EPA-680/4-73-001-5
February 1974
ENVIRONMENTAL RADIOACTIVITY
LABORATORY INTERCOMPARISON STUDIES PROGRAM
1973 - 1974
by
Quality Assurance Branch
Technical Support Laboratory
National Environmental Research Center
Las Vegas, Nevada
ROAP Number 22ADB
Program Element 1HA327
NATIONAL ENVIRONMENTAL RESEARCH CENTER
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
LAS VEGAS, NEVADA 89114
For sale by the Superintendent of Documents, U.S'. froVernment Printing Office, Washington, D.C. 20402 - Price 65 ewits
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PREFACE
Quality assurance is an integral part of any viable environ-
mental monitoring activity. The primary goals of the Environmental
Protection Agency's (EPA) quality assurance program are to improve
and document the credibility of environmental measurements. To
achieve these goals, quality assurance is needed in nearly all seg-
ments of monitoring activities and should cover personnel, methods
selection, equipment, and data handling procedures.
Five major functions, each essential to an effective quality
assurance effort, comprise EPA's quality assurance program:
Promulgation of standardized methods of
measurement
Distribution of standard reference materials
Issuance of guidelines and procedures
Training and technical assistance
Evaluation and certification of monitoring
activities
This manual has been prepared to assist laboratories involved
with environmental radiation measurements in developing and maintain-
ing a quality control program and documenting the precision and
accuracy of their data. All EPA monitoring programs are requested
to make use of this document in planning their own radiation measure-
ments and in assisting the States in carrying out radiation monitoring
activities.
Comments concerning the utility of this document, along with any
suggestions for possible changes and revisions, are welcomed. Questic
on matters related to quality assurance of environmental measurements
in various field should be directed to the following person(s):
Air Pollution
Mr. Seymour Hochheiser, Chief
Quality Control Branch
Quality Assurance and Environmental
Monitoring Laboratory
National Environmental Research Center
Research Triangle Park, North Carolina 27711
ii
-------
Hater
Mr. Dwight Ballinger, Director
Methods Development and Quality Assurance
Research Laboratory
National Environmental Research Center
Cincinnati, Ohio 45268
Pesticides
Dr. M. T. Shafik, Acting Chief
Chemistry Branch
Primate and Pesticides Effects Laboratory
National Environmental Research Center
Research Triangle Park, North Carolina 27711
Radiation
Mr. Arthur N. Jarvis, Chief
Quality Assurance Branch
National Environmental Research Center
Las Vegas, Nevada 89114
During the months ahead, manuals and docoments will be issued
which provide guidelines to be followed in all phases of monitoring
activitiessampling, analysis, and data handlingand in all media;
air, water, and land. Use of these guidelines throughout the Agency
will enable a uniform approach to be established within EPA which
ultimately can be implemented at the State level. This should permit
a significant improvement in the validity and reliability of environ-
mental data which the Nation collects.
The implementation of a total and meaningful national environ-
mental quality assurance effort cannot succeed without the full
support of all monitoring programs. Your cooperation is appreciated.
ill
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TABLE OF CONTENTS
Preface ----------____ -j
I.
II.
III.
IV.
\/
i au i c \j i ounuciiu- -- - _____
The Laboratory Intercomparison Studies Program
Types of Environmental Samples Distributed - -
final \/c-ic n-f Hata _ - _ -
Participation in the Laboratory Intercomparison
- lit
1
- 3
7
14
1C
Request Forms
IV
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I. THE LABORATORY INTERCOMPARISON STUDIES PROGRAM
Environmental measurements for radiation are made daily by
many different Federal, State, local and private agencies. The data
from these measurements are used for a wide variety of purposes,
including health effects, the establishment of standards and guides,
and for enforcement activities. It is therefore imperative that
the precision and accuracy of the data be assured in order that
policy decisions concerning environmental quality are based upon
valid and comparable data.
In order to attain this goal, an Agency-wide quality assur-
ance program has been implemented within the U.S. Environmental
Protection Agency (EPA). In the area of radiation, quality control
responsibilities have been assigned to the Quality Assurance Branch
at the EPA's National Environmental Research Center-Las Vegas which
carries out a program designed to encourage the development and
implementation of quality control laboratory procedures for sample
collection, analysis, data handling, and reporting purposes.
A major objective of this program is to assist laboratories
involved in environmental radiation measurements to develop and main-
tain both an intralaboratory and an inter!aboratory quality control
program. In part, this is accomplished through an extensive labora-
tory intercomparison study ("cross-check") program involving environ-
mental media (milk, water, air, food, soil and gases) and a variety
of radionuclides with activities at or near environmental levels.
A number of different environmental samples, containing pre-
cisely known amounts of one or more radionuclides, are prepared and
routinely distributed to all laboratories requesting them. These
laboratories perform the required analyses and return their data to
-------
the Quality Assurance Branch for statistical analysis and compari-
son with other participating laboratories. A computer report and
a continually updated performance chart are returned to each par-
ticipant. The program thus enables a laboratory to document the
precision and,accuracy of radiation data, identify instrumental
and procedural problems, and to compare performance with other
laboratories.
Each laboratory participating in a cross-check study is ex-
pected to have an internal quality control program in operation to
insure that all instrumentation is calibrated and functioning and
that analytical procedures are being carried out properly. Such a
program includes continual monitoring of instrumentation, the plot-
ting of instrument control charts, frequent analysis of replicate
samples to check precision, and the regular measurement of samples
to which known amounts of activity have been added, to check the
accuracy of systems.
Participation in a laboratory intercomparison does not auto-
matically guarantee the precision and accuracy of a laboratory's
data and should not be considered as a substitute for a continuous
quality control program within a laboratory. However, intercom-
parison data may be useful either for indicating previously unsus-
pected instrumental problems or procedural deficiencies, or for
documenting the precision, accuracy and validity of a laboratory's
work. Participation in a laboratory intercomparison study program
thus serves as a check on the' internal quality control program.
If your laboratory does not now participate in the cross-
check activities of the Quality Assurance Branch at the NERC-LV,
or if you wish to expand its participation, you are encouraged to
do so.
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II. TYPES OF ENVIRONMENTAL SAMPLES DISTRIBUTED
The current laboratory intercomparison studies program in-
volves the analysis of a variety of media containing environmental,
or near environmental, levels of radioactivity. These include:
MILK
Four-liter milk samples containing 40K, 89Sr, 90Sr, 131I,
137Cs, and 140Ba are distributed on a monthly basis.
WATER
Water containing several different mixtures of radioactive
materials are included in the cross-check program.
Four-liter samples for the analysis of gross alpha
and gross beta analysis are sent to participating
laboratories every other month.
Four-liter samples containing 51Cr, 63Zn, 60Co,
106Ru, 134Cs, and 137Cs for gamma analysis are
distributed every other month.
Sixty-milliliter samples for tritium analysis, are
mailed on a monthly basis.
Four-liter water samples containing 239Pu are
shipped to laboratories during May and November
of each year.
Four-liter samples of well water containing 226Ra
are distributed in November, January, May and July.
-------
AIR
Air filters, with optional 2-inch or 4-inch
diameters, are sent out on a quarterly basis for
gross alpha, gross beta, and 239Pu analysis.
SOIL
One-hundred-gram soil samples, containing 239Pu,
will be distributed twice each year beginning in
December 1973.
FOOD
Three 4-liter food slurries containing 89Sr, 90Sr,
131I, 137Cs, 140Ba, and K are sent to participants
once each quarter.
URINE
Urine samples (60 ml) containing tritium are
shipped on a quarterly basis.
GASES
Cylinders containing either 85Kr or 133Xe are dis-
tributed twice each year.
Sample size, activity levels, type of analysis, and other
pertinent information concerning the cross-check samples are summa-
rized in Table 1. The distribution schedule is outlined in Table 2,
A laboratory may participate in as few or as many of the
studies as it desires.
-------
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III. ANALYSIS OF DATA
Each participating laboratory is expected to carry out three
independent determinations for each radionuclide included in a par-
ticular cross-check and to report its results on a form (Figure 1)
provided with the sample.
Upon receipt of the reports from all participating labora-
tories, the data are transferred to punch cards and introduced into
a CDC 6400 computer for analysis. As indicated in the sample cal-
culations (Appendix I), this analysis includes determination of the
experimental standard deviation, calculation of the normalized
range, normalized deviation, experimental error, and the grand
average of all laboratories. The expected analytical precision
values used as a basis for judging laboratory performance for spe-
cific nuclides are summarized in Table 3.
A report is generated containing the data reported by all
participating laboratories, listed according to their identity code,
along with the results of the computer analysis (Table 4, Figure 2).
In addition., a control chart is generated and reproduced for each
radionuclide included in the sample (Figures 3 and 4). The control
charts are updated each time a laboratory participates in a par-
ticular cross-check study, thus giving each laboratory a continuous
record of its performance.
A copy of the computer printout and a control chart for each
radionuclide is mailed to each participant approximately 2 weeks
following the report due date.
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\ U.S. ENVIRONMENTAL PROTECTION AGENCY
g ^^f^7 $ NATIONAL ENVIRONMENTAL RESEARCH CENTER
\^**^g LAS VEGAS, NEVADA
% *X
QUALITY ASSURANCE BRANCH
Laboratory ID
Contact Person Phone
Sample Type Tritium in Water
Collection Date 8-10-73 0400 PST
Analysis #1
Analysis #2
Analysis #3
NOTE: All results are in pCi/1 with background
subtracted. Total activity is less than
3500 pCi/1 3H.
Please send your results no later than September 17, 1973* to:
U.S. Environmental Protection Agency
National Environmental Research Center
Quality Assurance Branch
P.O. Box 15027
Las Vegas, NV 89114
*Results not received by this date will not be included in final report,
Figure 1. Results reporting form
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Table 3
Laboratory Precision
One Standard Deviation Values
For Various Analyses
Nuclide
131
137Cs
89Sr
9°Sr
K
Ca
Gross Alpha
Gross Beta
3H
226Ra
239Pu
Level
5 to 100 pCi/1 or Kg
> 100 pCi/1 or Kg
5 to 100 pCi/1 or Kg
> 100 pCi/1 or Kg
5 to 100 pCi/1 or Kg
> 100 pCi/1 or Kg
5 to 100 pCi/1 or Kg
> 100 pCi/1 or Kg
2 to 30 pCi/1 or Kg
> 30 pCi/1 or Kg
>_ 0.1 g/1 or Kg
>_ 0.1 g/1 or Kg
>_ 1 pCi/1
1 to 25 pCi/1
> 25 to 130 pCi/1
> 130
< 4000 pCi/1
> 4000 pCi/1
>_ 0.1 pCi/1
Standard Deviation
Single Determination
5 pCi/1
5%
5 pCi/1
5%
5 pCi/1
5%
5 pCi/1
5%
1.5 pCi/1
5%
0.06 g/1
0.02 g/1 or Kg
25%
25%
6.5 pCi/1
5%
% Is = 16985x(pCi/l)--9067
10%
15%
pCi/1, gram or sample 10%
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Title:
Column 1:,
Column 2:
Column 3:
Columns 4
& 5:
Program name, sample collection date, sample code
letter, analysis type, known concentration of radio-
nuclide, expected standard deviation of analysis -
single determination.
Laboratory identification code (A, B, C, etc.).
Laboratory results (0-25 results listed down column) .
1 s (standard deviation) of the experimental results.
Normalized Range Value in "Mean Range + Standard Error
of the Range" (R + OR) units for comparability. (See
Statistical Techniques for Quality Control of Environ-
mental Radioassay, AQCS Report Stat-1, November 1964,
pp 4-8) (SR = OR for printing purposes).
Column 6 : Average Value.
Column 7 : Normalized Deviation from the Grand Average Value of
all laboratories expressed in a^ units.
Column 8: Normalized Deviation from the Known Value expressed in
cfy units.
Bottom of Is experimental error of all laboratories and the
Chart: Grand Average of all laboratories.
Figure 2. Explanation of terms used in participant date report
10
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Table 4. SAMPLE ANALYSIS AND REPORT OF PARTICIPANT'S DATA
NFRC-LV TRlTlL. IN '.«!ATPR CROSSCHECK PROGR'
12/27/72 SA"PLE - A
1579.00 +/-
S
LAB
0
0
0
p
D
p
4G
AG
AG
AH
AM
AH
AI
AI
AI
1500.0
1400.0
1^00.0
187?. 0
1688.0
1596.0
1^30.0
1810.0
1740.0
1626.0
1477.0
16b?.0
2011.0
1713.0
2473.0
SIGMA
57.74
140.53
47.26
94.43
382.94
MO OATA
R +
R
.18 + 0
.49 + 0
.16 + 0
.31 + 0
1 + .41
PCI/L
NORMALIZEO DEVIATION
-------
Title:
Name of Program, Laboratory Code Letter, and Type
of Analysis.
Upper Graph:
"Normalized Deviation from Known versus the Month
of Analysis." (The 95.0% (y ± 2oM) and the 99.7%
(p ± 30^) Confidence Levels were chosen as the
Warning Levels and Control Limits respectively.)
Middle Graph:
"Normalized Deviation from the Grand Average Value
of All Laboratories versus the Month of Analysis."
(The 95.0% (x ± 2aM) and the 99.7% (x ± 3aM)
Confidence Levels were chosen as the Warning Levels
and Control Limits respectively.)
Lower Graph:
"Normalized Range Values_(R + OR) versus the_Month of
Analysis." (The 97.5% (R + 2oR) and -100% (R + 3oR)
Confidence Levels were chosen as the Warning Levels
and Control Limits respectively.)
Figure 3. Explanation of terms used in the control chart
12
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TRITIUM IN WATER CROSS CHECK PROGRAM
LAB-D 3H
NORMALIZED DEVIATION FROM KNOWN
4
3
2
| o
4
3
2
5
(D 0
1971
X N A -'
V V
1972
.
' \ A^ f^^**\
v \/ \^
CL
WL
WL
PI
JFMAMJJASONDJFMAMJJASOND
NORMALIZED DEVIATION FROM GRAND AVERAGE
1971
«,
Y
1972
x^ ^-*^^^
v^ ^N^
>
CL
WL
WL
CL
JFMAMJJASONDJFMAMJJASOND
NORMALIZED RANGE
R + 3
R + 2
R + 1
T O
1971
. _ . . 1 1 1 .
1972
1 i. .1.1 1 _ .
CL
WL
JFMAMJJASONDJFMAMJJASOND
Figure 4. Control chart
13
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IV. PARTICIPATION IN THE LABORATORY INTERCOMPARISON STUDIES
PROGRAM
Any laboratory involved in, or concerned with, environmental
radiation monitoring and surveillance, is eligible to participate
in any one or all of the cross-checks described. Moreover, depend-
ent upon personnel available and their workload, a laboratory may
elect to receive samples on a less frequent basis than indicated on
the distribution schedule (Table 2).
To become a participant in the laboratory intercomparison
studies program, complete one of the forms included in this publi-
cation and return to:
U.S. Environmental Protection Agency
National Environmental Research Center
Quality Assurance Branch
P.O. Box 15027
Las Vegas, NV 89114
Should the laboratory require additional types of cross-check
samples at some later date, a second formindicating the samples
desiredshould be submitted.
14
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V. APPENDIX
Statistical Calculations
To illustrate the computations performed by computer, sample calcu-
lations are given using data for three hypothetical samples analyzed at
one laboratory.
First, the analytical results are listed and the mean (sample calcu-
lation a) and the standard deviation (sample calculation b) are computed.
These statistics provide measures of the central tendency and dispersion
of the data. In our example the mean, X , equals 60 pCi/1 and the
standard deviation, S , equals 10 pCi/1-
Next, the normalized range (sample calculation c) is computed by
first finding the mean range, R , the control limit, CL , and the
standard error of the range, OR . The normalized range measures the
dispersion of the data (precision) in such a form that control charts
may be used. Control charts allow one to readily compare past analytical
performance with present performance. In the example, the normalized
range equals 1R + 2.600R which falls between the upper warning level,
R~ + 2oD , and the upper control limit, R + 3on . The precision of the
K K
results may be suspect.
The normalized deviation is calculated (sample calculation d) by
computing the deviation and the standard error of the mean, a . The
normalized deviation allows one to readily measure central tendency
(accuracy) through the use of control charts. Trends in analytical
accuracy can be determined in this manner. For this example, the
normalized deviation is +0.693 which falls between the upper and lower
warning levels. The accuracy of the data is acceptable.
Finally, the experimental error of all laboratories, the grand
average, and the normalized deviation from the grand average are
calculated in order to ascertain the performance of all the laboratories
as a group. Any bias in methodology or instrumentation may be found
from these results. Since the results of only one laboratory are listed
in the Appendix, the equations are shown without any sample calculations.
15
-------
Sample Calculations
a. Analysis Data:
Known value = 62 pCi/1
Standard deviation (single determination) = 5 pCi/1
Sample No.
1
2
3
Activity pCi/1
50
60
70
Number of samples (N) = 3
x. = 180 pCi/1
X = 60 pCi/1
b. Experimental Standard Deviation (S)
(I
S =
N - 1
S =
I50L+60
S = 10 pCi/1
16
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c. Calculation of Normalized Range
Step 1. Mean Range (R)
R = 6-20 Where d2 = Central line factor*
R = (1.693)(5 pCi/1) d2 = 1.693* for N = 3
R = 8.465 pCi/1 a = Standard deviation
(single determination)
Step 2. Control Limit (CL)
CL = R + 3aR Where D^ = Control Limit factor*
= Diji Dk = 2.575
= (2.575)(8.465 pCi/1)
= 21.797 pCi/1
Step 3. Standard Error of the Range (OR)
aR = 1/3 (R + 3oR - R)
= 1/3 (D^R - R)
= 21.797 pCi/1 - 8.465 pCi/1
3
= 4.444 pCi/1
* Rosenstein, M. and A. S. Goldin, Statistical Techniques for
Quality Control of Environmental Radioassay, AQCS Report Stat-1.
U.S. Department of Health, Education and Welfare, PHS, Nov. 1964
17
-------
Step 4. Normalized Range (Range expressed in terms of R and OR)
Where w = # of R and x = # of OR defining R
If R > R let w = 1 and solve for x
If R <_ R let x = 0 and solve for w
Since, in this example, R > R (i.e., 20 > 8.465)
let w = 1 and solve for x
R = wR + xaR
R - wR
x =
°R
20 - (1)(8.465)
x 4.444
x = 2.598
Normalized Range = 1R + 2.598aR
d. Calculation of the Normalized Deviation
1. Deviation = True Value - X
= 62 pCi/1 - 60 pCi/1
= 2 pCi/1
18
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2. Standard Error of the Mean (am)
Jm ,
V N
_ 5 pCi/1
°m =
3
am = 2.887 pCi/1
XT i j rv Deviation
3. Normalized Deviation =
2 pCi/1
2.887 pCi/1
= 0.693
e. Experimental Error = (x.2) - ^ Xi)
(All labs) N
N-l
Where x-^ are the "1, 2, 3, ...i" results and N equals the
number of results in the calculation.
f . Grand Average = ri where x^ and N are defined as in "e" above.
g. The Normalized Deviation from the Grand Average is calculated as
in "d" except the Grand Average value is used instead of the
Known Value.
19
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
W-T6§8/4-73-001-b
3. RECIPIENT'S ACCESSION-NO.
|4. TITLE ANDSUBTITLE
Environmental Radioactivity Laboratory Intercomparison
Studies Program, 1973-1974
REPORT. DATE . .
December 1973 (preparation)
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Quality Assurance Branch
Technical Support Laboratory
8. PERFORMING ORGANIZATION REPORT NO.
n/a
Ig. PERFORMING ORGANIZATION NAME AND ADDRESS
National Environmental Research Center
U.S. Environmental Protection Agency
P. 0. Box 15027
Las Vegas, NV 89114
10. PROGRAM ELEMENT NO.
1HA327
11. CONTRACT/GRANT NO.
in-house report
12. SPONSORING AGENCY NAME AND ADDRESS
Office of Research and Development
U.S. Environmental Protection Agency
Washington, DC 20460
13. TYPE OF REPORT AND PERIOD COVERED
interim (]973-19741
14. SPONSORING AGENCY CO6E
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The U.S. Environmental Protection Agency's intercomparison studies program for
laboratories involved in environmental radiation measurements is described. The
types of environmental samples distributed, the analysis required for each sample,
the distribution schedule, and the statistical analysis anci reporting of results
are discussed. Instructions and application forms are included for laboratories
desiring to participate in the program.
This document is not a research report. It is designed for use by laboratories
participating or desiring to participate in this quality assurance program.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
quality assurance
quality control
quantitative analysis
radioactivity
statistical quality control
07 05/14 04
13. DISTRIBUTION STATEMENT
Release unlimited
(NERC-LV, NTIS)
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
20. SECURITY CLASS (Thispage)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
-------
INSTRUCTIONS
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