nd reanalyzed.
Spiking solutions were provided for the
MDL phase of the study. These
concentrates were used to spike aliquots
of the digested matrix waters by the
Method of Standard Additions.
Finally, an additional Youden sample
pair, designated 7-8, was included in this
study. These samples were prepared at
50% of the concentration level of
samples 5-6, which were at the lowest
concentration level of the optimum
working range specified in SW-846.
Digestion and analyses of these samples
were to proceed the same as for the
regular six samples.
Verification Analyses
To assure that the spiking solutions
were properly prepared, they were
analyzed using freshly prepared
standards before being spiked into the
test waters. A set of spiked test waters
was then digested and submitted to
QARD analysts to verify sample integrity.
These analyses confirmed the accuracy
of the distributed samples.
Selection of Test Waters
The four test waters selected for this
study were reagent water, as the control,
Ohio River Water, an electroplating
company effluent and a municipal
sewage treatment plant secondary
effluent.
Each test water was preserved, at the
time of collection, by adjusting the pH to
below 2.0. Prior to dispensing, each test
water was thoroughly mixed to ensure
homogeneity. Aliquots were removed
from each, digested according to Method
3010, then sent to QARD analysts for
Inductively Coupled Plasma Spectros-
copy analyses to determine the back-
ground concentrations of the 21
elements covered in this study.
Selection of Participating
Laboratories
The Quality Assurance Research
Division of EMSL-Cincinnati selected the
participating laboratories. As per the
standard competitive bid process, an
abstract of the scope of work was
announced in the Commerce Business
Daily. Interested laboratories were for-
warded the complete request for proposal
(RFP) which included the evaluation
criteria upon which the offerer would be
scored.
The submitted technical proposals
were evaluated based upon laboratory
experience and quality control practices.
Laboratories whose proposals were
acceptable were evaluated further in a
preaward performance evaluation study.
The participants selected for the formal
study were the nine laboratories with
acceptable proposals who performed
best in the preaward study.
Results and Discussion
The primary objective of this study was
to characterize the performance of SW-
846 Method 3010 in terms of recovery,
overall precision, single-analyst precision
and the effect of water type on recovery
and precision. The statistical results for
each of these performance
characteristics will be discussed below.
Rejection of Outliers
In this study, the IMVS program
rejected a total of 995 data points or
21.9% of the 4536 data points submitted.
Reagent water had the lowest number of
rejected data with 195. The number of
rejected data was higher for the other test
waters but did not vary significantly
among the waters. The number of
rejected data were 279 for Ohio River
Water, 258 for municipal secondary
effluent, and 263 for electroplating
effluent. For a single element, across all
water types, the number of rejected data
ranged from a low of 25 for thallium to a
high of 78 for beryllium. For purposes of
this report, an element was considered to
have excessive outliers if its total number
of rejected data was equal to or greater
than 54 (25% of the total submitted data).
Using this criterion, the following eight
elements fell into this category: aluminum
(57), beryllium (78), chromium (56),
cobalt (54), molybdenum (54), sodium
(58), vanadium (61), and zinc (72).
Laboratory 6 had the highest number of
rejected data with 234 while Laboratory 7
had the lowest number of rejected data
with 27.
Mean Recovery
The mean recoveries were calculated
for the 21 elements in each water type by
inserting the midpoint concentration of
the range studied into the mean recovery
equations given in Table 1. For reagent
water the percent recoveries for the 21
trace metals were excellent, ranging from
91% to 108%, with silver (44%) being the
only exception. For all waters, the
recoveries ranged from 94% to 109%
with barium (74%) and silver (28%) as
the exceptions.
A look at the barium recovery
estimates shows excellent results for
reagent water (97%) and Ohio River
Water (98%) but extremely poor
recoveries for the municipal secondary
effluent (60%) and the electroplating
effluent (42%). It was theorized that sulfur
oxides were present in the later waters
causing barium to precipitate as the
sulfate.
Low silver recoveries, i.e., as low as
9%, were reported in all water types. The
percent recoveries of silver in reagent
water showed acceptable recovery for the
low Youden pair samples, 98% and 96%,
with a significant decrease in percent
recovery with increasing concentrations.
This indicates a solubility problem with
silver at higher concentration levels.
Precision
The mean overall precision for all
metals, expressed as %RSDs, across
water types, ranged from 2.9% for
thallium to 13.9% for calcium with two
exceptions, barium (31.2%) and silver
(65.7%). The poor silver precision was
observed in all water types while the
barium precision was acceptable for
reagent water (13.9%) and Ohio River
Water (12.0%) and poor for the municipal
secondary effluent (31.6%) and the
electroplating effluent (67.2%). The
%RSDs in reagent water ranged from
2.6% (thallium) to 13.9% (barium) with
the exception of silver (52.6%).
The single-analyst precision for all
metals, expressed as %RSD-SRs, across
water types, ranged from 1.6% (copper)
to 7.6% (calcium) with two exceptions,
barium (15.2%) and silver (37.4%). The
poor single-analyst precision for silver
was observed in all water types while the
barium precision was acceptable for
reagent water (6.5%) and Ohio River
Water (8.4%) and poor for the municipal
secondary effluent (16.9%) and the
electroplating effluent (28.8%). The
%RSD-SRs for all elements in reagent
water ranged from 1.2% (nickel) to 8.0%
(calcium) with silver 30.9% being the
only exception.
Effects of Water Type
The recovery and precision estimates
across water types were subjected to an
analysis of variance test to determine the
effect water type had on the results. Nine
elements: calcium, cobalt, iron, man-
ganese, molybdenum, sodium, antimony,
zinc, and barium were found to have
statistically significant matrix effects that
were of practical significance when
compared to reagent water. Lead was
also found to have a statistically
significant matrix effect but this was not
considered to be of practical significance.
-------
Practical significance was determined by
a review of the retained data and judging
whether the statistically significant matrix
effects are influenced by the retention of
errant data points or non-uniform
recovery of one of the Youden sample
pairs. If no anomalies are found, the
effect was considered to be of practical
significance. The effect of water type on
analyses for silver was not evaluated
because of the poor recovery and
precision results obtained.
Method Detection Limits (MDLs)
Method detection limits (MDLs) were
experimentally determined in the four test
waters by nine participating laboratories.
The MDL for each element in reagent
water was compared with the MDLs
found in the SW-846 method manual.
This comparison showed for the
elements: barium, molybdenum, cobalt,
copper, nickel, and thallium, MDLs in this
study were 1 to 1.5 times higher than the
SW-846 MDLs. The MDLs for elements
aluminum, beryllium, calcium, iron,
magnesium, antimony, vanadium, silver,
cadmium, chromium, manganese, lead,
and zinc were 2 to 3 times higher than
the SW-846 MDLs. The MDL for
potassium was one fifth of the SW-846
MDL while the MDL for sodium was 7.5
times higher than the SW-846 MDL.
Evaluation of Lowest
Concentration Levels
The final objective of this study was to
verify that the lowest concentration levels
specified in the SW-846 method manual
are obtainable. Comparison between a
sample at the lowest specified
concentration level with another sample
at 50% of that concentration level was
performed for mean recovery, overall
precision and single-analyst precision.
The net changes in the mean recoveries
were compared in reagent water for the
21 elements. The average percent
recovery for the sample at 50%
concentration level was only 3.0% lower
than the average percent recoveries at
the lowest concentration level specified
by the SW-846 method manual. Twelve
elements: aluminum, calcium, cobalt,
chromium, copper, iron, magnesium,
sodium, nickel, lead, vanadium, and
barium had less than ± 5% net change
in percent recovery. Six elements:
beryllium, cadmium, manganese, anti-
mony, zinc, and potassium had a net
change between ± (5% - 10%). For
molybdenum and thallium, the percent
recoveries for the 50% concentration
levels were 19.6% and 16.7% lower,
respectively, than the percent recoveries
for the lowest concentration specified in
SW-846. Silver had a mean recovery
17.4% higher, for the 50% concentration
level, when compared to the specified
concentration.
The average overall %RSD for the
sample at 50% the method concentration
level was 4.9% higher than the average
overall %RSD at the lowest concentration
specified in the SW-846 method manual.
Fourteen elements: aluminum, calcium,
cobalt, chromium, copper, iron,
magnesium, molybdenum, sodium, lead,
vanadium, zinc, barium, and potassium
had a net change in %RSD of less than
± 5%. Five elements: beryllium,
cadmium, manganese, nickel, and
antimony had a net change in %RSD
between ± (5% - 10%). The overall
%RSD for silver and thallium at the 50%
concentration level was 14.0% and
26 9% respectively, higher than the
%RSDs at the lowest specified SW-846
concentration.
The average single-analyst precision
for samples at 50% the concentration
level, was 0.9% higher than the samples
at the lowest concentration level specified
in SW-846. Twelve elements: aluminum,
antimony, barium, beryllium, cadmium,
cobalt, copper, magnesium, potassium,
silver, sodium, and thallium had net
changes less than ± 5%. Seven
elements: calcium, chromium, lead,
manganese, nickel, vanadium, and zinc
had net changes between ± (5% - 10%).
For iron and molybdenum, the single-
analyst precision was 11.8% and 15.4%
higher, respectively, for the 50%
concentration level sample.
Conclusions
The primary objective of this study was
to characterize the performance of
Method 3010 in terms of recovery, overall
precision, single-analyst precision, and
the effect of water types on recovery and
precision. Through the IMVS computer
programs, statistical analyses of 4536
analytical values provided estimates of
recovery and precision expressed as
regression equations which are presented
in Table 1. These equations may be
used to predict the recovery and
precision of the 21 elements over the
range tested.
The IMVS programs rejected 995 data
points (21.9%) of the 4536 data points
submitted. The percentage of rejected
data did not vary significantly among the
water types, ranging from 20% for
reagent water to 28% for Ohio River
Water. Thallium had the fewest rejected
data with 15 while beryllium had the mo
with 78. The number of rejected data t
laboratory ranged from 27 for Lab 7
234 for Lab 6. The rejected data were n
evenly distributed among th
laboratories. Labs 3, 4, 6 and
accounted for 624 of the 995 tot
rejected data (62.7%).
Recovery estimates for the 2
elements were calculated at the midpoii
concentration of the range studied usiri
the regression equations in Table 1. Th
average percent recovery of all elemen1
across all water types were excellei
ranging from 94% to 109% with tw
exceptions, silver (28%) and bariui
(74%).
Silver recoveries were concentratio
dependent. The silver concentratio
range used in this study was 0.10 to 4.
ug/mL as recommended in the SW-84
method manual. In reagent water th
percent recoveries of the low sampl
concentration pair, 0.10 and 0.15 ug/m
were 97.8% and 95.6% respectively
However, as the concentration level
increased the percent recover
decreased dramatically to 20% at th
4.0 ug/mL concentration level. Thes
findings support the conclusions c
Hinners, EMSL-Las Vegas, as reference'
in the main report.
Barium recoveries were good ii
reagent water (97%) and Ohio Rive
Water (98%), but were poor in municipj
secondary effluent (60%) am
electroplating effluent (42%). It wa
theorized that the presence of sulfu
oxides in the later two water matrice
caused the barium to precipitate a
barium sulfate.
For all metals, the overall standart
deviations expressed as %RSD, wer<
good. Across all water types the rang*
was from 3% to 14% with the exception:
of silver (66%) and barium (31%). Thi
high silver variability was observed in al
four test waters while the barium %RSE
was high in the municipal secondary
effluent (32%) and the electroplating
effluent (67%), and low in reagent wate
(14%) and Ohio River Water (12%).
The single-analyst standard deviations
expressed as %RSD-SR, were good
Across all water types the range wa:
from 2% to 8% with the exceptions o
silver (34%) and barium (15%). The higt
silver variability was observed in all fou
test waters while the barium %RSD-SF
was high in the municipal secondary
effluent (17%) and electroplating effluen
(29%) and low in reagent water (6%) anc
Ohio River Water (8%).
Statistical comparisons were performed
on all elements to determine if there were
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Affects due to water type. The statistically
gnificant matrix effects for calcium,
jobalt, iron, manganese, molybdenum,
sodium, zinc, silver and barium were
ound to be of practical significance. The
statistically significant matrix effects were
lot considered to be of practical
significance for lead and antimony. The
silver statistics were too variable to draw
my conclusions.
Method detection limits (MDLs) were
ietermined experimentally by nine
aboratories on 21 elements in the four
est waters. In reagent water, the
ixperimental MDLs for barium,
nolybdenum, cobalt, copper, nickel, and
hallium were equivalent to the SW-846
nethod manual MDLs (1 to 1.5 times the
5W-846 MDLs). Aluminum, beryllium,
:alcium, iron, magnesium, antimony,
'anadium, silver, cadmium, chromium.
nanganese, lead, and zinc had MDLs 2
o 3 times higher than those reported in
ie SW-846 manual. Potassium was one
ifth lower and sodium was 7 5 times
ugher than the SW-846 MDLs. Except for
lOtassium and sodium, the experimen-
ally determined MDLs in this study
ipproximated the MDLs reported in SW-
46.
The analyses of the additional Youden
ample pair indicated that Method 3010
an be used to analyze elements at a
:oncentration level 50% lower than
ecommended in SW-846 with a
ecreased in recovery on the average of
1.0% and a decrease in overall and
•ingle-analyst precision on the average of
.9% and 0.9%, respectively.
Recommendations
SW-846 Method 3010 is recommended
or the analysis of aluminum, beryllium,
:alcium, cadmium, cobalt, chromium,
:opper, iron, magnesium, manganese,
nolybdenum, sodium, nickel, lead,
antimony, thallium, vanadium, zinc, and
Dotassium in wastewaters. The linear
•egression equations obtained from this
study, and presented in Table 1, can be
jsed to predict the mean recovery,
overall precision and single-analyst
Drecision of these elements at concen-
rations in the ranges investigated in this
study.
Statistical review of barium data
revealed low recovery and poor precision
(high variability) in municipal secondary
effluent and electroplating effluent but
good recovery and precision from
reagent water and Ohio River Water.
Precipitation reactions involving barium
ilfate have been hypothesized for these
.natrix effects. Analysts are cautioned to
interpret barium data carefully from any
water matrix.
The mean recovery of silver was found
to decrease significantly with increasing
concentration in the range studied (0.1 -
4.0 ug/mL). These findings, as well as
those of Hinners, suggest that further
investigation into the optimum working
range for silver analyses is recom-
mended
Table 1. Study 38, SW 846 Method 3010. Trace Metals, AA Flame Weighted Linear
Regression Equations for Mean Recovery and Precision (in
Water Type
Aluminum, Al
Beryllium, Be
Calcium, Ca
Applicable Cone. Range
Reagent Water
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 1
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 2
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 3
Single-Analyst Precision
Overall Precision
Mean Recovery
(5.00 - 50.00)
(0.04 - 2 00)
(18.00 - 120.00)
SR = 0.054X + 0.17 SR = 0.019X + 0.01 SR = 0097X - 0.87
S=0.086X-002 S=0.118X + 000 S = 0.117X - 0.02
X = 1.026C -0.29 X = 0.913C + 000 X = 1 001C + 2.12
SR = 0.02X + 0.09 SR = 0020X * 0 00 SR = 0.105X - 0.71
S = 0.071 X - 0.07 S = 0.054X -000 S = 0 200X - 2.41
X = 0.947C - 0.25 X = 0.951C +000 X = 0.938C - r.36
SR = 0021X + 0.08 SR = 0.032X + 0 00 SR = 0.018X + 2.46
S = 0026X + 037 S = 0.048X + 0.00 S = 0.122X + 1.29
X = 0.993C -032 X = 0.966C + 000 X = 1 051C + 0.97
SR = 0.024X -002 SR = 0.020X + 0 00 SR = 0.016X + 2.67
S = 0.036X + 006 S = 0.038X + 0.00 S = 0./67X -095
X = 1 019C -021 X -0.967C + 0.00 X =08940 + 228
Water Type
Cadmium, Cd
Cobalt, Co
Applicable Cone. Range
Reagent Water
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 1
Single-Analyst Precision
Overall Precis/on
Mean Recovery
Water 2
Single-Analyst Precis/on
Overall Precision
Mean Recovery
Water 3
Single-Analyst Precision
Overall Precis/on
Mean Recovery
(0 04 - 2.00)
SR = 0017X +000
S = 0 029X +000
X = 0.993C •*• 0.00
Sfl = 0.016X + 000
S = 0 034X + 000
X = 0 989C - 0 00
SR = 0.022X +000
S = 0.042X +001
X = 0.988C +000
SR = 0019X +000
S = 0 029X + 0.01
X = 1.001C + 0.00
(2.50 - 15.00)
SR = 0.032X - 0.05
S = 0 066X - 0.07
X = 0985C + 0.01
SR = 0.015X + 0.06
S = 0.086X + 0.00
X = 0.992C - 0.09
SR = 0.014X + 021
S = 0 056X + 0.20
X = 0.967C + 0.39
SR = 0.031 X -0.04
S = 0.044X + 0.08
X =0.990C - 0.05
X = Mean Recovery
C = True Value for the Concentration
Water \ = Ohio River Water
Water 2 = Municipal Secondary Effluent
Water 3 = Electroplating Effluent
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Table 1. (Continued)
Water Type
Chromium, Cr
Copper, Cu
Iron, Fe
Magnesium, Mg
Applicable Cone. Range
Reagent Water
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 1
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 2
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 3
Single-Analyst Precision
Overall Precision
Mean Recovery
(0.50 - 10.00)
SR = 0.0J9X + 0.06
S = 0.090X + 0.01
X = 1.082C - 0.03
SR = 0.030X - 0.00
S = 0.079X + 0.03
X = 1.093C + 0.02
SR = 0.027X + 0.03
S = 0.077X * 0.03
X = 1 116C-0.06
SR = 0.034X + 0.00
S = 0.088X + 0.07
X =1.077C-0.02
(0.20 - 5.00)
SR = 0.012X + 0.07
S = 0.030X + O.OT
X = 0.997C + 0.00
SR = 0.024X - 0.00
S = 0.026X + 0.01
X = 0.988C + 0.00
SR = 0.010X + 0.00
S = 0.022X + 0.0?
X = 0.993C + O.Or
SR = 0.016X -0.00
S = 0.036X + 0.01
X =0.997C + 0.00
(0.30 - 5.00)
SR = 0.010X + 0.05
S = 0.051X + 0.03
X = 0.955C + 0.01
SR = 0.031 X + 0.06
S = 0.058X + 0.10
X = 0.962C -0.12
SR = 0.002X + 0.08
S = 0.027X + 0.10
X = 0.985C - 0.05
SR = 0.026X + 0.04
S = 0.075X + 0.06
X = 7.065C - 0.75
C5.00 - 40.00)
SR = 0.022X - 0.03
S = 0.058X - 0.24
X = 7.027C - 0.02
SR = 0.009X + 0.22
S = 0.020X + 0.35
X = 1.018C - 0.10
SR = 0.072X-0.70
S = 0.059X + 0.07
X = 1 021C - 020
SR = 0.014X + 0.08
S = 0 034X - 0.00
X =1.011C - 0.03
Water Type
Manganese, Mn
Molybdenum, Md
Sodium, Na
Nickel, Ni
Applicable Cone. Range
Reagent Water
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 1
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 2
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 3
Single-Analyst Precision
Overall Precision
Mean Recovery
(0.10-3.00)
SR = 0.020X + 0.01
S = 0.030X + 0.01
X = 1.019C + 0.01
SR = 0011X + 0.00
S = 0.020X + 0.02
X = 1.008C -0.01
SR = 0.006X + 0.01
S = 0.027X + 0.07
X = 0.987C - 0.00
SR = 0.020X + 0.00
S = 0.048X + 0.00
X = 7.024C + 0.00
C7.00 - 40.00;
SR = 0.064X + 0.25
S = 0.107X + 0.22
X = 1.031C -0012
SR = 0.058X - 0.01
S = 0.111X - 0.05
X = 1.011C + 0.019
SR = 0.049X + 0.02
S = 0.143X -0.07
X = 1.051C + 0.107
SR = 0.043X + 008
S = 0.123X -0.02
X = 7.002C + 0.043
(96.00 - 600.00)
SR = 0.038X - 1.82
S = 0.068X - 0.42
X = 1 025C - O.J7
SR = 0.025X - 0.80
S = 0.038X + 0.37
X = 0.986C + 2.44
SR = 0 066X - 2.56
S = 0.066X + 2.03
X = 0.991C- 1.80
SR = 0050X •*• 0.74
S = 0.033X + 11 92
X = 0.988C-8.97
(0.30- 5.00;
SR = 0.004X + 0.02
S = 0.029X + 0.03
X = 0.997C - 0.07
SR = 0075X + 0.01
S = 0.051X - 0.00
X = 0 997C - 0.07
SR = 0 026X + 0.03
S = 0 032X + 0.05
X = 1.020C - 0.02
SR = 0.008X + 0.04
S = 0 034X + 002
X =1 011C - 0.01
X = Mean Recovery
C = True Value for the Concentration
Water 1 = Ohio River Water
Water 2 = Municipal Secondary Effluent
Water 3 = Electroplating Effluent
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Table 1. (Continued)
Water Type
Lead, Pb
Antimony, Sb
Thallium, Ti
Vanadium, V
Applicable Cone. Range
Reagent Water
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 1
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 2
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 3
Single-Analyst Precision
Overall Precision
Mean Recovery
Reagent Water
Single-Analyst Precis/on
Overall Precision
Mean Recovery
Water 1
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 2
Single-Analyst Precision
Overall Precision
Mean Recovery
Water 3
Single-Analyst Precision
Overall Precision
Mean Recovery
(0.80 - 20.00)
SR = O.OT8X + 0.03
S = 0.079X + 0.09
X = 7.037C -0.02
SR = 0.028X + 0.05
S = 0.047X + 0.07
X = 7.023C + 0.04
SR = 0.030X + O.OT
S = 0.046X + 0.05
X = 1 046C - 0.08
SR = 0.047X - 0.02
S = 0.082X - 0.04
X =0976C + 0.03
(1.20 - 40.00)
SR = 0.023X + 0.19
S = 0.044X + 0.20
X = 1.057C-0.25
SR = 0.03TX + 0.70
S = 0066X + 0.72
X = 7.055C - 0.22
Sfl = 0.077X + 0 74
S = 0 039X + 0.79
X = 1.049C -0.11
SR = 0.003X + 007
S = 0.006X + 0.19
X = 1.050C + 0.01
(1.00 - 20.00)
SR = 0.009X + 0.07
S = 0.021X + 0.05
X = 7.039C - 0.03
SR = 0.079X + 0.05
S = 0.033X + 0.05
X = T.028C - 0.04
SR = 0.076X + 0.01
S = 0.017X + 0.06
X = 1.028C -0.03
SR = 0.073X + 005
S = 0 024X + 0.05
X =1.032C -001
(2.25 - 99.00)
SR = 0.064X + 0.15
S = 0.109X -0.02
X = 1.047C + 0.003
SR = 0.045X - 0 06
S = 0.099X -0.72
X = 1 052C + 0.06
SR = 0.027X + 0.01
S = 0.128X-0.14
X = 1.056C - 0.08
SR = 0.011X + 0.03
S = 0.079X - 0.04
X = 1.055C * 0.03
Water Type Zinc, Zn
Applicable Cone. Range (0.10 - 1.00)
Silver, Ag Barium, Ba Potassium, K
(0.10- 4.00) (1.00 - 20.00) (4.80 - 30.00)
SR = -0.009X + 0.01
S = 0.035X + 0.01
X = 0.984C + 0.01
SR = 0.039X + 0.02
S = 0.067X + 0.02
X = 0 983C - 0.06
SR = -0.022X + 0.05
S = -0 007X + 006
X = 0.959C +002
SR = 0.02 7 X + 0.02
S = 0 026X + 0.02
X = 0 953C + 0.00
SR = 0.343X - 0.03
S = 0.583X - 0.05
X = 0.402C * 0.07
SR = 0.221X - 0.00
S = 0 765X - 0.04
X = 0 172C + 0.07
SR = 0.368X-003
S = 0.607X -005
X = 0345C + 006
SR = 0.979X -006
S = 0.956X -007
X =0 058C + 0.06
SR = 0 067X - 0.02
S = 0 742X - 003
X = 0967C +005
SR = 0 089X - 0.05
S = 0.127X -0.07
X = 0970C + 0.07
SR = 0.197X -0.17
S = 0361X -027
X = 0.536C + 0.64
SR = 0389X -0.42
S = 0.874X - 0.84
X =0.329C + 0.86
SR = 0.072X + 0.38
S = 0.080X + 0.02
X = 0923C+ 0.75
SR = 0.069X + 0.00
S = 0.113X -0.70
X = 0.976C + 0.01
SR = 0.055X + 0.78
S = 0.707X + 0.07
X = 0.927C + 0.37
SR = 0.032X + 0.36
S = 0.052X + 0.45
X = 0.961C -0.06
X = Mean Recovery
C = True Value for the Concentration
Water ; = Ohio River Water
Water 2 = Municipal Secondary Effluent
Water 3 = Electroplating Effluent
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K. W. Edgell and 0. M. Withers are with The Bionetics Corporation, Cincinnati,
OH 45246
Edward L Berg is the EPA Protect Officer (see below).
The complete report, entitled "USEPA Method Study 38 SW-846 Method 3010
Acid Digestion of Aqueous Samples and Extracts for Total Metals for
Analysis by Flame Atomic Absorption Spectroscopy," (Order No. PB 89-
181 945/AS; Cost: $21.95, subject to change) will be available only from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA 22161
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Environmental Monitoring Systems Laboratory
U.S. Environmental Protection Agency
Cincinnati, OH 45268
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
BULK RATE
POSTAGE & FEES PAID
EPA
PERMIT No. G-35
Official Business
Penalty for Private Use $300
EPA/600/S4-89/011
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