EPA-680/4-75-007
JUNE 1975
                                         Environmental Monitoring Series
                            PRELIMINARY MILK REPORT
                                    NATIONAL ENVIRONMENTAL RESEARCH CENTER
                                       OFFICE OF RESEARCH AND DEVELOPMENT
                                      U.S. ENVIRONMENTAL PROTECTION AGENCY
                                                 LAS VEGAS, NEVADA 89114

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              RESEARCH REPORTING SERIES
Research reports of the Office of Research and Develop-
ment, U. S.  Environmental Protection Agency,  have  been
grouped into five series.   These  five broad categories
were established  to  facilitate further development and
application of environmental technology.  Elimination of
traditional  grouping  was consciously planned to foster
technology transfer and  a  maximum interface in related
fields.  The five series are:

    1.  Environmental Health Effects Research
    2.  Environmental Protection Technology
    3.  Ecological Research
    4.  Environmental Monitoring
    5.  Socioeconomic Environmental Studies
This report has been assigned to the ENVIRONMENTAL MONI-
TORING series.  This series describes research conducted
to develop new or improved methods  and  instrumentation
for  the  identification and quantification  of  environ-
mental pollutants at the lowest conceivable significant
concentrations.   It  also includes studies to determine
the ambient concentrations of pollutants in the environ-
ment and/or the variance of pollutants as a function of
time or meteorological factors.
                  EPA REVIEW NOTICE

This report has been reviewed by the  National  Environ-
mental Research Center-Las Vegas, EPA, and approved for
publication.  Approval does not signify that the contents
necessarily reflect the views  and  policies of the U.S.
Environmental  Protection  Agency,  nor does  mention  of
trade  names or commercial products constitute endorse-
ment or recommendation of use.
Document is available  to  the  public  for  sale  through
the National Technical Information Service, Springfield,
Virginia 22161.

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                                   EPA-680/4-75-007
                                   June 1975
        PRELIMINARY MILK REPORT
                  by

Arthur N. Jarvis and David G.  Easterly
       Quality Assurance Branch
     Technical Support Laboratory
National Environmental Research Center
          Las Vegas, Nevada
           ROAP 21BEK/22AAJ
        Program Element 1HA327
NATIONAL ENVIRONMENTAL RESEARCH CENTER
  OFFICE OF RESEARCH AND DEVELOPMENT
 U.S. ENVIRONMENTAL PROTECTION AGENCY
       LAS VEGAS, NEVADA  89114

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                               ABSTRACT

      A summary of the results of the milk cross-check  program  from
July 1973 through November 1974 is given.   These data indicate  a  need
for improvement in the laboratory analysis of both  beta and  gamma-
emitting radionuclides in milk,   Also, the expected relationship, i.e.,
with increasing sample activity the accuracy of the analysis should
improve, was not seen with any consistency at the levels of  activity
used in these studies.  Accurate analysis  of strontium-89 was particu-
larly difficult for most laboratories to achieve, while the  accurate
analysis of cesium-137 was the least difficult.
     These results exemplify the need for improvement in analytical
procedures through the adoption of standard reference methods,  more
frequent calibration and maintenance of counting instruments, improved
quality control practices within each laboratory, and greater partici-
pation in laboratory intercomparison studies conducted  by the National
Bureau of Standards, the Energy Research and Development Administration,
and the U.S. Environmental Protection Agency.
                                   iii

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                             CONTENTS
                                                               Page
Abstract	•  H*
List of Tables and Figures 	    v

Introduction 	    *
Methods and Procedures 	    2
Results and Discussion 	    3
Summary  	    6
References	    31
APPENDIX.   Statistical Calculations  	    32
                                  1v

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                                TABLES
Number                                                            Page
   1   Summary of Cross-Check Programs 	  ...     8
   2   Summary of Milk Analysis Data, July 1973 to
       November 1974	     9
   3   Limits Established by the Analytical  Quality
       Control Service 	    12
   4   Results of Milk Cross-Check Analyses, July 1973
       to November 1974	    12
                               FIGURES
Number                                                            Page
   1   Sample Analysis and Report of Participant's Data  ....   13
   2   Control Chart 	   15
  3-A  Histogram of Monthly Analysis for Strontium-89  	   17
  3-B  Histogram of Monthly Analysis for Stront1um-90  	   20
  3-C  Histogram of Monthly Analysis for Sarium-140  	   23
  3-D  Histogram of Monthly Analysis for Iodine-131  	   25
  3-E  Histogram of Monthly Analysis for Cesium-137  	   28

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                     PRELIMINARY  MILK REPORT

INTRODUCTION

     Environmental  radiation measurements  are made  daily  by  federal,
state,  local, and private agencies.   The data obtained  from  these
measurements are utilized by the  U.S.  Environmental  Protection Agency
(EPA) and other agencies for such purposes as estimating  dose and
health effects, establishing standards and guides,  and  conducting
regulatory activities.   It is therefore imperative  that the  precision
and accuracy of the data be assured so that policy  decisions concerning
environmental quality are based on valid and comparable data.
     The present radiation quality assurance program of the  EPA  is
designed to encourage the development and  implementation of  quality
control procedures at all levels of sample collection,  analysis, data
processing, and reporting.  As an integral part of the EPA's program,
the Quality Assurance Branch of the National Environmental Research
Center-Las Vegas (NERC-LV) distributes calibrated radionuclide solutions
for  instrument calibration and chemical yield determinations, and con-
ducts a number of laboratory performance studies involving the analysis
of radionuclides in environmental media.
     The intercomparison  studies program enables participating labora-
tories to maintain checks on their analyses  and assists  them in docu-
menting the  validity of  their data.   In addition, this program enables
the  EPA to obtain an overall estimate of  the precision and  accuracy of
environmental  radiation  measurements,  or more precisely  the precision
and  accuracy of  laboratory  radioassay procedures of environmental
samples.

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      Studies  currently  in  progress  involve  samples of most environmental
 media and  include milk,  air, water,  soil, diet, urine, and noble gases.
 Table 1  is  a  summary of  the cross-check  programs.  Participants include
 nuclear  facilities  or their contractors, state, federal, and inter-
 national laboratories.   The number  of participants has increased
 steadily during  the past two years.  Because of the large number of
 participants  and the continuing nature of the programs, sufficient
 data  are generated  to enable valid  periodic statistical assessment
 of  the quality of environmental data.
      Laboratories perform  the analyses and  return their data to the
 Quality  Assurance Branch for statistical analysis.  Comparisons are
 made  between  laboratories  and within an  individual laboratory for
 accuracy and  precision.  A computer  report  and a periodically updated
 performance chart are returned to each participant.  This enables each
 laboratory to document the precision and accuracy of its radiation
 data,  to identify instrumental and procedural problems, and to compare
 performance with other laboratories.

 METHODS  AND PROCEDURES

     Through December 1973, reconstituted powdered milk was used in the
 milk cross-check program.  Two modifications were made to the program
 beginning 1n  1974:  (1)  fresh, whole, pasteurized, homogenized milk
 was used in preparing the  samples, and (2) sample distribution was
 changed  from monthly to  a  bimonthly basis.
     The milk was prepared for distribution by thoroughly mixing with
 10 ml/gallon of  formalin and 3.79 ml/gallon of antifoaming agent
 (Dow Corning Antifoam,R  FG-10 Emulsion, Food Grade).  Three aliquots
were gamma counted  for background determination.  The remaining milk
was "spiked" using  calibrated solutions of the radionuclides.  The milk
was again thoroughly mixed and three aliquots taken for gamma analysis.
 If these results Indicated homogeneity, the milk was packaged for

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 shipment.  A 4-liter  sample containing strontium-89, strontium-90,
 cesium-137, iodine-131, and barium-140 was distributed to each of
 approximately 35 participating laboratories.
     Each participating laboratory made three independent determinations
 for each radionuclide included in the particular cross-check sample and
 reported its results  to the Quality Assurance Branch.  Control limits
 (sigma limits) previously established by the Analytical Quality Control
 Service in Winchester, Massachusetts, were used in analyzing the quality
 of the results obtained by these laboratories (1,2).  These limits were
 based on the purpose  for which the data were being obtained and on
 reasonable laboratory ability.  Upon receipt of the reports from all
 participating laboratories, the data were transferred to punch cards
 and analyzed using a CDC 6400 computer.  This analysis included determi-
 nation of the experimental average and standard deviation of the sample,
 the normalized range, standard error normalized deviation, experimental
 sigma, and the grand average of all laboratories for each radionuclide.
 Examples of sample calculations to illustrate the computations per-
 formed by the computer are shown in the appendix.
     A report was generated containing the data reported by all par-
 ticipating laboratories, listed according to their identity code, along
with the results of the data analysis.  Examples are shown in Figure 1.
 In addition, a control chart was generated for each radionuclide in-
 cluded in the sample  (Figure 2).  The control charts are updated each
 time a laboratory participates in a 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 radio-
nuclide is mailed to each participant approximately two weeks following
the report due date.

RESULTS AND DISCUSSION

     A summary of the results of the milk analysis data is shown in
Table 2.   All  participants received samples containing strontium-89,

                                   3

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 strontium-90, cesium-137, iodine-131, and barium-140;  however,  all  did
 not submit results for each analysis.  This  resulted  in  a  different
 number, N, being reported for the various radionuclides.
      A comparison may be made between the experimental standard  devia-
 tion, s, calculated from the data supplied by  the  participating  labora-
 tories (Table 2) and the standard deviation, a,  expected for  various
 analyses listed  in Table 3.
      For the purpose of  comparison,  the  experimental  [(s/known)100] and
 expected [(a/known)100]  standard  deviations, expressed as  a percent of
 the known values,  are shown  for each  month in  Table 2.  The experimental
 standard deviation divided by  the known  value  (s/p) indicates no im-
 provement in  the analytical  results when whole milk was used  instead
 of powdered.
      Figure 3-A  shows  the results  in  the form of a histogram for the
 strontium-89 analysis  by month.*   The February results were the poorest
 over  the  period  for which strontium-89 data were analyzed.   When com-
 paring  the grand average  (X) to the known  value (u), a negative bias
 was observed for all monthly samples except February.   No explanation
 for either the negative bias or the poor analytical performance by the
 participating laboratories is readily apparent.  It is now  necessary
 to determine if this is due to the analytical  method(s) being  used and
 if so if a different method of analysis or modification of  the existing
 method(s) is warranted.
     The monthly results  of the strontium-90  analysis  are shown in
 Figure 3-B.  On an average the (s/y)  values were lower and  the devia-
tions from y were less than for strontium-89  analysis.   Even though
the results show some inconsistency from month  to month,  in general
they may be viewed with some optimism since data for at least  one
*  For all data used in this report, Chauvenet's criterion was used as
the basis for acceptance or rejection of the X value of each laboratory.

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month are sufficiently accurate to indicate  good  results are attainable.
More frequent calibration and maintenance  of counting  instruments, im-
proved quality control practices within  the  laboratories, and greater
participation in laboratory intercomparison  studies may be  beneficial
for some of the laboratories having analytical  difficulties.
     The monthly results of the barium-140 analysis are shown in  Figure
3-C.  Because of the manufacturer's production  schedules and the  half-
life of barium-140, some monthly cross-check samples  did not contain
this isotope.  Unlike strontium-89 and 90, generally  no  "wet" chemistry
is involved in the barium-140 analysis.   Most analysts determine  the
gamma emitters by gamma spectroscopy.   This  would indicate  errors arise
from improper, infrequent, or erroneous calibration;  faulty or  inade-
quate instrumentation; or erroneous processing  and interpretation of
data.  Participants obtaining inaccurate results for  their  barium
analysis should restandardize and calibrate their instruments more
frequently using the same geometry as that used for sample  counting.
It appears from this limited amount of data that the barium-140 results
are better in terms of accuracy and (s/y) than the strontium  analysis.
     The monthly results of  the iodine-131 analysis are shown  in Figure
3-D.  These results are as good as the barium-140 results in  terms of a
small deviation from y, and are better than the barium-140 results in
terms of s/y.  With proper calibration and interpretation, accurate
results appear  readily attainable.  During the six-month period where
reconstituted powdered milk  was used, the results were relatively good,
with  two of the six analyses  having an experimental sigma value  of
less  than 10  pCi/liter.   Results  were the best for the September
sample.
      The monthly results  of the cesium-137  analysis are shown  in Figure
3-E.  These  results are  considerably  better  in terms  of the ratio s/y
than  those  for  any of the other radionuclides  used in the milk cross-
check program.  The  reason for the better results with cesium  may be
partially attributed  to the fact that many  participants standardize
their instruments  with a cesium-137 source.  The cesium-137 peak area

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 may also be somewhat  easier defined than  the iodine-131 and barium-140
 peaks.   Even  better results for  cesium-137 analysis could be attained
 if improvement was made by a few of the participants,  This may best be
 accomplished  through  consultation with the laboratories having the
 analytical  problem.
      Table  3  gives the limits previously  established by the Analytical
 Quality  Control Service (1,2).   During the period July 1973 to November
 1974, with  few exceptions, results from the milk cross-check program
 did  not  approach these established limits.  Examination of these results
 reveals  that  29% of the participants were within the plus or minus
 3  sigma  control limits for the strontium-89 analysis, 42% for the
 strontium-90, 52% for barium-140, 60% for iodine-131, and 77% for
 cesium-137  (Table 4).

 SUWARY

     Data compiled for the milk cross-check program from July 1973 to
 November 1974 indicate the need for improvement in analytical  procedures
 for  all radionuclides  studied.   Accurate analysis  of strontium-89 was
 particularly difficult for most laboratories  to achieve, while the
 accurate analysis of cesium-137 was the least difficult.
     It is hoped that  results  similar to those obtained for cesium-137
 can  be accomplished for analysis of the other radionuclides.   The data,
 although generally having  relatively large measures of random devia-
 tions, indicate this may be possible for all  except strontium-89.
 There was at least one month  where the experimental  sigma approached
the  established limits for all  radionuclides  except strontium-89.   In
September 1973 the cesium-137  experimental sigma was less  than the
established limits.  These data would  indicate  the laboratories  can
achieve good accuracy  for most  of the  samples  being analyzed.
     Two things  are apparent  from these data.   The expected  relation-
ship, i.e.,  the accuracy of the analysis  should improve with increas-
ing sample activity, was  not seen with any consistency at  the  levels

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of activity used in the studies (Table 2).   There is a need for con-
siderable improvement in the laboratory analysis of both beta and gamma-
emitting radionuclides in milk.
     One reason for the variability in the  results may be due to the
expansion of the milk cross-check program to include new participants.
The number of participants more than doubled during the first half
of 1973.  As these laboratories become more familiar with the analysis,
hopefully the accuracy of the results will  improve.  For strontium-89,
and possibly strontium-90, it appears that new methods of analysis
should be evaluated since less than a third of the participating labora-
tories are doing a satisfactory job of strontium-89 analysis and less
than half for strontium-90.  If data over the next several months indi-
cate that the present limits are unrealistic for some radionuclides
and cannot be attained by the majority of participants, then the limits
should be made more realistic.  Available information does indicate
good internal precision for most laboratories, but poor accuracy in
many cases.  This exemplifies the need for improvement in analytical
procedures through the adoption of standard reference methods and
protocols for establishing equivalency to the reference method, more
frequent calibration and maintenance of counting instruments, improved
quality control practices within each laboratory, and greater partici-
pation in laboratory intercomparison studies conducted by the National
Bureau of Standards, the Energy Research and Development Administration,
and the Environmental Protection Agency.

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                                    Table 1.  SUMMARY OF  CROSS-CHECK  PROGRAMS*
SAMPLE
Milk
Water
Gross a, 6*
Gamma
3H
239pu*
226Ra
Air
Gross a, 0*
239pu*
Soil*
Diet
Urine
Gas
ANALYSIS
89Sr, 9<>Sr> 131If
137Cs, '""Ba, K

Gross o, B
60Co, 106Ru, 134Cs,
137Cs. 51Cr. 65Zn
3H
239pu
226Ra

a.' B» Y
239Pu
239pu
89Sr, 9°Sr, 1311,
137Cs. li.OBa. K
3H
85Kr
ACTIVITY
PER ISOTOPE
< 200 pCi/1

< 100 pCi/1
< 500 pCi/1
< 3500 pCi/1
< 10 pCi/1
< 20 pCi/1

< 200 pCi /sample
< 2 pCi/sample
< 50 pCi /sample
< 200 pCi/kg
< 3500 pCi/1
< 20 pCi/ml
QUANTITY
SUPPLIED
^ 4 liters

^ 4 liters
^ 4 liters
•v 60 ml
^ 4 liters
\> 4 1 i ters

3 - 2" or 4"
diam. air filters
3 - 2" or 4"
diam. air filters
-b 100 g
3 - 4-liter
samples
•v 60 ml
10 liters
PRESERVATIVE
Formalin

0.5 N HN03
0.5 N HN03
none
0.5 N HN03
0.5 N HN03

none
none
none
Formalin
Formalin
none
DISTRIBUTION
Bimonthly

Bimonthly
Bimonthly
Bimonthly
Semiannual ly
Quarterly

Quarterly
Quarterly
Semi annually
Quarterly
Quarterly
Semiannual ly
TIME FOR
ANALYSIS
& REPORT
6 weeks

4 weeks
4 weeks
4 weeks
8 weeks
6 weeks

4 weeks
6 weeks
8 weeks
8 weeks
4 weeks
8 weeks
00
      * Laboratories are required to have the necessary licenses before receiving these  samples.

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                           Table 2.   SUMMARY  OF MILK ANALYSIS  DATA,  JULY  1973 TO NOVEMBER 1974
\0

Oul'73
Aug'73
Sep'73
Oct'73
Nov'73
Dec '73
Feb'74
Apr'74
Jul'74
Sep'74
Nov'74
Strontlum-89
Known pCi /liter
1 a limit pCi /liter
1 a/known %
N
X pCi/liter
s pCi /liter
s/known %
98
5
5.1
17
87.2
11.0
11.2
96
5
5.2
14
61.5
29.6
30.8
85
5
5.9
13
76.9
12.3
14.5
133
7
5.3
19
112.3
25.4
19.1
123
6
4.9
16
98.3
24.9
20.2
89
5
5.6
18
69.5
30.8
34.6
83
5
6.0
23
92.6
44.0
53.0
204
10
4.9
28
171.9
36.7
18.0
151
8
5.3
26
128.1
27.6
18.3
157
7.9
5.0
23
137.8
25.7
16.4
172
8.6
5.0
30
137.3
39.1
22.7
Strontium-90
Known pCi/liter
1 o limit pCi/liter
1 o/known %
N
55 pCi/liter
s pCi /liter
s/known %
65
3
4.6
23
64.0
8.3
12.8
158
8
5.1
17
130.4
44.5
28.2
72
4
5.6
16
67.6
6.4
8.9
119
6
5.0
23
106.1
19.9
16.7
135
7
5.2
22
115.2
26.9
19.9
103
5
4.9
22
93.1
16.4
15.9
198
10
5.1
21
182.7
20.0
10.1
172
9
5.2
31
169.9
22.9
13.3
152
8
5.3
29
152.7
28.8
18.9
124
6.2
5.0
28
124.1
15.6
12.6
102
5.1
5.0
33
94.1
15.2
14.9

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Table 2 (continued).  SUMMARY OF MILK ANALYSIS DATA,  JULY  1973 TO NOVEMBER 1974

Jul'73
Aug'73
Sep'73
Oct'73
Nov'73
Dec' 73
Feb'74
Apr' 74
Jul'74
Sep'74
Nov'74
Barium- 140
Known pCi/ liter
1 a limit pCi/liter
1 a/known %
N
X pCi/liter
s pCi/liter
s/known %
148
7
4.7
27-
152.6
11.0
7.4
152
8
5.3
21
158.4
24.9
16.4
146
7
4.8
22
145.3
27.9
19.1
104
5
4.8
32
107.4
19.2
18.5
0






0






159
8
5.0
35
159.3
11.9
7.5
0






0






193
9.6
5.0
33
195.2
21.9
11.3
0






Iodine- 131
Known pCi/liter
1 a limit pCi/Hter
1 a/known %
N
X pC1/liter
s pCi/liter
s/known %
115
6
5.2
33
125.1
18.3
15.9
144
7
4.9
22
147.8
13.7
9.5
123
6
4.9
22
121.3
8.8
7.2
493
25
5.1
34
486.3
28.2
5.7
104
5
4.8
26
99.7
11.0
10.6
177
9
5.1
25
175.8
9.6
5.4
150
8
5.3
40
149.9
27.7
18.5
150
8
5.3
41
154.6
20.7
13.8
142
7
4.9
35
145.8
15.9
11.2
188
9.4
5.0
31
192.2
20.4
10.9
126
6.3
5.0
36
122.4
10.5
8.3

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Table 2 (continued).  SUMMARY OF MILK ANALYSIS DATA,  JULY 1973  TO  NOVEMBER 1974

Jul'73
Aug'73
Sep'73
Oct'73
Nov'73
Dec '73
Feb'74
Apr'74
Jul'74
Sep'74
Nov'74
Cesium- 137
Known pCi/liter
1 o limit pCi/liter
1 o/known %
N
X pCi/Hter
s pCi/liter
s/ known %
116
6
5.2
34
116.5
6.6
5.7
122
6
4.9
22
120.1
7.7
6.3
84
5
6.0
22
81.6
3.9
4.6
91
5
5.5
35
88.7
8.5
9.3
126
7
5.6
28
123.1
9.3
7.4
101
5
5.0
30
100.1
9.4
9.3
214
11
5.1
38
208.9
12.7
5.9
174
9
5.2
42
171.1
16.1
9.3
155
8
5.2
37
157.3
10.0
6.5
126
6.3
5.0
35
132.2
7.6
6.0
101
5.1
5.0
38
102.8
5.6
5.5

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Table 3.  LIMITS ESTABLISHED BY THE ANALYTICAL
            QUALITY CONTROL SERVICE
Radionucl ide
131J
137 Cs
'""Ba
89Sr
90 Sr
la Limits for Single Determination
For Levels <100 pCi/1 iter
(pCi /liter)
5
5
5
5
For Levels <30 pCi /liter
1.5
For Levels >100 pCi/liter
(X)
5
5
5
5 -
For Level s >30 pCi/1 iter
(*)
1.5
Table 4.  RESULTS OF MILK CROSS-CHECK ANALYSES,
           JULY 1973 TO NOVEMBER 1974
                          Radionucl ide
a Limits
<1
<2
<3
>3
89Sr
90Sr
llt0Ba
131J
137Cs
Laboratories Within a Limits (%)
11.2
20.7
28.5
71.5
19.4
31.6
42.4
57.6
25.3
42.9
52.0
48.0
29.7
49.9
59.7
40.3
39.0
63.1
76.7
23.3
                        12

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NERC-LV RADIONUCLIDES IN MILK CROSS-CHECK  PROGRAM — JUNE 1975

                    6/15/75         SAMPLE -  A          137CS

                                           KNOWN VALUE  =   101 PCI/L
   EXPECTED LABORATORY PRECISION (IS,  1  DETERMINATION)  =   5.1 PCI/L

               EXPERIMENTAL   RNG ANLY             NORMALIZED DEVIATION
LAB   RESULT      SIGMA       (R + SR)  AVERAGE    (GRAND AVG)  (KNOWN)
 D       98
 D      102
 D      102        2.3           .46       101           -.7        -.1

 P        NO DATA PROVIDED

 Q      104
 Q      104
 Q      108        2.3           .46       105            .9         1.5

 R       95
 R       99
 R       93        3.1           .69        96          -2.4       -1.8

 S      108
 S      105
 S      106        1.5           .35       106          1.2        1.8

 V       96
 V      110
 V       98        7.6          2.18       101          -.5         .1
 EXPERIMENTAL  SIGMA (ALL  LABS)   =   7        GRAND AVERAGE   =   103

  * -  NOT USED FOR CALCULATING  GRAND AVERAGE
 ** -  INSUFFICIENT INFORMATION  TO  CALCULATE
         Figure 1.   Sample Analysis  and Report of Participant's  Data
                                    13

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Explanation of terms  in Figure 1:
     Title:
     Column  1:
     Colume  2:
     Column  3:
     Columns 4
      and  5:
     Column 6:
     Column 7:

     Column 8:
     Bottom of
      Chart:
Program name, sample collection date, sample code
letter, analysis type, known concentrations 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).
Is (standard deviation) of the experimental results.
Normalized range value in "mean range + standard  error
of the range" (R + aR units for comparability.   (See
Statistical Techniques for Quality Control of Environ-
mental Badioaasay,  AQCS Report Stat-1. November 1964,
pages 4-8.) (Sp = c^ for printing purposes.)
Average value.
Normalized deviation from the grand average value of
all laboratories expressed in a^ units.
Normalized deviation from the known value expressed in
cfy units.
Is experimental  error of all  laboratories, and  the
grand average of all laboratories.
                                   14

-------
RADIONUCLIDES IN MILK CROSSCHECK PROGRAM
       LAB - D              137CS
  NORMALIZED  DEVIATION FROM  KNOWN
         1973                 1974
1U
9
8
7
6
5
4
3
s 2
' 1
® o
M
A -1
-2
-3
-4
-5
-6
-7
-8
-9
_m








.
L* r-f i A
FA f\ ;^
V^ / L_j
A/
*














>»-^ — J^v
^" X
N^^x^ w









CL
WL
WL
CL
           NORMALIZED  RANGE
         1973                1974
R +5
R +2
R +1
R +0
O





.
J F M A M J

I
J A

_J



1
.1 . 1 •
SONDJ FMAHJJASUND
CL
WL
            Figure 2. Control Chart
                    15

-------
Explanation  of terms  used  in  the control chart (Figure 2).

     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 ± 2 M) and the 99.7%
                     (y  ±  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 + 2cR) and
                     ^100% (R + 3aR) confidence levels were chosen as
                     the warning levels and control limits respec-
                     tively.]
                                   16

-------
                STRONTIUM-89 IN MIX
                  JULY 1973
    FREQ.
5 .
4 .
3 -
2 -
1 .
0

U -
x" =
s =

i i i i
0 10 20

98
87.
11.0

|
30




pCi/liter
2


|

"
..

| |
40



I i
50



I
60
                                                            I  I  I  I I  I I  I  I
                                 50 60  70  80  90  100  110  120 130  140 150 160
                                      CONCENTRATION IN pCi/liter
    FREQ.
    FREQ.
5..
4 . .
3 --
2 -.
1 4.
0
                STRONTIUM-89 IN MIX


                  AUGUST 1973

                     Jl = 96 pCi/liter
                     X = 615

                     S = 296
                     X
                     +
                 10  20 30   40   50  60  70  80  90  100  110  120  130 140 150  160

                                     CONCENTRATION IN pCi/liter
5 ..
4 . .
3 --
2-.
1 ..
0  _
STRONTIUM-89 IN MILK


 SEPTEMBER 1973

      U = 85 pCi/liter

      X" = 76.9  "
      S = 12 3



 I I   I I  I  111
                                                            I I  I I  I  I
                 10   20  30  40  50  60  70 80  90  100  110  120  130 140 150  160
                                     CONCENTRATION IN pCi/liter
           5 ..
           4 ..
   FREQ.   3 . .
           2 -.
           1 . .
           o L
    STRONTIUM-89 IN MILK


     OCTOBER 1973

       L| = 133 pCi/liter
       X = 112.3
       S = 254
                 I  I  I  I I  I I  I  I  I  I  I
             0  10  20  30  40  50 60  70  80  90 100  110 120 130  140 150 160
                                     CONCENTRATION IN pCi/liter
Figure  3-A.    Histogram  of Monthly  Analysis  for  Strontium-89

                                     17

-------
        5 , .
        4 . .
 FREQ.   3 . .
        2 - .
        1 . .
        o L
STRONTIUM-89 IN MILK


 NOVEMBER 1973

     U, « 123 pCi/liter

     X = 98.3

     S = 24 9
          0  10  20 30  40  50  60  70  80  90 100  110 120  130 140 150  160

                               CONCENTRATION IN pCi/titer
            STRONTIUM-89 IN MILK
        5 . .
        4 . .
 FREQ    3 . .
        2. .
        1 . .
        0
 DECEMBER 1973

    LI » 89 pCi/litef

    7 = 69 5  •

    S = 308
         0   10  20  30  40  5C 60  70  80  90  100  110  120 130  140 150  160

                              CONCENTRATION IN pCi/liter
         STRONTIUM-89 IN MILK


             FEBRUARY 1974


       6- -
       5- -     L) = 83 pCi/liter

FREQ   4--     x = 926  •
       3T
       2-
       1

       °   I  '  ' I  I	I I  I  I I  I  I  I I  I  I I  I  I |  |  I  ^^ I  I I  ff I  I  I  I |  I  I I
        0  10  20  30  40  50  60  70  80  90  100  110  120 130  140 150  160 170  180 190 200 210 220 230

                                    CONCENTRATION IN pCi/liter
         STRONTIUM-89 IN MILK


            APRIL 1974

       6- -
       5- .     L| = 204 pCi/liter
FREO   4- .     X = 171 9
       3- •     S = 36 7
       2- -

       o'l  I  I I I  I I I  |  I |  I  I I
        0  10   20  30 40  50  60  70  80  90  100  110  120 130  140' 150' 160 ' 170'  180' «o' 200 210'220 '230
                      11''  r^rtJrTvl~"^^~^W~^^~H-^^-
                                    CONCENTRATION IN pCi/liter
Figure  3-A.   Histogram  of Monthly  Analysis for  Strontium-89 (continued),

                                        18

-------
 FREQ.
  STRONTIUM-89 IN MILK

     JULY 1974
6 ""     LI = 151 pCi/liter
4 -~     X = '28.1   ••
                    27,6
3--
2- -
o'l  I  |  I I I I  I  I  I  I  I B I  I  I ^^  m-^^-^^ff fl  I  I I  I  M  M |  M
  0  10  20  30  40  50  60  70  80  90 100 "0  120 130 140  150  160 170  180  190 200 210 220 230
                                CONCENTRATION IN pCi/liter
          STRONTIUM-89 IN MILK
 FREQ
            SEPTEMBER 1974

                JJ = 157  pCi/liter
                    137.8
6--
5--
4- -
3--      S =  257
2- -
1 - -
0   < |  I  I I I I  I—|  I  I  I I  | I  i  i—fiii—i—n—i—i '  « i  i  t «—i  i  i  i  i  i i  i  i  i  i i  T—r
  0  10  20  30  40  50  60  70  80  90 100 110  120 130 140  150  160 170 180 190 200 210 220 230
                                       CONCENTRATION IN pCi/liter
          STRONTIUM-89 IN MILK
 FREQ
 6- -
 i".
 3- -
NOVEMBER 1974
   U - 172 pCi/liter
   X = 137 3  -
   S = 39.1   -
   1  I I  |  I  |  I  I I  |  I
  0   10  20  30  40  50  60  70 80  90  100  110 120  130 140 150 160' 170'
                                CONCENTRATION IN pCi/liter
                                                                                      I  I  I I M
                                                                                190 200 210 220 230
Figure  3-A.   Histogram  of Monthly Analysis  for Strontium-89 (continued).
                                             19

-------
           STRONTIUM-90 IN  MILK
FRED
              JULY 1973
                                              i i  i  i
           0   10  20  30  40  50  60  70  80  90 WO  110  120  130  140  150  160 170 180 190  20C 210 220

                                         CONCENTRATION IN pCi/liter
FREQ
   STRONTIUM-90 IN  MILK

      AUGUST 1973

        L4 = 158 pCi/liter
        )T = 130.4
        S = 44.5
              10   20   30  40  50  60  70  80   90  100  110  120  130  140  150  160 170 180  190  20C 210 220

                                         CONCENTRATION IN pCi/liter
FREQ
           STRONTIUM-90 IN MILK
SEPTEMBER 1973
6 -
5 -
4 -
3 -
2 -
1 .
0
(
U = 72 pCi/liter
X = 67.6
S = 64
i 1 I I I i | | i




i
1 1 1 1 1 1 T 1 1 	 1 	
3 10 20 30 40 50
                                              I I I
                                                     I  I  I  I  I  I  1  I  I  I
                                                                    I  •! I  1  I  I  I  I  I  |  |l
                                     70  80  90  100  110  120  130  140  150  160  170 180 190  20C 210  220

                                         CONCENTRATION IN pCi/liter
           STRONTIUM-90 IN MILK
FREQ
6 --
5 --
4 --
3 --
2 --
1 --
0
  0
OCTOBER 1973

   L|  - 119 pCi/liter
   X  = 106.1
   S  = 19.9
                                                                        I  I  I  I  I  I  I  I  I I  I   I  |l
              10   20  30  40  50  60  70  80  90  WO  110  120  130  140  150  160 170 180 190  20C 210  220

                                         CONCENTRATION IN pCi/liter
     Figure  3-B.   Histogram  of  Monthly  Analysis  for  Strontium-90
                                              20

-------
               STRONTIUM-90 IN MILK
    FREQ.
6 --
5 --
4 - -
3 --
2 --
1 -j-
0
NOVEMBER 1973

    Lj = 135 pCi/liter
    X = 115.2
    S - 26.9
                  10
                     20  30  40  50  60   70  80  90  CO  110 120 130  140  150  160  170 180 190  20C 210 220

                                            CONCENTRATION IN pCi/liter
    FREQ
    FREQ.
   STRONTIUM-90 IN  MILK

    DECEMBER 19/3

        M = 103 pCi/liter
        X = 93.1
        S = 16 4
                                                                            I  I I
              0   10  20  30  40  50  60   70  80  90  CO  110 120 130  140  150  160  170 180 190  20C 210 220

                                            CONCENTRATION IN pCi/liter  ,
               STRONTIUM-90 IN MILK
6 - -
5 --
4 - -
3 •-
2 --
1 - -
o  L-
FEBRUARY 1974

    M = 198 pCi/liter

    X = 1827   ••

    S = 20.0
                I  I  I .11  I  I  I  I  I  I I  I I  I  I  I  I  I  I  I  I  I I I
              0   10  20  30  40  50   60   70  80  90  100  110  120 130 140  15O  160  170  180 190  20C 210  220

                                            CONCENTRATION IN pCi/liter
               STRONTIUM-90 IN MILK
    FREO
6 --
5 --
4 --
3 --
2 --
1 --
o  L.
APRIL 1974

   U, =  172 pCi/liter
   3? =  169.9   ••
   S =  22.9   "
                                    -H-
              0   10  20  30  40  50 60   70  80  90  OO  110  120 130 140  150  160  170 180 190  20C 210  220

                                            CONCENTRATION IN pCi/liter
Figure  3-B.    Histogram of Monthly Analysis  for  Strontium-90 (continued),
                                                 21

-------
 FREQ
FREQ
   STRONTIUM-90 IN MILK

    JULY 1974
6  I   L| = 152 pCi/liter
5 •-  X = 1527
3 "  S = 288
2 •-
0 T|  |  |  | |  |  |  |  |  |
   0  10  20   30  40  50  60  70  80  90  XX)  HO  120 130  140  150 160  170  180 190  20C 210 220
                                CONCENTRATION IN pCi/liler

   STRONTIUM-90 IN MILK

    SEPTEMBER 1974
6 • -    H = 124 pCi/liter
4 . _    X = 124.1
3 - -    s = 15.6
2 :-
1 . -
0  I  I I  I I  I  I I  I I  I  I  I  I I
   0   10  20   30  40  50  60  70  80  90  100  110  120 130 140  150 160  170  180 190  20C 210 220
                                CONCENTRATION IN pCi/liter
 FREO.
           STRONTIUM-90 IN MILK
             NOVEMBER  1974
                                                           I  I  I  I  I  I  I I  I  I  I  I  I  I I  I  I  I  II
               10  20  30 40  50  60  70  80  90  100  HO  120  130 140 150  160 170 180  190  20C 210 220
                                        CONCENTRATION IN pCi/liler
Figure  3-B.   Histogram  of  Monthly Analysis  for Strontium-90 (continued)
                                              22

-------
          BARIUM-MO IN MILK
 FREQ.
           JULY 1973
         L| = 148 pCi/liter

         3< = 152.6   ••

         S = 11.0
                 I  I  I i I
                       I  I  I  I I  I  I  I
           40  50  60  70 80  90 100 110  120 130 140 150 160 170 180 190 200 210 220 230240

                                         CONCENTRATION IN pCi/litec
         BARIUM-140 IN MILK
FREQ
FREQ.
AUGUST 1973
7 -
6 •
5 -
4 -
3 -
2 -
1 „
0

M • '52



pCi/liter

\ 7 = 158.4
S = 24.9


I-Ul I J I 4.



i-L I I
          40  50  60  70  80 90  100  110 120 130 140 150 160  170 180  190 200 210 220 230240

                                         CONCENTRATION IN pCi/l.ter
         BARIUM-140 IN MILK
7 ••
6 --
5 --
4 - -
3 --
2 --
1 - -
o L_i
SEPTEMBER 1973

   U • 146 pCi/Uter
   X = 145 3
   S = 27.9
                   -M-4
          40  5O  60 70  60 90  100  110 120 130 140 (50 160  170 180  190 200 210 220 230240

                                         CONCENTRATION IN pCi/liter
         BARIUM-(40 IN MILK
           	M  I -t  I .41  M  M I  I  I  I
          40  50  60  70  80 90  100  110 120 130  140 150 160  170 180 190 200 210 220 230240

                                         CONCENTRATION IN pCi/liter
   Figure  3-C.   Histogram  of  Monthly Analysis  for Barium-140

                                         23

-------
           BARIUM-140 IN MILK
  FREQ.
            FEBRUARY 1974
7 • •
6 --
5 -•
4 - -
3 --
2 --
1 - -
LJ = 159 pCi/liter

>T = 159-3   "

S = 1V9
            40  50  60 70  80  90 100  110  120 130 140 150 160 170 180  190 200 210 220 230240

                                         CONCENTRATION IN pCi/liter
           BARIUM-140 IN MILK
         7  -•
         6  --

  FFREQ. 4  "
         3  --
         2  --
         1  - -
         0   -
    SEPTEMBER 1974

        Lj = 193  pCi/liter
        X - 195.2
        S = 21 9
            40  50  60  70  80 90 100 110  120 130 140 150 160 170 180 190 200 210 220 230240

                                         CONCENTRATION IN pCi/liter
Figure  3-C.   Histogram  of Monthly  Analysis for  Barium-140  (continued).

                                         24

-------
       IODINE-131 IN MILK
FREQ.
 FREQ.
JULY
9 -
8 -

7 -
6 -
5 -
4 -
3 -
2 -
1 -
n










1973
U =

X =

s =






115

125

18.3






pCi/liter

1

.




, J
                                                             M  M  I  I  I I I  M  I  I  I  I  I  I
                              90  100  110 120 130  140  150 160 170 180 190 200 210 220 230 240 250
                                        CONCENTRATION IN pCi/lrter
       IODINE-131 IN MILK
           AUGUST 1973
9 -
8 - -
7 - -
6 - -
5 - -
4 - -
3 - -
2 - -
1 - -
0 I—"
                 L| = 144 pCi/liler
                 H. = 147.8
                 S = 13.7
             I  I  I  I  I  1  I  I  I  1  I I I  I  I
                                                                I  I  I  I  I I  I  I  I  I  I  I
           40   50  60  70  80  90  100  110 120 130  140  150 160 170 180 190  200 210 220 230 240 250

                                        CONCENTRATION N pCi/liter
FREQ.
       IODINE-131 IN MILK
           SEPTEMBER 1973
9 - •
8 - -
7 - -
6 - -
5 - •
4 - -
3 - -
2 - -
1 - -
0  -
\\
                     123 pCi/liter
                   = 121.3
                  S = 8.8
                                                                     I  I  I  I  I I I  I  I  I  I
           40  50  60  70  80
                              90  100  110 120 130  140  150  160  170 180 190 200 210 220 2-30 240 250
                                        CONCENTRATION IN pCi/liter
FREQ.
9
8
7
6
5
4 4-
3 - .
2 -.
           OCTOBER 1973
                  U = 493 pCi/liter
                  X = 4863
                  S = 282
                                          420 430 440 450 460  470 480 490 500 510 520 530 540 550 560
                                     CONCENTRATION  IN pCi/liter
        Figure  3-D.    Histogram  of Monthly  Analysis  for  Iodine-131
                                             25

-------
       IOOINE-131 IN MILK
          NOVEMBER 1973

      9 - •       H = 104 pCi/liter

      7 " !      "X • 99 7
      6 - -      S = 11 0
      5 - •
FREO.  4 . .
      3 - -
      2 - -
      1 - -
      0 '  I I  I  I  I  I
                                                I  I  I  I I  I I  I  I  I  I I I  I  I  I  I  I  I I  I  I  I

          40  50  60  70  80  90  100 110  120  130 140 150 160  170 180 190  200 210 220 230 240 250

                                      CONCENTRATON N pCi/liter
       IODINE-131 IN MILK

          DECEMBER 1973
      9 - •       L| - 177 pCi/liter
      7 '. '.       ^ = 1/58  "

FREQ.  65::       s = 96    •'
      4 . .
      3 - -
      2 - -
      1 - -
      0  ' |  |  I  I  I I  t  I  I  |  I  I I I  I  I  I  I  I  I I '
          40  50  60  70  80  90  100  110 120 130  140 150 160  170  180 190 200 210 220 230 240 250

                                       CONCENTRATION IN pCi/liter



       IODINE-131 IN MILK
          FEBRUARY 1974
                 U - 150 pCi/liter
                 7 * 149 9   ••

                 8-27-7   "
           I  I  I  I  I I  I  I  I

          40  50  60  70  80  90  100  110 120 130  140 150 160  170  180 190 200 210 220 230 240  250

                                       CONCENTRATION IN pCi/liter
       IODINE-131 IN MILK
          APRIL 1974
       9  -•
       8  • •
       7  - •

FREO.   |  " ~
       4  • •
       3  - -
       2  - -

       o  T
                 D = 150 pCi/liter

                 X = 154.6
                 S - 20 7
           40  50  60  70  80   90 100  110  120 130 140  150 160 170  180  190 200 210 220
                                        CONCENTRATION IN pCi/liter
                                                                                 230 240 250
    Figure 3-D.    Histogram  of  Monthly Analysis  for  Iodine-131(continued).

                                             26

-------
    FREQ.  « "*"
         4 ..
         3 --
         2 --
         1 --
          IOOINE-131 IN MILK


            JULY 1974
         9 .-      L| - 142 pCi/liter
         8 •-      X = 1458 - "
         7 +      S = 159
               I I  I I I >
                     I  I I I  I I  ^^^—^^^^^^^^^^^^^^^^—^—I—(—f—
            40 50  60  70  80  90  100 110 120 130 140 150 160 170 180  190 200 210 220 2-30 240 250
                                     CONCENTRATION IN pCi/liter



         IODINE-131 IN MILK

            SEPTEMBER 1974                                     _
      9  • •
      8  - -


FREQ.  I  " ;
      4  - -
      3  - -
      2  --
                  LJ = 188 pCi/liter
                  X = 1922   "
                  S • 20.4
                         *



             JLJL-i   j
'  I I'll 1H~^^^T~f~+•
            •1 I  I I  I  I I  I  I |  I I  I I I  I

            40  50 60  70  80  90 100  110  120 130 140 150  160 170 160 190 200 210 220 230 240 250

                                     CONCENTRATION IN pCi/Mer



         IODINE-131 IN MILK


            NOVEMBER 1974
         9  • •
   FREQ.
            40  50  60 70  80  90 100 110  120 130 140 150 160  170 180 190 200 210 220 2-30 240 250

                                     CONCENTRATION IN pCi/liter
Figure 3-D.   Histogram of  Monthly Analysis for Iodine-131 (continued),

                                        27

-------
           CESIUM-137 IN MILK

             JULY 1973
 FREQ.
            40  50  60  70  80  90  100  110  120 130 140  150  160 170 180  190 200  210 220 230 240

                                          CONCENTRATION IN pCi/liter
           CESIUM-137 IN MILK


            AUGUST  1973
        12
        11
        10
        9
        8
 FREQ.   7
        6
        5
        4
        3
        2
        1
        0
  40   50   60  70  80  90  100  110 120 130  140 150 160 170  180  190 200 210 220 230 240

                                CONCENTRATION IN  pCi/liter
 CESIUM-137 IN MILK


 SEPTEMBER 1973
 • • U « 84  pCi/liter   x
   7 = 816     ••   I

- • S = 3.9
                                       M I  I  I  I  I  I  I  M I I  I  I  I  I  I  I  I  I  I I  M  I  I
           40  50  60  70 80  90  100  110  120 130 140 150  160  170 180 190  200 210 220 230 240
                                         CONCENTRATION IN pCi/liter
          CESIUM-137 IN MILK
          OCTOBER 1973
FREQ
                                            I  I  I  I I  I  I  I  I  I  I  I  I  I  I I  I  I  I  I  I  I  I  I
           40   50   60  70  80  90 100 110  120 130  140 150 160 170  180  190 200 210 220 230 240
                                        CONCENTRATION IN pCi/liter

      Figure 3-E.    Histogram of Monthly Analysis  for Cesium-137

                                           28

-------
            CESIUM-137 IN MILK
         12 - -
  FREQ
  FREO.
  FREQ
            40   50  60  70  80  90 100 110  120 130  140 150 160 170  180  190 200 210 220  230  240

                                          CONCENTRATION IN  pCi/liter
            CESIUM-137 IN MILK
             DECEMBER 1973
                                                I  I  I I  I  I  I  I  I  I  I  I I  I  t  I  I  I  I  I I  I t
            40   50  60  70  80  90 100 110  120 130  HO 150 160  170  180 190 200 210 220 230  240
            CESIUM-137 IN MILK
                                          CONCENTRATION IN pCi/liter
         12
         11
         10
         9
         8
  FREO   7
         6
         5
         4
         3
         2
          1
         0
    FEBRUARY 1974

        (Lj = 214pCi/liter

        "X » 2089 "

        S = 127   "
     I  I  I  I  i  I I 1 I  II  I  I  I  I  I I  I  I  I  .....
             40  50  60   70  80  90  100  110 120 130  140  )50 160 170  180  190 200 210 220 230 240

                                           CONCENTRATION IN pCi/liter
           CESIUM-137 IN MILK
12
11
10
9
8
7
6
5
4
3
2
1
0
             APRIL 1974
                    174 pCi/liter

                    171.1

                    16.1
             I  (  I  I  I  I  I  I  I  I I I  I  I  I  I  I  I
            40  50  60  70  80  90 100 110  120  130 140 150 160  170  180 190 200 210 220 230 240
                                          CONCENTRATION IN pCi/liter

Figure  3-E.   Histogram  of  Monthly Analysis  for  Cesium-137  (continued)

                                             29

-------
             CESIUM-137 IN MILK
               JULY 1974
           12 - -
           11 - -

           9 -.
           8 . .

     FREQ.  6 '. ".
           5 - -
           4 . .
           3 - -
           2 - -
       U = 155 pCi/Uter

       S = W.O
               | | |  |  I  I I I  I  |  |  I I  I  I  I I I
               40  50  60  70  80  90 100 110  120 130  140 ISO 160  170 180  190 200 210 220 230 240

                                           CONCENTRATION IN pCi/liler
  CESIUM-137 IN MLK


    SEPTEMBER 1974

  ' '   L| = 126 pCi/liter

10 - •    3( = 1323
9 . .
8 - .
            9  - •    S - 7.6
     FREQ.   I
            6  - -
            5  . .
            4  - -
            3  - -
            2  - -
            1  - -
                                  I  I  I I I  |^PPPPPM-M-I  I  I I  I  I  M I
               40  50  60  70  80  90  100  110 120  130 140 150  160 170  180 190  200  210 220 230 240

                                           CONCENTRATION  IN pCi/liter
              CESIUM-137 IN MIX

                NOVEMBER 1974
            12 J-
            11 - -    |J  *  101 pCi/litef
            10 - •
            9 - .
            8 -.     5=56
     FREQ.   I ' •
            6 - *
            5 --
            4 . .
            3 - -
            2 - -
        X = 1028
                M  I  I M I  I  I I F^^^^-t-l  I I  I  II I  I  I  I  I  I I  M  I I  I  I  M I
               40  50  60   70  80  90  100  110 120 130 140 150  160 170  180 190 200  210 220 230  240

                                            CONCENTRATION IN pCi/liler
Figure 3-E,    Histogram of Monthly  Analysis for  Cesium-137  (continued),

                                            30

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                             REFERENCES


1.   F.  Knowles,  "Interlaboratory Study of Iodine-131,  Cesium-137,
    Barlun-140,  Strontium-89,  and Strontium-90 Measurements  in  Milk,
    May-July 1970," Technical  Experiment  70-MKAQ-l,  Analytical  Quality
    Control Service, Bureau  of Radiological  Health (1970).

2.   F.  Knowles,  "Rapid Field Method for  Radiostrontium in  Milk,"
    Technical Report 70-TEC-l, Analytical Quality Control  Service,
    Bureau of Radiological  Health (1970).
                                    31

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                 APPENDIX.   STATISTICAL CALCULATIONS

     To  illustrate the computations performed by the computer, example
 calculations are given using data for three actual samples analyzed at
 one laboratory  (Laboratory D).
     The experimental data are listed and the mean, range, and the
 experimental sigma are computed.  These statistics provide measures of
 the central tendency and dispersion of the data.
     The normalized range is computed by first finding the mean range,
 R, the control  limit, CL, and the standard error of the range, aD.
                                                                K
 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 per-
 formance.   In the example, the normalized range equals 0.3 R which
 falls inside the upper warning level, R + 2oR.   The precision of the
 results is acceptable.
     The normalized ^deviation is calculated 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 -0.7
which falls within  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 cal-
culated 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.
                                   32

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EXAMPLE CALCULATIONS  (Laboratory D Data)

Experimental  data:
     Known value =  y  = 3273  pCi  3H/liter  urine on September 24, 1974
     Expected laboratory precision =  a =  357  pCi /liter
                Laboratory    Samp! e         Result
                    D           Xi     3060  pCi/liter
                    D           x2     3060  pCi /liter
                    D           x3     3240  pCi /liter
     Mean = x
                    N
             x  =     -  =  T-  =  312° PCi /liter
                     M         j
where     N = number of results

     Range = r
              r  =  [maximum result - minimum result)
                 =  | 3240 - 3060 |   =  180 pCi /liter

     Experimental sigma = s
                     N - 1
-  V
              3060)' +  (3060)^ + (3240)^ - (3060 + 3060 + 3240)^
        =  103.9 pCi/liter
                                   33

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      Normalized range = wR + xaR
           Mean range = R
                       R  =  d2a            where d2  =  1.693 for N = 3*
                          = (1.693)(357)
                          =  604.4  pCi/liter
           Control  limit = CL
                      CL  =  R + 3aR
                          =  DuR            where  D* =  2.575 for N = 3*
                          =  (2.575)(604.4)
                          =  1556 pCi/liter
           Standard  error of  the range = OD
                                         K
                     aR  =  1/3 (R + 3aR -  R)
                          =  1/3 (D*R - R)
                          =  1/3 (1556 - 604.4)
                          =   317.2 pCi/liter
               wR + xaR  =  1R + XCTR
                            1R
                                  r - wR
                                    °R
on       for r > R
*  Rosensteln, M., and A.  S.  Goldin,  Statistical Techniques for Quality
Control of Environmental Radioassay,  AQCS Report Stat-1,  U.S.  Depart-
ment of Health, Education and Welfare,  PHS,  November  1964.
                                   34

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              wR + xaR  =  wR + oaR
                           wR
                           Frl R                  for r <  R
                           LRj
OTT
                                                  since  18° < 604-4
                        =  0.30 R
Normalized deviation of the mean from the known value  =   ND
     Deviation of mean from the known value  =  D
                        D  =  x - y
                           =  3120 - 3273
                           =  - 153 pCi /liter
     Standard  error of  the mean  =  a
     ND  =   _
            am
         _  -  153
         "  2S57T
         =  -  0.7
                           =  357

                           =  206.1 pCi/liter
                                   35

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 Experimental  sigma (all laboratories) = st
                        =  149 pCi/liter

Grand average = GA
                            N
                             N
                           49345
                        =  3290 pCi/liter
Normalized deviation from the grand  average = ND1
     Deviation of the mean from the  grand average  = D'
                    D1   =  x - GA
                        =  3120 - 3290
                        =  - 170 pCi/liter
ND'   =   .
        am
     -   -  170
        20FT
     =   -  0.8
                                   36

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                                   TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse before completing)
1. REPORT NO.
  EPA-680/4-75-007
                                                        3. RECIPIENT'S ACCESSIOWNO.
4. TITLE AND SUBTITLE
   Preliminary Milk Report
                                                           5. REPORT DATE
                                                             June 1975
                                                        6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
  Arthur N.  Jarvis and  David  G.  Easterly
                                                        8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORG \NIZATION NAME AND ADDRESS
   Technical  Support Laboratory
   National Environmental  Research Center
   P.  0.  Box 15027
   Las. Vegas, Nevada 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, D.C. 20460
                                                         13. TYPE OF REPORT AND PERIOD COVERED
                                                         14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
   A summary of the results of the milk cross-check program from  July 1973 through
   November 1974 is given.   Examination of  these results reveals  that 29% of the
   participants were within the plus or minus  3 sigma control limits for strontium-89
   analysis, 42% for the  strontium-90, 52%  for barium-140, 60%  for iodine-131, and
   77% for cesium-137.  These results indicate the need for improvement in analytical
   procedures for the  radionuclides studies.   Accurate analysis of strontium-89 was
   particularly difficult for most laboratories to achieve, while the accurate
   analysis of cesium-137 was the least difficult.
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                              b.lDENTIFIERS/OPEN ENDED TERMS
                                                                       c. cos AT I Field/Group
milk analysis
isotopes  89Sr,  90Sr,
quality control
quantitative analysis
laboratory  performance
                                131I,  13?Cs
i sotopes
quality assurance
radioactivity
radiochemistry
07 05
12 02
14 07
18 02, 04,  08
18. DISTRIBUTION STATEMENT

   Release unlimited
                                            19. SECURITY CLASS (This Report)
                                                unclassified
                         21. NO. OF PAGES
                              40
                                              20. SECURITY CLASS (Thispage>
                                                  unclassified
                                                                       22. PRICE
EPA Form 2220-1 (9-73)
                                                                              GPO 693-
                                                                                 i-740/4
                                                                                       '60

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