WATER PHYSICS NO. 1

       Report Number 39
      Report of a Study Conducted by

  ANALYTICAL REFERENCE SERVICE
    R. J. Lishka and E. F. McFarren
       Division of Water Hygiene
ENVIRONMENTAL PROTECTION AGENCY
          Water Quality Office
         Cincinnati, Ohio 45213
                1971

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     WATER PHYSICS NO. 1

       Report Number 39
      Report of a Study Conducted by

  ANALYTICAL REFERENCE SERVICE
    R. J. Lishka and E. F. McFarren
       Division of Water Hygiene
ENVIRONMENTAL PROTECTION AGENCY
          Water Quality Office
         Cincinnati, Ohio 45213
                1971

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                            FOREWORD

        The Analytical Reference Service (ARS) is conducted by the
Division of Water Hygiene of the Environmental Protection Agency to
evaluate laboratory methods in the environmental field.  Cooperative
studies by member organizations,  who analyze identical samples and
critically review methodology, provide the mechanism for:

                Evaluation of analytical procedures, including
                precision and accuracy,  by comparison of the
                procedures and results  reported  by participating
                laboratories.

                Exchange of information regarding method char-
                acteristics.

                Improvement or replacement of existing methods
                by development of more accurate procedures,  and
                development of new methodology  for determination
                of new pollution compounds.

       Samples are designed to contain measured amounts of selected
constituents.  Decisions as to qualitative makeup are made by the
membership,  consultants, and the ARS staff.  Notice of each study is
sent to the entire membership.  To those who desire to participate, a
portion of the study sample is sent, along with data forms for reporting
numerical values, a critique of the procedures used, comments on
modifications, sources of error,  difficulties encountered, or other
pertinent factors.   The results and comments  received are compiled,
and a report of each study is prepared.

       Now primarily directed toward examination of water, in the
past studies have included methods for analysis of air, milk, and food.
Some studies  are periodically repeated for the advantage of new mem-
bers, the evaluation of new methods,  or the reevaluation of existing
methods.

       The selection of studies is guided by requests from standard
methods committees and the responses to questionnaires periodically
circulated among the  membership, which now  includes 299 Federal,
state,  and municipal agencies; industries; universities;  consulting
firms; and foreign agencies.
                                 HI

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                     COMPLETED STUDIES
Water Minerals
Water Metals
Water Fluoride
Water Radioactivity
Water Surfactant
Water Oxygen Demand
Water Trace Elements
Calcium, magnesium,  hardness,  sulfate,
chloride, alkalinity, nitrite, nitrate,  sodium,
and potassium; study No. 1 completed in 1956,
No. 2 in 1958 and No.  3 in 1961.

Lead, copper, cadmium, aluminum, chro-
mium, iron, manganese, and zinc;  study No.
1 completed in 1957 and No. 2 in  1962.  These
same metals plus silver; study No.  3  com-
pleted in 1965.  Except for the substitution of
magnesium for aluminum, these same metals
were  analyzed by atomic absorption in 1967;
study No.  4.  Copper,  manganese,  and alum-
inum  in the presence and absence of  interfer-
ences; study No.  5  completed in 1969. Alum-
inum, beryllium and barium by atomic absorp-
tion; study No.  6  completed in 1970.

Fluoride in the presence and absence  of inter-
ferences,  with and  without distillation by a
specified procedure; study No.  1  completed
in 1958  and No. 2 in 1961.  Fluoride by ion-
exchange and fluoride electrode; study No.  3
completed in 1969.

Gross beta activity; study No.  1 completed
in 1959 and No. 2 in 1961.  Gross beta and
strontium-90 activity;  study No. 3 completed
in 1963.

Surfactant in various waters; study No.  1
completed in 1959,  No. 2 in 1963 and  No. 3
in 1968.

Biochemical oxygen demand and chemical
oxygen demand; study  No. 1 completed in
1960.  Chemical oxygen demand;  study No.
2 completed in 1965.

Arsenic, boron,  selenium, and beryllium;
study No. 1 completed in 1962.  These same
metals plus vanadium; study No.  2  completed
in 1966.

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Freshwater Plankton
Water Nutrients
Evaluation of the precision and accuracy
obtainable by the use of various methods of
plankton counting and identification; study
No.  1 completed in 1964.

Silicate, phosphate, ammonia nitrogen,
organic nitrogen,  and nitrate nitrogen;
study No. 1 completed  in 1966.  Ammonia
nitrogen, nitrate nitrogen and ortho, poly,
and organic phosphate;  study No.  2 completed
in 1969.
Water Phenols
Water Cyanides
Water Chlorine
Air Inorganics
Phenol and 2, 4-dichlorophenol in water by
two specified methods; study No. 1 completed
in 1966.

Potassium cyanide and potassium ferricyanide
in water by two specified methods; study No.
1 completed  in 1967.

Free and combined chlorine by nine different
methods; study No.  1 completed in 1969.

Chloride, sulfate, fluoride,  and nitrate in
aqueous  solution and on glass-fiber, high-
volume filter mats;  study No. 1  completed
in 1958.
Air Lead
Air Particulates
Air Sulfur Dioxide
Water Pesticides
Filter paper tape impregnated with lead;
study No. 1 completed in 1961.

Microscopic identification of some common
atmospheric particulates; study No.  1 com-
pleted in 1964.

Sulfur dioxide in air by a specified method;
study No. 1 completed in 1963.

Lindane, heptachlor epoxide, DDE, and
dieldrin in water; study No.  1  completed in
1965.  Lindane, heptachlor,  aldrin,  hepta-
chlor epoxide,  p, p'-DDE, dieldrin, endrin,
o, p'-DDT, p, p'-DDT, and methoxychlor in
water; study No. 2  completed in 1968.  Lin-
dane, heptachlor epoxide, dieldrin, hepta-
chlor, p, p'-DDT and endrin; study No. 3
completed in 1970.

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Food Pesticides          DDT in milk; study No.  1 completed in 1962.
                         Lindane,  heptachlor epoxide, DDE, and diel-
                         drin in milk; study No. 2 completed in 1965.

Water Physics           Total Alkalinity, pH,  specific conductance
                         and total  residue in water; study No. 1 com-
                         pleted in  1970.

       Copies of these reports are available from ARS on request as
long as the present supply lasts.  In most cases  reports published prior
to 1965 are no longer available.  Order by title;  namely, Water Metals
No. 4,  or Water Surfactant  No. 3, etc.

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                       CONTENTS
                                                    Page
PREFACE	  ix
PARTICIPANTS IN THIS STUDY	   x
ABSTRACT	xv
DESIGN OF THE STUDY	   1
TREATMENT OF THE DATA	   i
RESULTS	   2
       Alkalinity	   2
       pH	21
       Specific Conductance	21
       Total Residue	45
COMMENTS OF THE PARTICIPANTS	77
SUMMARY AND CONCLUSIONS	80
BIBLIOGRAPHY	81
APPENDICES	83
       A. Tabulation of Results	84
       B. Glossary of Statistical Terms	138
       C. Tests for Normality and Rejection of Outliers .  . 141
       D. Comparison of Methods for Statistically
          Significant Differences in Precision
          and Accuracy	144
       E. Analytical Reference Service Membership .  .  .  . 147
                           Vll

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                             PREFACE

       The present 12th edition of Standard Methods for the Exami-
nation of Water and Wastewater offers three methods of detecting the
endpoint in the total alkalinity titration which have not been evaluated
by collaborative study.  This study was proposed to perform such an
evaluation and at the same time develop precision and accuracy data
for the measurement of total residue at the  two different drying tem-
peratures suggested in Standard Methods.  The nature of the samples
made it expedient also to evaluate the precision and accuracy of the
specific conductance measurement, and to reevaluate the measure-
ment of pH because the precision and accuracy data presently in
Standard Methods were obtained from a study conducted 12 years  ago
and since then,  many improved pH meters have been developed.

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                PARTICIPANTS IN THIS STUDY

Alabama Water Improvement Commission, Montgomery
Allentown City Laboratory, Pennsylvania
Arkansas Pollution Control Commission, Little Rock
Armco Steel Corporation, Middletown, Ohio
Atlanta Department of Public Health,  Georgia
Bay Area APCD,  San Francisco,  California
Bio-Technics  Laboratories, Inc., Los Angeles,  California
Black & Veatch, Kansas  City, Missouri
Borg-Warner  Corporation, Des Plaines, Illinois
Brown & Caldwell Laboratories,  San  Francisco, California
Bureau of Industrial Hygiene,  Richmond, Virginia
BWH Fluoridation Laboratory, Bethesda,  Maryland
California State Health Department, Los Angeles
California Water  Service Company, San Jose
Calgon Corporation,  Pittsburgh,  Pennsylvania
Carnegie-Mellon  University,  Pittsburgh, Pennsylvania
Central New York Laboratory, Syracuse
Chrysler  Corporation, Detroit, Michigan
City of Amarillo,  Texas
City of Charlotte  Water Department,  North Carolina
City of Cincinnati, Department of Sewers, Ohio
City of Durham, North Carolina
City of Flint Water Plant, Michigan
City's Institute for Health Protection,  Beograd,  Yugoslavia
County of Fresno, California
Denver Board of Water Commissioners, Colorado
Department of Energy, Mines &  Resources, Ottawa, Ontario, Canada
Department of Health & Rehabilitative Services,  Jacksonville, Florida
Department of Municipal Laboratories, Hamilton,  Ontario, Canada
Department of National Health & Welfare,  Vancouver, B.C., Canada
Department of Public Health, Lidcombe, N. S,  W.,  Australia
Department of Water & Air Resources, Raleigh, North Carolina
Department of Water & Power of  the City of Los Angeles, California
East Bay  Municipal Utility District, Oakland, California
Environmental Health Centre, Ottawa, Ontario,  Canada
Environmental Health Services Laboratory,  Edmonton, Alberta, Canada
Erie County Health Laboratory,  Buffalo, New York
FMC Corporation, Pocatello,  Idaho
FWPCA,  College, Alaska
FWPCA,  Evansville, Indiana
FWPCA,  Pomona, California
FWPCA,  Wheeling,  West Virginia
First U.  S. Army Medical Laboratory, Ft.  George G. Meade,  Maryland
Fish-Pesticide Research Laboratory,  Columbia,  Missouri
Fourth U. S.  Army Medical Laboratory, Ft. Sam Houston, Texas

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Goodyear Atomic Corporation,  Piketon, Ohio
Hach Chemical Company, Ames, Iowa
Hackensack Water Company, New Milford, New Jersey
Hammond-Montel Inc.,  Elmhurst, New York
Havens and Emerson, East  Paterson, New Jersey
Hawaii Department of Health,  Honolulu
Holzmacher, McLendon & Murrell, Melville,  New York
Houston City Health Department Laboratory,  Texas
Illinois Department of Public Health,  Chicago
Illinois State Water Survey,  Peoria
Indiana State Board of Health, Indianapolis
Industrial Chemicals, Inc. ,  South Bend,  Indiana
INFILCO,  Tucson,  Arizona
Institute of Health Laboratories,  Hato Key, Puerto Rico
Isotopes -  A Teledyne Company,  Sandusky, Ohio
Johns-Manville Research &  Engineering Center, Manville, New Jersey
Kentucky State Department of Health,  Frankfort
Lawrence Experiment Station, Massachusetts
Lincoln-Lancaster City Health Department,  Nebraska
Long Beach Water Department,  California
Los Angeles County Flood Control,  California
Los Angeles Department of  Public Works, Playa Del Rey, California
Louisiana State Board of Health,  New Orleans
Louisville  Water Company,  Kentucky
Maryland  Department of Water Resources, Annapolis
Maryland  State Department  of Health,  Baltimore
Mekoroth  Water Company,  Bnei-Brak, Israel
Metropolitan Corporation of Greater Winnipeg, Manitoba
Metropolitan St. Louis Sewer District, Missouri
Metropolitan Utility District, Omaha,  Nebraska
Michigan Department of Public Health, Lansing
Minneapolis Water Department,  Minnesota
Minnesota  Department of Health, Minneapolis
Monroe County Health Department Laboratory, Rochester, New York
Montana Bureau of Mines &  Geology,  Butte
Montana Health Department, Helena
Moutrey & Associates, Inc., Tulsa, Oklahoma
Nalco Chemical Company, Chicago, Illinois
Nassau County Department of Health,  Hempstead, New York
Nevada Health Division, Reno
New Hampshire Water Supply &  Pollution Control,  Concord
New Jersey State Department of Health, Trenton
New Mexico Bureau of Mines, Socorro
New York State Conservation Department, Avon
New York State Department  of Health, Albany
North Jersey District Water Supply Commission, Wanaque, New Jersey
Ohio Department of Health,  Columbus

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Ontario Water Resources Commission,  Rexdale
Orange County Air Pollution Control District, Anaheim,  California
Oregon State Board of Health, Portland
Pacific Engineering Laboratory, San Francisco, California
Pan American World Airways,  Patrick AFB, Florida
Pennsylvania Department of Health, Harrisburg
Pennsylvania State University,  University Park, Pennsylvania
Philadelphia Suburban Water Company,  Bryn Mawr,  Pennsylvania
Philadelphia Water Department, Pennsylvania
Puerto Rico Aqueduct and Sewer Authority, San Juan
Rensselaer Polytechnic Institute, Troy, New York
Reynolds Electric and Engineering Company, Las Vegas, Nevada
Sandia Laboratories, Albuquerque,  New Mexico
Sanitary Bacteriology Laboratory, Springfield, Illinois
Seattle Water Department,  Washington
Scientific Research Council,  Kingston, Jamaica, W. I.
South Carolina Pollution Control, Columbia
South Carolina State Board of Health,  Columbia
Springwells  Filtration Plant,  Dearborn, Michigan
St. Louis County Water Company,  University City,  Missouri
State Department of Health, Bismarck,  North Dakota
State Department of Public Health, Montgomery, Alabama
State Department of Water  Resources, Sacramento,  California
State Water  Survey Division, Urbana, Illinois
Sydney Water Board, Australia
TVA Water Quality Laboratory,  Chattanooga,  Tennessee
Tennessee Stream Pollution Control,  Nashville
Tenth U. S.  Army Medical Laboratory, APO, New York, New York
Texas  Gulf Sulphur Company, Aurora, North Carolina
The Anaconda Company, Grants,  New Mexico
The Procter & Gamble Company, Cincinnati, Ohio
The Water Commission, Kingston, Jamaica,  W. I.
USAF Environmental Health Laboratory, McClellan AFB, California
USAF Environmental Health Laboratory, Kelly AFB,  Texas
USPHS, Winchester, Massachusetts
U. S. Army Environmental  Hygiene Agency,  Edgewood Arsenal,  Mary-
 land
U. S. Geological Survey, Columbus, Ohio
U.S. Geological Survey, Denver, Colorado
U.S. Geological Survey, Harrisburg,  Pennsylvania
U. S. Geological Survey, Little Rock,  Arkansas
U. S. Industrial Chemicals  Company,  Tuscola,  Illinois
U.S. Pipe and Foundry Company, Birmingham, Alabama
University of Arizona,  Tucson
University of California, Berkeley
University of California, Richmond
University of Dayton,  Ohio
                                 XII

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University of Massachusetts,  Amherst
University of Wisconsin,  Madison
Utah State Division of Health, Salt Lake City
Virginia State Water Control Board,  Richmond
Washington State Department  of Health,  Seattle
Washington State University,  Pullman
Water Purification Laboratory,  Chicago, Illinois
Water Resources Division,  Charleston,  West Virginia
Water Service Laboratories,  Inc.,  New York, New York
Williams and Works,  Grand Rapids,  Michigan
Yonkers Water Bureau Laboratory,  New York
                                xiii

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                             ABSTRACT

       In this study each participant received three polyethylene cubi-
tainers containing samples to be analyzed for total alkalinity,  pH,
specific conductance, and total residue after drying at both 104 and
180C.  A total of 150 participants submitted results indicating that
the potentiometric method is the best and methyl orange the poorest
endpoint  indicator for alkalinity titration; pH and specific conductance
are accurately and precisely measured by all currently popular  instru-
ments; and total residue can be  accurately and precisely measured if
something is known about the  composition of the sample and, accordingly,
the correct temperature and drying time are used.

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                     WATER PHYSICS NO. 1

                     DESIGN OF THE STUDY

       In this study each participant received three polyethylene cubi-
tainers containing samples to be analyzed for total alkalinity, pH,
specific conductance, and total residue after drying at both 104  and
180C.

       The samples were designed in such a way that a firm theoreti-
cal value for each determination would be provided by at least one of
the samples.  The remaining values were determined empirically.

       Sample 1 was a 0. 001M solution of KC1, the  standard reference
for specific conductance. Sample 2 was a pH 6. 8 Clark and Lubs
phosphate buffer diluted  1:25. Sample 3 was a pH 8. 7 Clark and Lubs
borate buffer diluted 1:5. A slight increase in pH was observed, how-
ever, when the buffers were diluted, and hence, the samples  were  of
slightly higher value as indicated in Table 1.  The sample design pro-
vided values in the range likely to be encountered in potable water
analysis.  These  values  are shown in Table 1.

               Table 1.  COMPOSITION OF SAMPLES

  Parameter Measured            Sample 1    Sample 2    Sample 3
Total Alkalinity^**

pH
Specific Conductance(jumhos/cm)
mg/1 Total Residue at 104 C
mg/1 Total Residue at 180 C
0

4. 72
147
75
75
47.3

6. 87
303
293
293
141.6

8.80
228
500
468
       Participants were requested to use only methods described in
the 12th edition of Standard Methods for the Examination of Water and
Wastewater.
                   TREATMENT OF THE DATA

       After the results of analysis were received, the data were coded
and analyzed by computer for normality of distribution and  subsequent
rejection of outliers (see Appendix C) that were nonrepresentative be-
cause of errors in calculation, dilution, or other indeterminate factors.

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       It was observed that many participants submitted results for
total alkalinity that were high by a nearly constant value for all three
samples.  Since the value for sample 1 should have been zero,  it was
felt that the nearly constant error might  be due to a failure to determine
a titration blank.  Accordingly, a correction was calculated for all
laboratories reporting more than 1 mg/1 alkalinity in sample 1,  by
subtracting the value submitted for sample 1 from all three sample
values. These results  are reported  as corrected alkalinity.

       The results for  each method were also plotted on normal prob-
ability paper as a visual check on normality of distribution and  the
possible presence of outliers.

       Bar graphs are  included in the text for methods involving 10 or
more values,  to provide a pictorial display of the data.  Rejected values
are indicated by broken bars or labelled  as outliers, and values are
given for bars  off the scale of the chart.


                    DISCUSSION OF RESULTS

TOTAL ALKALINITY (Tables 2-4, Figures  1-15)

       The majority of participants used a potentiometric  end-point  to
measure total alkalinity.  Approximately equal numbers used methyl
orange and mixed indicator,  and a few used  methyl purple  indicator.

       All methods produced significantly high mean values for sample
1, which contained zero alkalinity.  The  methyl orange results  were
significantly less precise than the others, and the potentiometric re-
sults were the best.

       For sample 2, containing 47.30 mg/1 alkalinity,  the methyl
orange results were unacceptably high and imprecise as shown by the
relative error of 17. 82 and the relative standard deviation of 15. 12.
The total error of 53. 5 indicates that methyl orange is unacceptable,
while the total errors of 16. 2 for mixed  indicator,  16. 6 for potentio-
metric titration,  and 12. 7 for methyl purple are all excellent.  How-
ever, all mean values are significantly high.

       In sample  3, containing 141. 60 mg/1 alkalinity, there was no
significant difference in precision among the four methods but,  sur-
prisingly, methyl orange had a slightly lower standard deviation than
the others.  Again,  all means are  significantly high.

       Participants reporting more than 1 mg/1 alkalinity in sample 1
seemed to  have a  similar error in the results for samples 2 and 3.
Assuming that this error might be due to failure to determine the

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titration blank, a corrected alkalinity calculation was performed for
all results showing more than 1 mg/1 alkalinity in sample 1 by sub-
tracting the value submitted for sample 1 from all three sample values.
For  sample 1,  of course, all corrected alkalinity values were zero.
For  sample 2,  a great improvement  in accuracy was obtained for all
methods but only methyl orange showed a great improvement in pre-
cision.  The total errors now categorize all methods as excellent.
The  corrected values for sample 3 likewise showed a great improve-
ment in accuracy but little change in precision.  Again, all methods
are excellent according to the small  total errors.

       The most frequent comment offered by participants was that
the methyl orange endpoint was very difficult to detect. The validity
of this complaint is substantiated by  the data.


pH (Tables 5-7, Figures 16-25)

       The results for pH measurement were excellent.  Samples 2
and 3, being buffered solutions, were measured  with slightly greater
accuracy and precision than sample 1,  which was simply a solution of
potassium  chloride.  Even for  sample 1, however, the overall relative
error was  only 1. 59% and the relative standard deviation was 3. 89%.
There are  no significant differences  between the various instruments
used but if they are ranked according to the sum of total errors  for all
3 samples, the most expensive, Orion 801,  is first and the very old
Beckman H-2 is last.  However, this represents a range of average
total error of only 3.4 to 6.4 percent.

       There were no comments offered by the participants for  the
measurement of pH.

SPECIFIC  CONDUCTANCE  (Tables 8-10, Figures 26-35)

       Specific conductance is a measure of a water's capacity to con-
vey an electric current,  and is related to the total concentration of the
ionized substances in a  water and the temperature at which the measure-
ment is made.  Many participants were  upset by the unusual ratio of
total residue to specific conductance. However,  specific conductance
is more directly related to ionizable  substances than to total dissolved
substances and the conductance due to hydrogen ion and hydroxyl ion
are much greater than those due to other ions; hence, no direct  rela-
tionship exists.

       The specific conductance measurement was performed by 126
participants employing a variety of instruments.   No significant differ-
ence in performance of the instruments  was observed. However, the
                                                                 21

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YSI-31 instrument produced lower mean values for all three samples
than any other instrument, and had the least mean error in 2 of the
samples. The total error indicates that all instruments produce excel-
lent accuracy and precision.   The precision is similar for all three
samples as shown by the overall relative standard deviations of 8. 6,
7.8, and 8.4 for  samples 1,  2,  and 3 respectively.  The accuracy was
very similar for  samples 2 and  3 as shown by the overall relative errors
of 1. 9 and 3.0 respectively.   Less accuracy, as indicated by the overall
relative  error of 9.4, was obtained for sample  1.  Unfortunately, sample
1 was a 0.001 molar  solution of potassium chloride commonly used as
a reference solution for conductivity measurement and theoretically has
a conductance of  147. 0 ;umhos/cm.  The overall mean value of 160. 8
agrees closely with the value of 160.0 found by  the ARS  staff on checking
the sample after  several months. Apparently the sample absorbed CO-
or other gas  which  increased the conductance.


TOTAL RESIDUE (Tables 11-16, Figures 36-60)

       The determination of  the total residue on evaporation of a water
sample  appears to be a simple procedure.  It is,  however, one of the
more difficult analyses to replicate.  The type of materials  in the water
and the  drying time and temperature used determine the residue from a
given amount of material in solution.  Some  water of crystallization may
not be driven off  at low drying temperatures; most pronounced in highly
mineralized waters.  On the  other hand,  some solid salts  deposited may
be volatilized at the higher drying temperature; most important in waters
high in magnesium, chloride, and nitrate.  The use of 180 C as the drying
temperature  assures  complete conversion of bicarbonate to  carbonate
with loss of CO   and  HO. Therefore, the analyst must know the purpose
of the analytical result and should state the time and temperature of
drying.

       For this study,  the three samples typified three  different mecha-
nisms that may be encountered.  Sample  1, a solution of potassium chlo-
ride may lose chloride on prolonged or excessive heating.  This appar-
ently occurred at both 104 and  180 C when drying was extended beyond
24 hours.
       Excessive heating of sample 2, a solution of potassium dihydro-
gen phosphate and sodium hydroxide, may convert the KH PO. to KPO-
with a loss of HO.  The data indicates that at 104 this loss did occur
after approximately 16 hours of drying, and at 180  the loss occurred
within an hour.
       Sample 3, a solution of boric acid and sodium hydroxide, may
go through the most complex reaction of all.  After the stoichiometric
                                                                 45

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formation of sodium metaborate (NaBO2),  any excess boric acid loses
a mole of HO to form metaboric acid (HBO ) on drying at  100 C.
Upon further heating, additional water is lost with the conversion to
tetraboric acid (H0B  O_).  The data indicates that the calculated  loss
                 ^ 4 i
was  exceeded within one hour at 104, with a progressively greater
loss as the drying time was extended.  At  180, the calculated loss
was  exceeded only after more than 4 hours drying, with greater losses
occurring after prolonged drying.   Clearly,  no single set of conditions
will  serve for all water samples.

       Regardless of drying time  and temperature, the  results for
samples  2 and 3 would be considered excellent according to the low
total errors.  In general, a drying time of 1 1/2 to 4 hours at 180
appears to be preferable.  At 104, slightly more time such as 4 1/2
to 8  hours seems to be indicated.

       Sample 1, having failed to  perform exactly as predicted in the
other determinations  in the study,  must be suspect also in this deter-
mination. Although the corresponding total errors are substantially
greater,  the drying times and temperatures recommended above  still
appear to be valid. The results, while not excellent,  are acceptable.

       Proper technique, such as cleaning and conditioning the dishes,
and properly handling and cooling  the dishes after  drying the sample is
very important.   Of the many comments offered for this determination,
the most prevalent was to the effect that after drying at  180,  cooling
and weighing the dish was a critical part of the procedure.  This  was
especially true for sample 3 which became extremely hygroscopic and
could absorb moisture from  a desiccant that was not absolutely dry, or
from the air in the balance case if the weighing was not  done very
quickly.

       In addition to  the variables discussed herein, weight losses
might be due to volatilization of organic matter and gases from heat-
induced chemical decomposition, while a weight gain might be due to
oxidation.
 76

-------
              COMMENTS OF THE PARTICIPANTS

Total Alkalinity

1.  The "low alkalinity" method yielded a negative result on Sample 1.
    A titration curve was made and the sample was found to be past the
    equivalence point.

2.  Technicians found it easy to reproduce the appropriate end point
    pH with mixed indicator.

3.  Methyl orange produces a very poor endpoint.  Two drops of indi-
    cator were insufficient, so 5 drops were used.

4.  Fleisher methyl purple indicator was  used for this determination
    because color change from green to purple is easily noticed.

5.  End points, using either the mixed indicator or methyl orange, were
    very poor due to the use of a dilute titrant  (0. 02N H SO ).  The
                                                      i   4
    potentiometric plots were also far less than ideal for ascertaining
    the endpoint.  Perhaps, the best approach  would be to titrate a
    known volume of the sample to a specific pH value,  thereby reducing
    the errors associated with poor endpoints. The sluggishness in
    obtaining a well-defined endpoint could be readily monitored by
    potentiometric methods.  Also, the potentiometric method would
    permit the analyst to observe the presence of any buffering capacity
    in the  sample. Such phenomena are not readily discerned by the
    use of visual indicators.

6.  Methyl purple gives a more definite endpoint with boiler samples
    which may contain color.

7.  Methyl orange method has a very poor endpoint from  orange to pink.

8.  Xylene cyanol acts as  an intensifier for the methyl orange color
    changes.
    None
Specific Conductance

1.  A Sproule conductance cell of constant 1.0 and an Industrial Instru-
    ments platinized cell of constant 0. 1 both yielded similar results.
                                                                 77

-------
 2.   There is an abnormality of the ratio residue/specific conductance
     in Sample 3.

 3.   A drop of roughly 5 /umhos/cm occurred in all samples after 10
     days from the date of reported analysis.
 Total Residue

 1.   There were only minor changes between 60, 90, and 120 minute
     readings.

 2.   Sample No. 1 was run and checked twice at 105C.  The weight
     each time was 82 mg/1 and 81 mg/1.  When dried at 180C it in-
     creased in weight to 88 mg/1.   It was again dried at 105 C and re-
     tained its  weight of 88 mg/1.   For some reason it seems to have
     become more hygroscopic.

 3.   After drying for 16 hours, a further 24 hours drying resulted in no
     detectable change in weight.  Our standard practice is to employ
     porcelain  dishes and to dry overnight in an oven at  103-105C.

 4.   Samples were very hygroscopic after drying at 180C.

 5.   Changes in total residue from 105  to 180C of synthetic samples
     may not be analogous to changes of natural samples.

 6.   Samples were evaporated at 105 C instead of steam evaporation.
     Drying at  180 C was performed on separate portions after the
     pre-evaporation at  105C.  Samples were dried 2 additional hours
     at  180C.   No significant weight change was observed.

 7.   Porcelain dishes gained weight during storage over CaCl2  after
     being heated to 179-181C, and this gain was not related to the
     sample.

 8.   Constant weight achieved in 1  hour.  Test was carried out to 2 hours
     without any apparent change in weight.

 9.   Weight change after drying for second hour not greater than  0. 5 mg.,
     therefore,  constant weight considered attained after one hour drying
     time.

10.   When using the  179-181C temperature the weight at the end of 1
     hour drying time was always less than after 2 hours (after which
     it remained constant).
  78

-------
11.   All samples except No.  3 at 180C reached constant weight after
      1 hour.  Sample No.  3 attained constant weight after 2 hours.

12.   Immediate weighing as soon as cool is essential.  Platinum evap-
      orating dishes are essential for repeatability of tare weights of
      sample containers of samples being dried.

13.   Difficult to determine the correct weight of sample dried at 180C
      because of rapid uptake  of moisture from air.

14.   Conductivity vs residue  does not seem to be following a normal
      pattern.

15.   Increments of 1 hour drying time were used.  Sample 1 took 1  hour
      to achieve constant weight at both 103 C and 180C. Sample 2 took
      1 hour at 103 C and 2 hours at 180 C. Sample 3 took 2 hours at
      both 103 C  and 180 C.  Pyrex dishes were used.

16.   Sample 3 took 2 hours drying time for constant weight at each
      temperature; whereas the other samples took only 1 hour.

17.   These samples were  difficult to dry to constant weight,  due to
      hygroscopic characteristic.

18.   Suggest a drying time of 120-125C.   Moisture could be picked up
      in transfer from oven to dessicator quite readily at 179-181C.

19.   Although sample 3 was dried for 18 hours at 180C,  it never
      appeared completely dry.

20.   Sample 3 was apparently quite hygroscopic and had to be weighed
      "on the fly. "

21.   Constant weights were readily obtained after one hour of drying
      for all three samples, probably because the residues were very
      small (less than 30 mg.).

22.   Two hours drying was insufficient so we dried the  samples over-
      night (16 hours).

23.   Sample 1 is inexplicably lower at 103C than at 180C.

24.   We have found that a  cooled dish placed in the balance case, but
      not on the pan,  will send the optical scale up,  sometimes com-
      pletely out of sight.  The static charge will slowly leak away.  If
      one is not aware of this  phenomenon,  and places the dish directly
      on the pan,  the dish appears to gain weight as the charge leaks
                                                                79

-------
      away.  We intend to use staticmaster ionizing units both in the
      balance case and in the desiccator, but in the meantime are
      zeroing the balance,  placing the dish in the balance case but not
      on the pan, and periodically checking the zero setting.  The
      weighing is made only when the balance returns to its original
      zero point.  Room temperature has been 25C and relative
      humidity about 60%.  We realize the problems of desiccation,
      especially when a balance case does not provide the tightness of
      a desiccator.  We are using silica gel because the facilities  for
      the regeneration of magnesium perchlorate are not at hand and
      without  intolerable delays (and complicated modifications) desic-
      cator conditions are  not achieved in the balance case anyway.

25.   In all cases  1 hour drying resulted in constant weight.   Sample 2
      when tested  at 180 C showed greater lack of precision than 1 or
      3 in repeated trials.

26.   'Cooling' in  desiccator much over 1 hour has a tendency to increase
      weight.
                 SUMMARY AND CONCLUSIONS

      The measurement of total alkalinity tended to produce high results,
regardless of the means of endpoint detection; possibly caused by failure
to correct for the titration blank.   The use of methyl orange for endpoint
detection produced greater errors  than mixed indicator, methyl purple,
or potentiometric titration.

      The determination of pH presented no difficulty and there were no
significant differences between the various instruments used.  All pro-
duced excellent accuracy and precision.

      The specific conductance measurement likewise presented no diffi-
culty and all instruments used in the  study produced excellent accuracy
and prec Ision.

      In determining total residue, the temperature at which the residue
is dried and the length of time the residue is maintained at this temper-
ature,  in addition to the chemical and physical nature of the sample all
have an important bearing on the results. In general, constant weight
will be achieved in 1 1/2 to 4 hours at 180,  while at 104, 4 1/2 to 8
hours will be required.  The analyst  must select the temperature to
use after considering the purpose of the analysis and the type of residue
desired.  With careful technique,  excellent accuracy and precision can
be obtained.
80

-------
                         BIBLIOGRAPHY
A.  Alkalinity
    1.  Mixed Indicator.  Standard Methods for the Examination of
        Water and Wastewater, pp 48-52, 12th edition.  APHA, AWWA,
        WPCF.  New York,  1965.
    2.  Methyl Orange Indicator, ibid.
    3.  Potentiometric Titration, ibid.
    4.  Methyl Purple Indicator.
    5.  Other
B.  pH
    1.  Beckman Zeromatic Instrument, Glass Electrode Method.
        Standard Methods for the Examination of Water and Waste-
        water, pp 226-228.  12th edition.  APHA,  AWWA, WPCF.
        New York, 1965.
    2.  Beckman Expandomatic, ibid.
    3.  Orion 401, ibid.
    4.  Corning Model 12, ibid.
    5.  Beckman H-2,  ibid.
    6.  Orion 801, ibid.
    7.  Corning Model 7,  ibid.
    8.  Leeds and Northrup  7401, ibid.
    9.  Other
C.  Specific Conductance
    1.  Beckman RC 16 B2 Instrument,  Standard Methods for the
        Examination of Water  and Wastewater, pp  280-284.   12th
        edition.  APHA, AWWA, WPCF.  New York,  1965.
    2.  Beckman RC 16 Bl,  ibid.
    3.  Yellow Springs Instrument Model 31, ibid.
    4.  Radiometer CDM-2, ibid.
    5.  Leeds and Northrup  4866, ibid.
    6.  Other
                                                                81

-------
D.  Total Residue at 104 C
    1.  Dried for 1 hr.  Standard Methods for the Examination of
        Water and Wastewater, pp 244-245.  12th edition. APHA,
        AWWA,  WPCF.  New York, 1965.
    2.  Dried 1  1/2 to 4 hrs., ibid.
    3.  Dried 4  1/2 to 8 hrs., ibid.
    4.  Dried 8  1/2 to 16 hrs., ibid.
    5.  Dried 16 1/2 to 24 hrs., ibid.
    6.  Dried over 24 hrs., ibid.
E,  Total Residue at 180 C
    1.  Dried for 1 hr.  Standard Methods for the Examination of
        Water and Wastewater, pp 244-245.  12th edition. APHA,
        AWWA,  WPCF.  New York, 1965.
    2.  Dried 1  1/2 to 4 hrs., ibid.
    3.  Dried 4  1/2 to 8 hrs., ibid.
    4.  Dried 8  1/2 to 16 hrs., ibid.
    5.  Dried 16 1/2 to 24 hrs., ibid.
    6.  Dried over 24 hrs., ibid.
82

-------
APPENDICES
                              83

-------
                      APPENDIX A.
                 TABULATION OF RESULTS
      Table A-l.  Sample 1; Tota Alkalinity (0. 00 mg/liter)
LAB. NO.
1
2
4
5
5
5
5
S
9
5
5
S
6
7
9
9
9
9
9
9
10
13
1112
1125
RESULTS
0,0
0.0
2.2
3.0
0.0
0.0
1.0
1.0
1.0
1.0
2.5
.o
6.0
42.0
1.0
0.0
0.0
0.0
0.0
0.5
49*.0
0.0
3.0
0.2
METHOD
4
1
1
2
3
3
3
3
3
3
3
1
3
2
1
3
3
1
1
1
1
1
1
3
LAB. NO.
1124
1126
1136
1136
1211
1221
1222
1312
1314
1316
1322
1411
1511
1524
1711
1725
1816
1924
2112
2162
2222
2222
2223
2411
RESULTS
0.0
1.5
10.0
1.0
0.0
30.3
1.3
4.0
0.0
1.0
0.0
10.0
3.0
0.0
0.0
4.8
1.1
1.0
0.0
18.3
1.0
2.0
0.0
1.0
METHOD
1
2
2
4
3
2
1
1
3
1
3
2
2
1
3
3
3
4
1
2
3
2
3
2
84

-------
(Table A-l continued)
LAB. NO*
2526
2611
2626
2726
2811
2915
2926
3111
3116
3126
3211
3221
3222
3226
3311
3316
332Z
3326
3411
3415
3416
3426
3524
3611
RESULTS
5.0
0.0
0.6
18.0
6.8
8.0
0.0
3.7
3.0
0.0
0.0
0.0
0.5
1.0
13.0
9.4
20.0
0.0
2.0
40.0
0.4
0.0
12.2
1.3
METHOD
2
3
3
1
2
2
3
2
2
1
2
1
1
1
1
2
2
1
3
2
3
1
2
1
LAB. NO.
3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
4611
4623
4711
4716
4611
4821
4911
5111
5211
5221
5326
5426
5526
5611
RESULTS
5.0
2.0
3.2
3.0
0.0
6.0
0.0
1.7
2.0
2.0
3.0
2.0
7,0
3.0
0.0
10.0
1.5
2.5
0.0
1.0
2.0
3.0
3.0
2.0

2
1
3
3
3
2
1
2
3
2
3
3
3
3
4
2
3
3
3
3
2
4
3
1
                                        85

-------
                      (Table A-l continued)
LAB. NO,
5711
5711
5711
5811
5913
5963
6112
6115
6311
6314
6411
6536
6621
6622
6711
6715
6811
6812
6814
6816
6911
6914
6923
7112
RESULTS
3.3
1.0
2.0
6.0
0.5
0,0
4.0
0*0
1.0
0.0
1.0
0.5
3.0
1.5
1.0
3.0
1.0
4.5
0.5
2.1
1.4
0,5
2.0
0.0
METHOD
3
3
2
3
3
3
2
3
3
1
3
3
2
2
3
2
2
2
1
1
3
1
1
1
LAB. NO.
7123
7216
7222
7424
7512
7513
7522
7526
7622
7722
7813
7824
7846
7866
7866
7911
7914
7922
7926
8111
8112
8211
8222
8322
RESULTS
4,0
0.0
0,0
0,0
2.0
8.8
0.0
0.0
0,0
6.0
0.8
0.0
0.0
1.0
28.7
84.9
1.1
1.0
0,0
2.3
1.0
0.0
2.0
0.0
METHOD
2
3
3
3
3
2
3
3
2
2
3
3
2
4
2
2
3
3
3
3
1
3
1
3
86

-------

8342
8421
8512
8613
8622
8629
8725
8922
9113
9123
9215
9323
9525
RESULTS
2.0
1.0
2.0
0.3
12.0
0.3
0.0
0.5
2.0
4.4
0.0
4.9
0.0
METHOD
1
3
3
3
I
3
3
3
3
2
3
3
3

9922
9926
9526
9613
9715
9714
9714
9811
981*
9822
9829
9921
9921
RESULTS
1.0
0.0
0.0
3.5
1.0
0.0
0.0
12.0
0.0
9.0
2.8
5.2
5.5

3
3
3
2
1
1
3
2
2
1
2
1
1
87

-------
       Table A-2.  Sample 2; Total Alkalinity (47. 3 mg/liter)
LAB. NO*
1
2
4
5
5
5
5
5
5
5
5
S
6
7
9
9
9
9
9
9
10
IS
1112
1129
RESULTS
51.6
50.0
34.9
50.5
49.0
49.0
49.0
49.0
50.0
51.0
52.0
53.0
57.0
102.0
50.0
48.0
53.0
50.0
49.0
51.0
543.0
50.0
48.0
50.7
METHOD
4
1
1
2
3
3
3
3
3
3
3
1
3
2
3
3
1
1
1
1
1
1
1
3
LAB. NO.
1124
1126
1136
1136
1211
1221
1222
1312
1314
1316
1322
1411
1511
1524
1711
1725
1816
1924
2112
2162
2222
2222
2223
2411
RESULTS
50.0
54.0
49.0
56.0
51.0
79.8
48.8
51.0
48.9
50.8
49.0
62.0
49.0
49.5
46.8
40.2
52.2
52.0
48.0
79.3
50.0
47.0
55.2
50.0
METHOD
1
2
4
2
3
2
1
1
3
1
3
2
2
1
3
3
3
4
1
2
2
3
3
2
88

-------

2526
2611
2626
2726
2811
2919
2926
3111
3116
3126
3211
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
3426
3524
3611

54.0 2
48,0 3
48.6 3
73.0 1
59.8 2
59.0 2
49.4 3
52.8 2
52.0 2
49.0 1
61.0 2
50.0 1
46.5 1
50.7 1
68.0 1
63.4 2
80.0 2
54.0 i
50.0 3
52.0 z
48.4 3
37.5 1
50.5 2
52.0 i

3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
4611
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5426
5526
5611

45.0 2
50.0 1
47.7 3
48.0 3
48.0 3
54.0 2
50.0 1
51.4 2
51.0 3
50.0 2
50.0 3
49.0 3
58.0 3
54.0 3
50.0 4
56.0 2
51.3 3
55.0 3
49.0 3
52.0 3
54.0 2
52.0 4
53.8 3
54.0 1
89

-------
                      (Table A-2 continued)

5711
5711
5711
58U
5913
5963
6112
6115
63U
6314
6411
6536
6621
6622
6711
6715
6811
6812
681
6816
6911
6914
6923


50.0
50.1
52.0
60.0
45*5
50.0
51.0
51.3
48.0
50.4
56.0
46.3
51.0
48.5
48.0
54.5
50.0
54.0
52.0
46.7
50.0
50.6
50.0


3
3
2
3
3
3
2
3
3
1
3
3
2
2
3
2
2
2
1
1
3
1
1

LAB. NO.
7123
7216
7222
7424
7512
7513
7522
7526
7622
7722
7813
7824
7846
7866
7866
7911
7914
7922
7926
8111
8112
8211
8222
8322
RESULTS
15.5
51.0
47,0
50.2
50.0
53.7
49.5
60.8
48.0
56.0
64.9
50.0
54.6
50.5
70.3
131.2
51.2
53.0
49.3
51.3
49.5
48.0
58.0
48.4
METHOD
2
3
3
3
3
2
3
3
2
2
3
3
2
4
2
2
3
3
3
3
1
3
1
3
90

-------
(Table A-2 continued)
LAB. NO.
8342
8421
8512
8619
8622
8623
8723
8922
9113
9129
9215
9323
9923
RESULTS
43.0
50.0
50.0
52.0
60.0
52.2
48.0
49.0
50.0
50.0
51.7
54.0
47.0
METHOD
1
3
3
3
1
3
3
3
3
2
LAB. NO.
9526
9613
9715
9714
9714
9811
9816
9822
9829
9921
3 9922
3
3
9926

RESULTS
44.1
3.0
52.4
50.0
49.5
64.0
49.0
56.0
52.8
56.4
50.0
50.0


3
2
1
1
3
2
2
1
2
1
3
3

                                        91

-------
       Table A-3.  Sample 3: Total Alkalinity (141.6mg/liter)
LAB. NO*
1
2
2
4
5
9
5
5
5
5
5
5
5
6
7
9
9
9
9
9
9
10
13
1112
RESULTS
150.0
8.3
U8.0
139.5
U2.0
143.0
U7.0
H8.0
UB.O
148.0
149.0
148.0
147.0
152.0
214.0
K9.0
149.0
U5.0
U5.0
143.0
148.0
645.0
147.0

METHOD
4
4
1
1
3
3
3
3
3
3
3
1
2
3
2
1
1
3
3
1
1
1
1
1

1123
1124
1126
1136
1136
1211
1221
1222
1312
1314
1316
1322
1411
1511
1524
1711
1725
1816
1924
2112
2162
2222
2222
2223
RESULTS
148.6
150.0
148.0
148.0
151.0
150.0
139.4
143.3
146.0
143.6
147.7
141.5
152.0
140.0
149.5
145.7
112.5
151.5
148.0
147.0
201.5
142.0
146.0
151.1

3
1
2
4
2
3
2
1
1
3
1
3
2
2
1
3
3
3
4
1
2
3
2
3
92

-------
(Table A-3 continued)
LAB. NO.
2411
2526
2611
2626
2726
2811
2919
2926
3111
3116
3126
3211
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
3426
3524
 ^ i ^
RESULTS
147.0
U5.0
146.0
146.0
125.0
153.3
150.0
146.1
145.0
148.0
147.0
183.0
148.0
138.0
147.3
152.0
164.1
200.0
153.0
146.0
149.5
147.6
104.0
145.9
METHOD 1
,
2
3
3
1
2
2
3
2
2
1
2
1
1
1
1
2
2
1
3
2
3
1
2 	
LAB. NO.
3611
3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
4611
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5426
5526
RESULTS
150.0
128.2
146.0
140.6
135.0
146*0
152.0
147.5
146.8
149.0
144.0
147.0
145.0
154.0
150.0
140.0
150.0
149.5
153.0
145.1
151.0
148.0
152.0
152.2

1
2
1
3
3
3
2
1
2
3
2
3
3
3
3
4
2
3
3
3
3
2
4
3
  ^
                                          93

-------
                      (Table A-3 continued)
LAB. NO. "
5611
5711
5711
5711
5811
5913
5963
6112
6115
6311
6314
6*U
6536
6621
6622
6711
6715
6811
6812
681*
6816
6911
6914
6923
RESULTS
1*9.0
152.6
155.0
1*8.0
17*. 0
133.0
1*9.0
1*3.0
1*8.0
1*2.6
1*9.2
1*0.0
141.2
1*6.0
1*8.5
1*8.0
152.5
1*6,0
152.0
1*8.5
137.1
1*7.0
1*8.8
1*8.0
METHOD I
1 1
3 1
2 1
3 1
3 1
3 1
3 1
2 1
3 1
3 1
1
3
3 1
2
2
3
2
2
2
1
1
3
1
1 !
_ LAB. NO.
7112
7123
7216
7222
7*2*
7512
7513
7522
7526
1 7622
7722
7813
782*
78*6
7866
7866
7911
791*
7922
7926
8111
8112
1 8211
1 8222
RESULTS
1*8.0
1*5.0
1*9.5
139.9
1*9.0
1*6.0
151.1
1*1.*
178.9
1*5.0
150.0
10.3
1*7.0
1*7.0
153.6
1*7.5
229.7
1*8.7
15*. 5
1*7.8
1*7.3
1*7.0
1*6.0
170.0
METHOD.
I
2
3
3
3
3
2
3
3
2
2
3
3
2
2
*
2
3
3
3
3
1
3
1
.^^^v^ 
94

-------
LAB. NO.
^ 
8322
8342
8421
8512
861S
8622
8629
8723
8922
9113
9123
9215
9323
RESULTS
  ^ 
U6.0
127.5
150.0
U8.0
150.0
152.0
154.3
U4.0
173.0
148.0
143.4
149.0
151.0
METHOD
^  
3
1
3
3
3
1
3
3
3
3
2
3
3
LAB. NO.
9529
9526
9619
9715
9714
971*
9811
981C
9822
9829
9921
9922
9926
RESULTS
140.0
136.5
87.0
149.5
147.6
145.5
154.0
145. 0
154.0
148.8
152.6
145.0
150.1
METHOD
3
3
2
1
1
3
2
2
1
2
1
3
3
95

-------
Table A-4. Sample 1: oH (4. 72)
LAB. RC.
1
2
4
?
5
S
9
S
S
S
S
9
6
t
9
9
9
9
9
9
9
10
IS
1112
RESULTS
A. 50
4. 43
4.60
4.90
4.90
4. BO
4. SO
4.85
4.88
4.90
4.98
5.02
4.95
5.00
4.50
4.89
4.93
4.50
4.88
4.91
4.92
4.60
4.67
4.90
METHOD
3
4
9
2
2
1
1
7
7
7
7
1
7
9
3
3
3
3
4
4
4
8
4
1
LAB. NO.
1123
1124
1126
1136
1211
1221
1222
1312
1314
1316
1322
1411
1511
1524
1711
1725
1816
1924
2112
2162
2222
2222
2223
2411
RESULTS
4.40
4.77
4.85
4.93
4.90
4.9
4.45
4.80
4.92
4.83
4.75
4.65
4.80
4.84
6.11
4.93
4.80
4.80
4.90
4.90
4.84
4.78
4.80
4.84
METHOD
9
9
3
9
9
9
9
8
9
4
1
9
1
9
4
9
7
9
1
2
4
4
1
9
96

-------
(Table A-4
LAB. NOt
2411
2526
2611
2626
2726
2811
2919
2921
3111
3116
3126
3211
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
3426
3524
RESULTS
4.90
6.55
4.50
4.70
4.80
4.25
6.74
4.88
4.84
4.40
4.70
5.00
4.90
5.10
4.80
4.80
4.78
4.60
5.07
4.95
4.83
4.70
3.82
5.05
METHOD
2
1
2
5
9
9
9
2
4
1
1
9
5
9
9
9
9
9
9
1
2
3
9
9
LAB. NO.
3611
3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
4611
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5426
5526
RESULTS
4.90
5.12
4.80
5.40
4.85
4.60
4.70
4.59
4.83
4.72
4,70
4.81
4.90
5.00
4.80
5.30
4.73
4.85
*.77
4.80
5.09
4.70
4.80
4.81
METHOD
6
2
5
2
1
1
8
2
9
9
2
1
2
1
8
9
2
6
9
5
1
5
1

                                       97

-------
                      (Table A-4 continued)
LAB. NO.
5611
5711
5711
5711
5811
5919
5969
6112
6115
6311
6314
6411
6536
6621
6622
6711
6715
6811
6812
6814
6816
6911
69l
6929
RESULTS
A. 60
4.45
5.05
4.80
4.90
4.67
4.40
4.82
4.22
4.78
4.70
4.90
4.65
4.90
4.87
4.90
4.91
5.00
4.55
4.80
4.75
4.97
4.65
4.82
METHOD
9
9
7
1
1
9
2
6
9
1
9
7
5
3
9
1
9
9
9
9
1
4
1
6
LAB. NO.
7112
7123
7216
7222
7424
7512
7513
7522
7526
7622
7722
7813
7824
7846
7911
7914
7922
7926
7926
8111
8112
8211
8222
8322
RESULTS
4.77
4.70
4.80
4.88
4.50
5.10
4.80
4.65
4.10
4. BO
5.10
4.74
4.84
4.81
4.70
4.73
4.91
4.98
4.95
4.90
4.95
4.80
5.00
5.10
METHOD
9
3
9
9
9
1
1
9
1
6
5
6
9
9
9
1
8
1
9
8
1
1
9
9
98

-------
(Table A-4 continued)
LB. NO. RESULTS METHoD
8342 4.80 3
8421 4.70 1
8312 4.95 9
8613 4.60 3
8622 4.85 9
8623 4.69 9
8723 4.90 2
8922 4.81 6
9113 4.90 1
9123 4.75 6
9215 4.60 9
9323 4.75 6

9323 4.90 3
9526 4.60 9
9613 4.52 2
9713 4.40 i
971* 4.99 9
9811 4.90 2
981 4,50 9
9822 4.90 9
9825 4.80 9
9921 4.22 9
9922 4.97 5
992 4.55 2
                                        99

-------
                Table A-5.  Sample 2: pH (6. 87)
LAB. NO.
1
2
4
9

9
f
f
5
5
9
5
6
7
9
9
9
9
9
9
9
10
IS
1112
RESULTS METHOD
6.80 3
6.71 4
6.65 9
7.00 2
7.00 2
6.90 1
6.90 1
6.76 7
6.80 7
6.80 7
6,94 7
6.92 1
7.00 7
6.95 9
6.88 3
6.89 3
7.07 3
6.83 3
6.87 4
6.88 4
6.88 4
6.80 8
6.73 4
6.81 1
LAB. NO.
1123
1124
1126
1136
1211
1221
1222
1312
1314
1316
1322
1411
1511
1524
1711
1725
1816
1924
2112
2162
2222
2222
2223
2411
RESULTS
6.50
6.98
6.95
6.95
6.90
6.95
6.94
7.00
7.00
7.05
7.00
6.80
6.80
7,00
8.31
6.95
6.73
7.00
6.90
7,00
6.98
6,97
6.90
6.99
METHOD
9
9
3
9
9
9
9
8
9
4
1
9
I
9
4
9
7
9
1
2
4
4
1
9
100

-------
(Table A-5 continued).
LAB. NO.
2411
2926
2611
2626
272
2811
2913
2926
3111
3116
3126
3211
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
342*
3524
RESULTS
7.00
6.65
6.70
6.90
7.15
6.45
6.96
7.00
6.96
6.60
6.90
7.10
6.90
7.00
7.01
6.90
6.94
6.80
7.04
7.00
6.94
6.70
6.11
7.05
METHOD
2
1
2
5
9
9
9
2
4
1
1
9
5
9
9
9
9
9
9
1
2
3
9
9

3611
3711
3731
3611
4111
4112
4226
4314
4421
4511
4516
4611
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5426
5526
RESULTS
6.97
7.12
6.98
6.80
6.92
6.70
6.85
6.81
6.97
6.90
6.80
7.00
6.80
7.00
6.90
6.80
6.98
6.87
7,00
6.71
7.07
6.80
6.99
6.86
METHOD
6
2
5
2
1
1
8
2
9
9
2
1
2
1
8
9
2
6
9
5
1
5
1
9
                                        101

-------
                      (Table A-S^ontlnued)
LAB. NO.
5611
5711
5711
5711
5811
5913
5963
6112
6119
6311
6314
6411
6536
6621
6622
6711
6715
6811
6812
6814
6814
6911
6914
6923
RESULTS
7.00
7.00
6.75
7.00
7.00
6.97
6.30
7.03
7.01
7.00
6.90
7.00
6.75
7.00
7.02
7.00
6.99
6.99
7.05
6.92
6.95
7.00
6.90
6.52
METHOD
9
1
9
7
1
9
2
6
9
1
9
7
5
3
9
1
9
9
9
9
1
4
1
6
LAB. NO.
7112
7123
7216
7222
7424
7512
7513
7522
7526
7622
7722
7813
7824
7846
7911
7914
7922
7926
7926
8111
8112
8211
8222
8322
RESULTS
6.83
6.S8
6.96
6.90
6.72
7.00
6.90
6.80
6.38
7.00
7.20
6.88
6.97
6.99
6.90
6.86
6.91
6.95
7.02
6.81
6.97
7.00
6.90
6.65

9
3
9
9
9
1
1
9
1
6
5
6
9
9
9
1
8
9
1
8
1
1
9
9
102

-------
(Table A-5 continued)
LAB. NO.
8342
8421
8512
8613
8622
862S
8723
8922
9119
9129
9215
9323
RESULTS
7.00
7.00
7.00
6.80
6.90
6.75
6.92
7.03
7.00
7.02
6.83
6.90
METHOD
3
1
9
3
9
9
2
6
1
6
9
6
LAB. NO.
952S
9526
9618
971S
971*
9811
9810
9822
9825
9921
9922
9924
RESULTS
7.00
6.80
6.94
6.71
6.98
7.06
6.70
6.90
6.96
6.91
6.88
6.70
METHOD
3
9
2
1
9
2
9
9
9
9
5
2
                                       103

-------
                  Table A-6.  Sample 3; pH (8.80)
LAB. NO.
1
4
$
9
5
5
5
5
5
5
9
<
7
9
9
9
9
9
9
9
1C
19
1112
1123
RESULTS
8.70
8.41
8.73
8.80
8.90
8.60
8.48
8.60
8.60
8.72
8.60
8.85
8.90
8.71
8.80
8.81
8.82
8.81
8.82
8.85
8.60
8*41
8.50
8.60
METHOD
3
9
1
2
2
1
7
7
7
7
1
7
9
3
3
3
3
4
4
4
8
4
1
9
LAB. NO.
1124
1126
1136
1211
1221
1222
1312
1314
1316
1322
1411
1511
1524
1711
1725
1816
1924
2112
2162
2222
2222
2223
2411
2411
RESULTS
8.70
8.75
8.84
8.70
8.68
8.80
8.80
8.80
8.89
8.80
8.60
8.60
8.85
10.08
8.75
8.35
8.90
8.80
8.75
8.70
8.74
8.80
8.81
8.80
METHOD
9
3
9
9
9
9
8
9
4
I
9
1
9
4
9
7
9
1
2
4
4
1
2
9
104

-------
(Table A-6 continued)

2526
2611
2626
272*
2811
2919
2926
3111
3116
3124
3211
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
3426
3524
3611
RESULTS
8.70
8.50
8.80
8.75
8.10
8.71
8.81
8.78
8.30
8.70
8.70
8.80
8.80
8.82
8.80
8.89
8.60
8.88
8.80
8.68
8.40
7.73
8.65
8.78
METHOD
1
2
5
9
9
9
2
4
1
1
9
5
9
9
9
9
9
9
1
2
3
9
9
6
LAB. NO.
3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
4611
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5426
5526
5611
RESULTS
8.88
8.81
8.5Q
8.82
8.60
8.60
8.59
8.87
8.78
8.40
8.90
8.^0
8.85
8.80
8.60
8.77
8.66
8.80
8.34
8.72
8.60
8.82
8.68
8.60
METHOD
2
5
2
1
1
8
2
9
9
2
1
2
1
8
9
2
6
9
5
1
5
1
9

                                        105

-------
                      (Table A-6 continued)
LAB. NO.
5711
5711
5711
5811
5913
5963
6112
6115
6311
6314
6411
6536
6621
6622
6711
6715
6811
6812
6814
681*
6911
6914
6923
7112
RESULTS
8.55
8.70
8.75
8.70
8.77
7.90
8.72
8.85
8.80
8.85
8.80
8.60
8.80
9.14
8.80
8.80
8.83
8.85
8.80
8.70
8.83
8.65
8.55
8.61
METHOD
9
7
1
1
9
2
6
9
1
9
7
5
3
9
1
9
9
9
9
1
4
1
6
9
LAB. NO*
7123
7216
7222
7424
7512
7513
7522
7526
7622
7722
7813
7824
7846
7911
7914
7922
7926
7926
8111
8112
8211
8222
8322
8342
RESULTS
8.74
8.72
9.35
8.48
8.70
8.62
8.61
8.09
8.70
8.80
8.72
8.80
8.79
8.60
8.63
8.71
8.75
8.75
8.50
8.77
8.80
8.80
8.50
8.80
METHOD
3
9
9
9
1
1
9
1
6
5
6
9
9
9
1
8
1
9
8
1
1
9
9
3
106

-------
jTable A-6 continued)
LAB. NO. RESULTS METHoD
8421 8.70 1
8512 B.SO 9
8613 8.50 3
8622 8.65 9
8628 8.37 9
872S 8.78 2
8922 8.76 6
911S 8.70 1
912S 8.75 6
9215 8.75 9
9323 8.80 6
9528 8.90 3
LAB. NO. RESULTS METHOD
9524 8.55 9
9613 8.82 2
9715 8.48 l
9714 e.8o 9
9811 8.85 2
9816 8.50 9
9822 8.80 9
9821 R. 85 9
9921 8.78 9
9922 8.53 5
992 8.45 2

                                         107

-------
    Table A-7.  Sample 1; Specific Conductance (147 gmhos/cm)
LAB. NO.
I
2
4
!
9
5

6
7
9
10
15
1112
1125
1124
1136
1211
1221
1222
1312
1316
1322
1511
1524
RESULTS
173.0
168.9
146.0
163.0
147.0
120.0
ue.o
150.0
155.0
169.0
280.0
201.0
130.0
156.0
163.0
154.1
164.0
170.0
160.0
156.2
260.0
161.0
146.0
170.0
METHOD
6
1
1
1
1
6
1
6
6
1
6
5
6
6
4
1
5
1
3
6
6
6
1
4
LAB. NO.
1711
1816
1924
2112
2162
2222
2223
2411
2526
2611
2626
2726
2915
2926
3126
3222
3226
3311
3326
3411
3415
3416
3426
3611
RESULTS
165.6
168.1
165.0
168.0
158.0
158.0
160.3
166.0
186.0
171.1
129.0
163.0
151.8
168.4
164.0
150.0
169.0
150.0
170.0
146.0
172.0
140.0
150.0
150.4
METHOD
6
i
4
2
5
6
6
5
2
2
6
1
3
5
1
3
5
1
1
6
6
6
6
2
108

-------
(Table A-7 continued)
LAB. NO.
3711
3731
4111
4112
4314
4421
4911
4516
4611
462S
4711
4711
4811
4911
5111
5211
5221
5326
5526
5611
5811
5919
5968
6112
RESULTS
161.3
240.0
140.0
195.0
166.2
151.4
76,0
161.0
142.0
174.0
162. 8
160.0
150.0
156.0
154.0
159.5
140.0
150.0
199.0
155.0
320.0
163.2
150,0
150.0
METHOD
5
6
6
1
1
6
3
2
6
6
1
6
1
6
1
6
1
1
1
3
6
1
6
1
LAB. NO,
6115
6311
6314
6411
6621
6622
6711
6715
6811
6812
6814
6911
6914
6923
7112
7216
7222
7424
7512
7522
7526
7622
7722
7813
RESULTS
302.0
112.0
152.0
181.0
160.0
166.1
153,0
168.9
162.0
185*0
160.0
170.0
165.8
160.0
180.0
162.0
174.0
162.0
172.0
168.4
139,0
166,0
178.0
161.0
METHOD
1
1
6
1
1
6
2
2
1
5
6
6
6
6
6
6
1
6
6
5
6
2
6
6
                                        109

-------
                      (Table A-7 continued^
LAB. NO*
782*
784
7866
791*
7922
7926
8111
8211
8222
8322
8342
8421
8512
8619
8622
RESULTS
160,0
166.3
135.9
129.0
170.0
180.0
188.1
163.9
120.0
162.0
165.3
175.0
160.0
288.0
198.0
METHOD
4
2
1
6
3
6
6
2
6
6
1
1
6
6
6
LAB. NO.
8621
872S
8922
9113
9123
9323
9523
9526
9619
9713
9714
9816
9921
9922
9926
RESULTS
45.4
165.0
161.0
164.0
157.5
167.0
170.0
160.0
155.0
174.0
164.0
155.0
170.0
167.7
160.0

6
1
6
5
1
6
6
6
6
1
6
6
1
1
6
110

-------
Table A-8.  Sample 2: Specific Conductance (303 /umhos/cm)

I
2
4
5
9
*
9
<
7
t
10
13
1112
1129
1124
1136
1211
1221
1222
1312
1316
1322
1511
1524
RESULTS
340.0
317,1
265.0
315.0
262.0
250.0
260.0
280.0
309.0
324.0
300.0
356.0
260.0
302.0
322.0
298.6
318.0
330.0
298.0
303.0
300.0
312.8
178.0
325.0
METHOD
6
1
1
1
1
6
1
6
6
1
6
5
6
6
4
1
5
1
3
6
6
6
1
4
LAB. NO.
1711
1816
1924
2112
2162
2222
2223
2411
2526
2611
2626
2726
2915
2926
3126
3222
3226
3311
3326
3411
3415
3416
3426
3611
RESULTS
320.8
322.6
321.0
318.0
309.0
305.0
316.7
322.0
298.0
331.8
250.0
317.0
286.0
322.4
316.0
298.0
314.0
275.0
290.0
295.0
321.0
280.0
331.0
296.4
METHOD
6
i
4
2
5
6
6
5
2
2
6
1
3
5
1
3
5
1
1
6
6
6
6
2
                                                          111

-------
                      (Table A-8 continued)
LAB. NO*
37U
3731
4111
4112
4314
4421
4511
4516
4611
4623
4711
471*
4811
4911
5111
5211
5221
5326
5526
5611
5811
5913
5963
6112
RESULTS
339.0
460.0
279.0
315.0
310.6
361.3
117.0
310.0
320.0
332.0
320.7
320.0
300.0
300.0
290.0
311.0
273.0
280.0
386*0
290.0
530.0
307.4
315.0
300.0
METHOD
5
6
6
1
1
6
3
2
6
6
1
6
1
6
1
6
1
1
1
3
6
1
6
1
LAB. NO.
6115
6311
6314
6411
6621
6622
6711
6715
6811
6B12
6814
6911
6914
6923
7112
7216
7222
7424
7512
7522
7526
7622
7722
7813
RESULTS
273.0
162.0
287.0
344.0
320.0
308.2
303.0
319.1
312.0
364.0
311.0
320.0
326.3
310.0
330.0
321.0
318.0
314.0
317.0
321.1
275.0
324.0
312.0
305*4
METHOD
1
1
6
1
1
6
2
2
1
5
6
6
6
6
6
6
1
6
6
5
6
2
6
6
112

-------
(Table A-8 continued)
LAR. NO*
782*
7846
786*
7914
7922
7926
8111
6211
8222
8322
8342
8421
8512
8619
8622
RESULTS
300.0
312,4
250.8
251.0
320.0
340.0
372,0
307.7
270,0
313*0
295.8
320.0
300.0
321.0
302.0
METHOD
4
2
1
6
3
6
6
2
6
6
1
1
6
6
6
LAB. NO.
862i
872
8922
9119
9129
9323
9529
9926
9619
9713
9714
9816
9921
9922
9926
RESULTS
120.0
320.0
312.0
323.0
304,9
324.0
320.0
300*0
260.0
341.0
319.0
300.0
315.0
330.9
320.0
METHOD
6
1
6
5
1
6
6
6
6
1
6
6
1
1
6
                                        113

-------
    Table A-9.  Sample 3: Specific Conductance (228 ^mhos/cm)
LAB. NO.
1
2
4
5
5
5
%
6
1
9
16
13
1112
112S
1124
1136
1211
1221
1222
1312
1316
1322
1511
1524
RESULTS
255.0
238.1
200.0
210,0
240.0
leo.o
212.0
215.0
225.0
244.0
220.0
278.0
180.0
232.0
244.0
224.8
239.0
255.0
223.0
227.2
225.0
239.2
230.0
245.0
METHOD
6
1
1
1
1
6
1
6
6
1
6
5
6
6
4
1
5
1
3
6
6
6
1
4
LAB. NO.
1711
1816
1924
2112
2162
2222
2223
2411
2526
2611
2626
2726
2915
2926
3126
3222
3226
3311
3326
3411
3415
3416
3426
3611
RESULTS
240.0
247.4
242.0
245.0
234.0
230.0
242.0
245.0
226.0
248.9
182.0
245.0
217.5
238.3
242.0
225.0
242.0
210.0
250.0
220.0
245.0
220.0
251.0
234.0
METHOD
6
1
4
2
5
6
6
5
2
2
6
1
3
5
1
3
5
1
1
6
6
6
6
2
114

-------
(Table A-9 continued)
LAB. NO*
3711
3731
4111
4112
4314
4421
4511
4516
4611
4629
4711
47U
4811
4911
5111
5211
5221
5326
5526
5611
5811
5913
596S
6112
RESULTS
256.4
340.0
220.0
246.0
239. S
278.3
112.0
233.0
237.0
257.0
239.0
255.0
234.0
229.0
224.0
242.5
203.0
200.0
295.0
229.0
430.0
238.5
255.0
220.0
METHOD
5
6
6
1
1
6
3
2
6
6
1
6
1
6
1
6
1
1
1
3
6
1
6
1
LAB. NO.
6115
6311
6314
6411
6621
6622
6711
6715
6811
6812
6814
6911
6914
6923
7112
7216
72Z2
7424
7512
7522
7526
7622
7722
7813
RESULTS
208.7
160.0
218.0
263.0
235.0
218.0
226.0
247.1
236.0
271.0
237.0
240.0
248.2
235.0
250.0
243.0
247.0
237.0
254.0
242.0
210.0
245.0
252.0
232.5
METHOD
1
1
6
1
1
6
2
2
1
5
6
6
6
6
6
6
1
6
6
5
6
2
6
6
                                       115

-------
                       (Table A-9 continued)
LAB. NO*
7824
7846
7866
791*
7922
7926
8111
8211
8222
8322
8342
8421
8512
8619
8622
RESULTS
235.0
238,7
19U6
189.0
240.0
380.0
277,8
232.6
180.0
248.0
226.2
250.0
220.0
241.0
226,0
METHOD
4
2
1
6
3
6
6
2
6
6
1
1
6
6
6
LAB. NO.
8629
8729
8922
9119
9129
9323
9529
9926
9619
9713
9714
9816
9921
9922
9926
RESULTS
137.0
245.0
236.0
242.0
232.5
246.0
250.0
237.0
210.0
262,0
245.0
225.0
241.6
249.3
240.0
METHOD
6
1
6
5
1
6
6
6
6
1
6
6
1
1
6
116

-------
Table A-10.  Sample 1; Total residue at 104 C (75 mg/liter)
LAB. NO.
1
2
4
5
9
9
%
5
%
9
9

7
9
10
13
1112
1125
1124
1126
1136
1211
1221
1222
RESULTS
88,0
90,0
92.5
105,0
106.0
81,0
88.0
96.0
83,0
92.0
107.0
82.0
92.0
84.0
80.0
107.0
72.0
91.0
76.0
76.0
79.0
92.0
92.0
80.0
METHOD
5
1
2
1
1
2
1
2
1
5
5
2
4
2
3
1
5
4
4
2
2
1
5
3
LAB. NO.
1312
1314
1316
1322
1411
1311
1524
1711
1816
1924
2112
2223
2411
2526
2611
2626
2726
2811
2915
2926
3111
3116
3126
3211
RESULTS
97.0
101.0
114.2
82.0
78.0
113.0
84.0
90.8
38.0
82.0
83.0
97.0
84*0
70.0
81.0
92.0
224.0
39.6
8.4
85.9
87.0
78.0
86.0
100.0
METHOD
2
2
2
9
4
1
2
2
6
2
3
2
9
5
2
4
2
3
2
2
4
2
2
3
                                                           117

-------
                       (Table A-10 continued)
LAB. NO*
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
3426
3524
3611
3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
4611
RESULTS
80.0
55.0
74.0
84.0
68.4
120.0
77.5
84.0
113.0
90,0
348.0
86.0
85.4
83.0
72.0
88.0
2.1
88.7
48.0
83.5
95.0
82.0
88.0
46.0
METHOD
2
5
5
6
4
2
1
2
1
2
5
2
1
5
3
1
3
1
3
2
1
1
3
1
LAB. NO.
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5526
5611
5711
5711
5711
5811
5913
5963
6112
6115
6311
6314
6411
6536
RESULTS
63.0
89.0
86.0
80.0
82.0
89.5
76.0
87.2
78.0
60.0
103.0
84.0
86.0
90.0
79.0
80.0
106.0
110.0
80.0
82.0
88.0
87.0
76.0
88.0

4
5
3
2
1
3
1
2
2
1
4
1
5
2
2
2
4
5
1
2
2
2
1
3
118

-------
(Table A-10 continued)
LAB. NO.
6621
6622
6711
6715
6811
6812
681*
6816
6911
6914
6923
7112
7128
7216
7222
7424
7512
751S
7522
7526
7622
7813
7824
7846
RESULTS
79.0
78.0
93.0
86.5
130.0
86.0
88.0
116.0
72.0
89.0
95.0
90.0
87.3
83.5
83.0
81.6
98.0
72.4
81.0
80.2
84.0
84.0
79.0
86.0
METHOD
5
2
2
2
2
6
5
1
5
5
2
5
2
2
2
2
1
5
2
4
1
2
4
1
LAB. NO.
7866
7911
7914
7922
7926
8111
8112
8211
8222
8322
8342
8421
8512
8613
8623
8723
8922
9113
9123
9323
9523
9526
9613
9713
RESULTS
84.0
54.0
109.0
95.0
79.0
79.0
75.0
74.0
92.0
79.0
89.5
110.0
70.0
84.0
77.0
78.0
87.0
75.0
85.3
85.0
55.0
70.0
69.0
96.0
METHOD
2
5
1
5
4
4
5
4
4
4
5
5
1
2
2
5
5
5
5
2
5
5
2
2
                                       119

-------
                      (Table A-10 continued)
UAB. NO*   RESULTS   METHQD
                      LAB.  NO.    RESULTS   METHOD
  9714




  9811



  9816



  9822
86.0




90.0



46.0



74.0
9821



9921



9922



992*
84.0



88.0



64.0



68.0
4



2



2



2
 120

-------
Table A-11.  Sample 2; Total residue at 104C (293 mg/liter)
LAB. NOt
1
2
4
5
9
5
9
5
9
5
5
A
7
9
16
IS
1112
112S
1124
1126
1136
1211
1221
1222
RESULTS
297.0
297.0
302.5
301.0
307.0
273.0
293.0
304.0
289.0
309.0
310.0
293.0
176.0
285.0
320.0
316.0
331.0
298.0
286.0
290.0
352.0
312,0
309.6
292,0
METHOD
5
1
2
1
1
2
1
2
1
5
5
2
4
2
3
1
5
4
4
2
2
1
5
3
LAS. NO.
1312
1314
1316
1322
1411
1511
1524
1711
1924
2112
2222
2223
2411
2526
2611
2626
2726
2611
2915
3111
3116
3126
3211
3221
RESULTS
291.0
309.0
315.9
300*0
353.0
307.0
295.0
303.6
296.0
304.0
289.1
296.0
294.0
308.5
289.0
294.0
288.0
392.0
35.2
275.0
267.0
312.0
301.0
288.0
METHOD
2
2
2
5
4
1
2
2
2
3
2
2
5
5
2
4
2
3
2
4
2
2
3
2
                                                           121

-------
                      (Table A-11 continued)
LAB. NO.
3222
3226
3311
3316
3322
3326
3411
3415
3414
3426
3524
3611
3711
3731
3811
4111
4112
4226
4314
4421
45H
4516
4611
4629
RESULTS
243.0
296.0
304.0
299.4
320.0
282.5
296.0
309.5
290.0
596.0
302.3
296.6
286.0
294,0
288.0
3.8
300.7
260.0
342.0
299.0
293.0
289.6
252,0
325.0
METHOD
5
5
6
4
2
1
2
1
2
5
2
1
5
3
1
3
1
3
2
1
1
3
1
4
LAB. NO.
4711
4716
4811
4821
4911
5111
5211
5221
5326
5526
5611
5711
5711
5711
5811
5913
5963
6112
6115
6311
6314
6411
6536
6621
RESULTS
292.0
300.0
300.0
280.0
290.5
289.0
299.9
290.0
285.0
289.0
270.0
312.0
284.0
384.0
280.0
343.0
317.0
294.0
297.0
418.0
315.0
287.0
292.0
294.0
METHOD
5
3
2
1
3
1
2
2
1
4
1
2
5
2
2
4
5
1
2
2
2
1
3
5
122

-------
(Table A-11 continued)
LAB. NO*
6622
6711
6719
6811
6612
681*
6816
6911
6914
6923
7112
7128
7216
7222
7424
7512
7513
7522
7526
7622
7813
782*
7846
7866
RESULTS
288.0
309.0
298,0
283.0
276,0
304.0
331.0
286.0
337,0
295.0
298.0
261.5
290.5
298.0
290.0
276.0
271.2
302.0
290.3
299.0
295.0
285.0
302.0
289.0
METHOD
2
2
2
2
6
5
1
5
5
2
5
2
2
2
2
1
5
2
4
1
2
4
1
2
LAB. NO.
7911
7914
7922
7926
8111
8112
8211
8222
0322
8342
8421
8512
8613
8623
8723
8922
9113
9123
9323
9523
9526
9613
9713
9714
RESULTS
254.0
295.0
298.0
295.0
300.0
229.0
268.0
292.0
298.0
277.3
308.0
292.0
292.0
306.0
284.0
260.0
301.0
297.5
294.0
270.0
286.0
273.0
270.0
308.0
METHOD
5
1
5
4
4
5
4
4
4
5
5
1
2
2
5
5
5
5
2
5
5
2
2
5
                                       123

-------
                     (Table A-11 continued)
LflR.NO.   RESULTS   METHOD
                       LAB. NO.   RESULTS    METHOD
  9811



  9816



  9822



  9829
296.0



360.0



278.0



330.0
9921      300.0       2



9922      279.0       2



992*      280.0       2
 124

-------
Table A-12.  Sample 3; Total residue at 104^C (500 mg/liter)

I
2
4
5
5
9
5
$
5
5
5
6
7
9
18
19
1112
1129
1124
1126
113*
1211
1221
1222
RESULTS
511.0
501.0
501.5
488.0
504.0
453.0
484.0
494.0
490.0
501.0
498.0
497.0
372.0
490,0
924.0
513.0
563.0
482.0
481.0
484,0
529,0
504.0
488.8
479.0
METHOD
5
1
2
1
1
2
2
1
5
5
1
2
4
2
3
1
5
4
4
2
2
1
5
3
LAB. NO.
1312
1314
1316
1322
1411
1511
1524
1711
1816
1924
2112
2222
2223
2411
2526
2611
2626
2726
2811
2915
2926
3111
3116
3126
RESOtTT-
479.0
485.0
517.3
496.0
481.0
524.0
494.0
500.0
435.0
485.2
501.0
464.4
506.0
488.0
519.0
485.0
456,0
564.0
470.0
86.4
502.5
508.0
491.0
500.0
METHOD
2
2
2
5
4
1
2
2
6
2
3
2
2
5
5
2
4
2
3
2
2
4
2
2
                                                            125

-------
                      (Table A-12 continued)
LAB. NO.
3211
3221
3222
3226
3311
3316
3322
3326
3411
3415
3416
342
352*
3611
3711
3731
3811
4111
4112
4226
4314
4421
4511
4516
RESULTS
470.0
479.0
440.0
490.0
508.0
425.6
520.0
477,5
476.0
510.0
498.0
796.0
507.6
495.8
498.0
480.0
486.0
5.6
504,0
434.0
504.0
503.0
514.0
508.4
METHOD
3
2
5
5
6
4
2
1
2
1
2
5
2
1
5
3
1
3
1
3
2
1
1
3

4611
4623
4711
4716
4811
4821
4911
5111
5211
5221
5326
5526
5611
5711
5711
5711
5811
5913
5963
6112
6115
6311
6314
6411
RESULTS
454.0
481.0
492.0
496.0
500.0
480.0
479.0
486.0
496.2
480.0
470.0
481.0
493.0
478.0
456.0
495.0
490.0
519.0
503.0
500.0
499.0
482.0
500.0
474.0

1
4
5
3
2
1
3
1
2
2
1
4
1
5
2
2
2
4
5
1
2
2
2
1
126

-------
(Table A-12jx>ntinued)
LAB. NO*
6536
6621
6622
6711
6713
6811
6812
681
6816
6911
6914
6923
7112
7129
7216
7222
7424
7312
75U
7322
7526
7622
7818
7824
RESULTS
483.0
498.0
485.0
506.0
501.5
533.0
457.0
499.0
532.0
492.0
493.0
514.0
488.0
484.5
477,5
510.0
496.0
523.0
451.2
497.0
487.8
487.0
500.0
476.0
METHOD
3
5
2
2
2
2
6
5
1
5
5
2
5
2
2
2
2
1
5
2
4
1
2
4
LAB. NO.
7S46
7866
7911
7914
7922
7926
8111
8112
8211
8222
8322
8342
8421
S512
8613
8623
8723
8922
9113
9123
9323
9523
9526
9613
RESULTS
512.0
493.0
454.0
509.0
485.0
495.0
480.0
452.0
486.0
489.0
481.0
490.0
500.0
464.0
504.0
477.0
473.0
489.0
494.0
503.7
503.0
470.0
464.0
515.5
METHOD
1
2
5
1
5
4
4
3
4
4
4
5
5
1
2
2
5
5
5
5
2
3
5
2
                                        127

-------
                      (Table A-12 continued)
LAB. NO. RESULTS METHOD
9713 498.0 2
9714 496.0 5
9811 500.0 2
9816 644.0 2
9822 480.0 2
LAB. NO. RESULTS METHOD
9829 477.0 4
9921 599.0 2
9922 464.0 2
9926 450.0 2

128

-------
Table
LAB. NO.
1
2
4
5
5
5
S
5
S
6
7
9
10
13
1112
112S
1124
1126
1136
1211
1221
1222
1312
1314
A-13.
RESULT
83.0
92.0
91.5
82.0
6ltO
77.0
89.0
66*0
77.0
88.0
164.0
83.0
96.0
95.0
92.0
103.0
56.0
68.0
79.0
80.0
81.2
77.0
79.0
53.0
Sample 1: Total residue at 180 C
S METHOD
4
1
2
1
1
2
2
1
1
2
4
2
3
1
3
4
4
3
1
1
5
3
2
5
LAB. NO.
1316
1322
1411
1511
1524
1711
1816
1924
2112
2222
2222
2223
2411
2526
2611
2626
2726
2811
2915
2926
3111
3116
3126
3211

RESULTS
105.8
4.0
70.0
80.0
81.0
87.6
65.0
82.0
80.0
102.4
81.6
82.0
81.0
44.0
77.0
88.0
188.0
20.8
69.6
83.0
80.0
79.0
81.0
69.0
METHOD
2
2
4
1
2
2
6
2
3
1
2
2
5
6
2
4
2
5
2
2
6
2
2

129

-------
                      (Table A-13 continued)^
LAB. F)0
3221
3226
3311
3316
3322
3411
3415
3416
3426
3524
3611
3711
3731
3811
4111
4112
4226
4421
4511
4516
4611
4623
4711
4716
RESULTS
70.0
79.0
66.0
91.4
84.0
78.0
85.0
88.5
240.0
85.0
75.6
88.0
73.0
70.0
1.5
91.3
0.0
84*0
89.0
82.4
54.0
60.0
93.0
84.0
METHOD
5
1
6
3
2
2
1
2
2
2
1
5
2
2
2
1
2
1
2
3
1
4
5
3
LAB. NO.
4811
4821
4911
5111
5211
5221
5326
5526
5611
5711
5711
5711
5913
5963
6112
6115
6311
6314
6411
6536
6621
6622
6711
6715
RESULTS
75.0
70.0
54.0
72.0
80.3
81.0
45.0
81.0
85.0
80.0
50.0
77.0
43.0
85.0
74.0
78.0
20.0
82.0
66.0
86.0
80.0
80.3
87.0
86.0
METHOD
2
1
2
2
2
2
1
4
1
5
1
2
4
5
1
2
2
3
1
2
5
2
2
2
130

-------
(Table A-13 continued)
LAB. NO.
6811
6612
661^
6816
6911
6914
6923
7112
712S
7216
7222
742*
7512
7513
7522
7526
7622
7813
7846
7866
7911
791*
7922
7926
8111
RESULTS
132.0
82.0
88.0
83.0
70,0
89.0
85.0
84.0
62.2
70.0
80.0
61.2
83.0
82.4
72.0
81.3
90.0
72.0
82.0
79.5
123.0
91.0
80.0
71.5
76.0
METHOD
2
6
5
1
2
5
2
2
2
2
2
2
1
5
2
4
5
2
1
1
4
1
5
2
4
LAB. NO.
8112
8211
8222
8322
8342
8421
8512
8613
8623
8723
8922
9113
9123
9323
9526
9613
9713
9714
9811
9816
9822
9825
9921
9922
992
RESULTS
70.0
74.0
92.0
83.0
100.0
86.0
70.0
86.0
91.0
73.0
84.0
81.0
87.5
83.0
85.0
32.5
19.0
80.0
78.0
40.0
78.0
74.0
78.0
54.0
72.0

1
3
2
4
5
5
1
2
2
5
5
2
5
2
2
2
2
5
2
3
2
4
2
1
2
                                         131

-------
    Table A-14.  Sample 2; Total residue at 180C (293 mg/llter)
LAB. NO*
1
2
4
5
9
9
5
5
5
e
7
0
10
IS
1112
112S
1124
1126
1136
1211
1222
1312
1314
1316
RESULTS
287.0
292.0
291.5
277.0
80.0
247.0
287.0
259.0
272.0
277.0
34^.0
274.0
312.0
292.0
172.0
305.0
266.0
290.0
297.0
290.0
270.0
288.0
234.0
294.0
METHOD
4
1
2
1
1
2
2
1
1
2
4
2
3
1
3
4
4
3
1
1
3
2
5
2
LAB. NO.
1322
1411
1511
1524
1711
1924
2112
2222
2222
2223
2411
2526
2611
2626
2726
2811
2915
3111
3116
3126
3211
3221
3226
3311
RESULTS
208*0
287.0
247.0
272.0
286.0
283.6
296.0
282.8
276*0
287.0
269.0
262.0
282.0
272.0
272.0
306.0
24.8
257.0
285.0
287.0
255.0
267.0
283.0
272.0
METHOD
2
4
1
2
2
2
3
2
1
2
5
6
2
4
2
5
2
6
2
2
2
5
1
6
132

-------
jTable A-14 continued)

3316
3322
3411
3415
3416
342
3524
3611
3711
3731
3811
4111
4112
4224
4421
4511
4516
4611
4629
4711
47l
4811
4821
4911
RESULTS
311.2
240.0
264.0
275.5
275.5
476,0
291.3
269.7
281.0
285.0
280.0
2.9
282.0
198.0
289.0
282.0
256.8
225.0
261.0
270.0
287.0
290.0
257.0
266.0
METHOD
3
2
2
1
2
2
2
1
5
2
2
2
1
2
1
2
3
1
4
5
3
2
1
2
LAB. NO.
5111
5211
5221
5326
5526
5611
5711
5711
5711
5913
5963
6112
6115
6311
6314
6411
6536
6621
6622
6711
6715
6811
6812
6814
RESULTS
269.0
275.4
282.0
255.0
267.0
283.0
256.0
365.0
270.0
227.0
275.0
306.0
279.0
244.0
296.0
270.0
274.0
273.0
275.0
306.0
289.0
284.0
244.0
288.0

2
2
2
1
4
1
1
2
5
4
5
1
2
2
3
1
2
5
2
2
2
2
6
5
                                         133

-------
                     (Table^A-14 continued)
LAB. NO.
6816
69H
69l
6923
7112
7123
7216
7222
7424
7512
7513
7522
7526
7622
7813
78*
7866
7911
7914
7922
7926
8111
8112
8211
RESULTS
294.0
272.0
311.0
289.0
294.0
252.1
268.5
294.0
251.0
277.0
268.4
271.0
286.5
281.0
271.0
282.0
282.0
302.0
289.0
2
-------
Table A-15.  Sample 3: Total residue at 180C (468 mg/llter)
LAB. NOt
1
2
4
9
5
*
5
5
5
B
t
9
10
19
1112
1129
1124
112
113<
1211
1221
1222
1312
1314
RESULTS
477.0
486,0
483.5
470.0
457.0
448.0
474.0
467.0
467.0
475.0
324.0
469.0
946.0
479,0
455.0
495.0
455.0
454.0
499,0
472,0
474.4
453,0
475.0
426.0
METHOD
4
1
2
1
1
2
2
1
1
2
4
2
3
1
3
4
4
3
1
1
5
3
2
5
LAB. NO.
1316
1322
1411
1511
1524
1711
1816
1924
2112
2222
2222
2223
2411
2526
2611
2626
2726
2811
2915
2926
3111
3116
3126
3211
RESULTS
488.9
428.0
458.0
453.0
472.0
473.6
394.0
470.0
433.0
459*6
448*4
479*0
457,0
454.0
475.0
448.0
532.0
310.0
34.4
479.5
439*0
490.0
468.0
472.0
METHOD
2
2
4
1
2
2
6
2
3
1
2
2
5
6
2
4
2
5
2
2
6
2
2
2
                                                             135

-------
                      (Table A-15 continued)
LAB. NO.
3221
3226
3311
3316
3322
3411
3415
3416
3426
3524
3611
3711
3731
3811
4111
4112
4228
4421
4511
4516
4611
4629
4711
47l
RESULTS
454,0
472.0
444.0
430.6
480.0
444.0
472.5
489.0
732.0
^83.3
453.5
469.0
468.0
472.0
5.2
492.7
390.0
483.0
483.0
475,2
391.0
419,0
474,0
476,0
METHOD
5
1
6
3
2
2
1
2
2
2
1
5
2
2
2
1
2
1
2
3
1
4
5
3
LAB. NO.
4811
4821
4911
5111
5211
5221
5326
5526
5611
5711
5711
5711
5913
5963
6112
6115
6311
6314
6411
6536
6621
6622
6711
6715
RESULTS
480.0
455.0
447.7
467.0
468.1
484,0
450.0
456*0
467,0
486.0
448.0
450.0
391.0
457.0
500.0
477.0
482,0
462.0
466.0
465.0
465.0
468.0
489*0
482.5
METHOD
2
1
2
2
2
2
I
4
1
2
1
5
4
5
1
2
2
3
1
2
5
2
2
2
136

-------
(Table A-15 continued)

6811
6812
681*
6816
6911
6914
6923
7112
7125
7216
7222
7424
7512
7513
7522
7526
7622
78i
7846
7866
7911
7914
7922
7920
8111
RESULTS
475.0
413.0
485.0
477.0
478.0
489.0
487.0
400.0
461.4
456.0
446.0
415.0
514,0
464.4
470.0
469.0
475.0
464.0
404.0
473.0
380.0
479,0
467,0
474.0
443.0
METHOD
2
6
5
1
2
5
2
2
2
2
2
2
1
5
2
4
5
2
1
1
4
1
5
2
4
LAB. NO.
8112
8211
8222
8322
8342
8421
8512
8613
8623
8723
8922
9113
9123
9323
9526
9613
9713
9714
9811
9816
9822
9825
9921
9922
992*
RESULTS
450.0
459.0
484.0
469.0
446.6
469,0
462.0
478,0
486.0
441.0
425.0
466.0
473.3
474.0
459.0
456.5
358.0
468.0
450,0
625.0
448.0
458.0
484.0
441*0
444.0
METHOO
1
3
2
4
5
5
1
2
2
5
5
2
5
2
2
2
2
5
2
3
2
4
2
1
2
                                       137

-------
                          APPENDIX B.
              GLOSSARY OF STATISTICAL TERMS
    A glossary of statistical terms defined as they are used in this
report is presented to ensure uniformity of understanding.
Arithmetic mean
The sum of the sample results divided by the
number of results in the sample.  Let X^
(i = 1, 2, . .  . . n) denote the i^h results in a
sample  of n results.  The arithmetic mean
                                            _  n
                               _           _
                        denoted X is given by X = 2
Median
Accuracy
Measures of accuracy
Halfway point in the results when they have
been arranged in order of magnitude (the
middle result of an odd number of results,
or the average of the middle two for an even
number).

The correctness of a measurement, or the
degree of correspondence between the results
and the true value  (actual amount added).

Measures that relate to the difference
between the mean of the results and the true
value when the latter is known or assumed.
The following measures apply:

Mean error The average difference with
regard to sign between the results and the
true value.  Equivalently, the difference
between the mean of the results and the true
value (T. V.).

    Mean error =  X - T. V.
                        Relative error   The absolute value of the
                        mean error expressed as a percentage of
                        the true value.
                                            IX - T.V.I
                            Relative error = J	=ryl
                                X 100
Precision
The reproducibility of sample results or the
degree of agreement among the results.
 138

-------
Measures of precision   Measures of the variation among the sample
                        results themselves, i. e., the spread or
                        dispersion of the results without regard to
                        the true value.  The following measures
                        apply:

                        Sample variance  Sum of squared deviations
                        of the sample results  from their mean divided
                        by one less than the number of results in the
                        sample. The sample  variance denoted  s^
                        is given by

                                  n        -  2
                                  2   
-------
                        where X and s are the sample mean and
                        standard deviation, t a/2 is the upper a/2
                        point of "Student's" t-distribution,  and n
                        is the numbe_r of results in the sample used
                        to compute X.

                        Tolerance limits  Limits within which one
                        can state with probability / that at least a
                        proportion P of the entire population will
                        lie.  The upper and lower tolerance limits
                        are given by

                            Tolerance limits = X    Ks,

                        where K is the factor for two-aided tolerance
                        limits for normal populations.    The value of
                        K depends upon the chosen values of  -y and P.

Total error             A criterion for judging acceptability of ana- 3
                        lytical methods.  The total error is given by


                        Absolute value of mean error + 2(Std.  Dev.) ..  , _
                        	-	 A  1 UU
                                        True Value

                        On the basis of this total error, methods can
                        be divided into three categories: excellent (total
                        error 25% or less),  acceptable (total error 50%
                        or less), and unacceptable (total error greater
                        than 50%).

                           REFERENCES

1.  Anon., Guide for the Measures of Precision and Accuracy.  Anal.
    Chem.  34;364R,  1962

2.  Natrella, M. G.  Experimental Statistics.  National Bureau of
    Standards.  1963.  p. T-10.

3.  McFarren,  E. F.,  R. J. Lishka, and J. H.  Parker.  Criterion for
    Judging Acceptability of Analytical Methods.  Anal.  Chem.  42:358,
    1970.
140

-------
                           APPENDIX C.

    TESTS FOR NORMALITY AND REJECTION OF OUTLIERS


Test for normality

    The Kolmogorov-Smirnov goodness-of-fit test was used to deter-
mine  whether the observations reported could reasonably be thought to
have come from  a normal distribution.

    Briefly, the test involves computing the observed cumulative fre-
quency distribution (the percent of values  less than or equal to each
value in the distribution)  and comparing it with the theoretical normal
cumulative frequency distribution.  The point at which the two distri-
butions, theoretical and observed, show greatest divergence is deter-
mined.  Reference of the value of the divergence to a table of critical
values for the Kolmogorov-Smirnov goodness-of-fit test indicates whether
such a large divergence is likely on the basis of chance. If such  a large
divergence is  not likely, the distribution is designated as nonnormal;
otherwise the  distribution is designated as normal.

Tests  for rejection of outliers

    1.   If the distribution is designated as nonnormal,  the suspected
outlier (the farthest value from the mean) is rejected only if the  distance
between it and the mean is  greater than three standard deviations; other-
wise the suspected outlier is accepted.

    2.   If the distribution is designated as normal and the sample size
is less than or equal to 30, the  suspected outlier, the farthest value
from  the mean, is tested for rejection by a method developed byDixon.
Briefly, this test involves computing a ratio that compares the distance
of the  suspected  value being tested from its neighbors with the range of
all, or most all, of the observations (depending on the total number of
suspected values in the sample).   Reference of the ratio to a table of
critical values for test ratios for gross errors indicates whether such
a large ratio is likely on the basis of chance.  If the ratio is greater
than or equal to the critical value, the probability that the suspected out-
lier is from the sample distribution is small; hence, the outlier  is re-
jected.  If the ratio is less than the critical value, the suspected outlier
probably came from the sample distribution; hence, the suspected out-
lier is accepted.

    3.  If the distribution is  designated as normal,  and the sample size
is greater than 30, the suspected outlier  is tested for rejection by a
method developed by Santner. 3 This method employs the statistic,
X - X0  , where  X is the  sample mean, Xo is the  suspected outlier (the
                                                                141

-------
farthest value from the mean) and s is the sample standard deviation.
This statistic is compared with a table of critical values to determine
whether its value is larger than would be expected on the basis of chance.
If the statistic is greater than or  equal to the  critical value, the sus-
pected outlier is rejected; otherwise, the suspected outlier is accepted.

Application of tests for normality and for rejection of outliers to ARS
studies

    The test for normality and the subsequent test for rejection of out-
liers are applied to the observed  data in two way: first, to each method
for a given substance at a given concentration; then to a given substance
at  a given concentration regardless of method.  In either case,  it is first
necessary  to determine whether the original distribution is normal or
nonnormal.  If the  original distribution is designated as nonnormal,
method 1 is used to test for  rejection of the suspected outlier farthest
from the mean.  If the suspected  outlier is not rejected, no further tests
for normality or rejection of outliers are made,  and the distribution is
designated as nonnormal.  On the other hand,  if the suspected outlier  is
rejected, the new distribution, which excludes the rejected observation,
is  then tested for normality.   If the new distribution  is nonnormal, the
next suspected outlier is tested for rejection by method 1.  This cycle
of testing for normality and testing for rejection of outliers  continues
until a suspected value is not rejected or the test for normality  desig-
nates the distribution as normal.   If the distribution  is designated as
normal,  subsequent tests for rejection of outliers made by method 2 or
3 are the same as if the original  distribution had been normal.  This
case is discussed next.

    If the original distribution is designated as normal or a new distri-
bution that was originally nonnormal  is designated as normal after the
rejection of one or more outliers, and if the number of observations is
not greater than 30, then method  2 is used to  test for rejection the sus-
pected outlier farthest from the mean.  If the suspected outlier  is not
rejected, no further tests are made,  and the distribution is designated
as normal.  If the suspected outlier is rejected,  then the suspected out-
lier farthest from the mean  of the new distribution is tested for rejection,
and so on until the suspected value of a new distribution is not rejected;
when this occurs, no further tests are made,  and the final distribution
is designated as normal.  On the  other hand,  if the number of observa-
tions in the original distribution is greater than 30, method 3 is used to
test the suspected outlier  for rejection.   If the suspected outlier is not
rejected,  no further tests are made,  and the  distribution is designated
as normal.  If the suspected outlier is rejected,  then the suspected
outlier farthest from the mean of the new distribution, which excludes
the rejected value, is tested for rejection. Testing for outliers  continues
by this method until a suspected outlier  is not rejected or the number of
142

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observations is no longer greater than 30, in which case, method 2 is
used for testing for rejection of any remaining suspected outliers.
                           REFERENCES
1.  Siegel, S.  Nonparametric Statistics for the Behavioral Sciences.
   McGraw-Hill Book Co., Inc.  New York,  N. Y., 1956. pp. 47-51.

2.  Dixon,  W. J. , Ratios Involving Extreme  Values.  Ann.  Math. Stat.
   2:  68-78,  1951.

3.  Personal communication.  J. Santner, Mathematical Sciences,
   Office of the Director, Robert A. Taft Sanitary Engineering Center,
   1966.
                                                               143

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                          APPENDIX D.

      COMPARISON OF METHODS FOR STATISTICALLY

 SIGNIFICANT DIFFERENCES IN PRECISION AND ACCURACY

    The methods are compared in two ways with respect to precision
and accuracy.  In the first case, two methods are compared at a given
concentration^with respect to precision and to accuracy.  The unknown
variances, cr j and cr i (estimated by the sample variances, s, and s2),
of the two methods are first compared by the F-test  to determine
whether there is a significant difference in the precision of the two
methods^ The unknown means, juj and /u2  (estimated by the sample
means,  X^ and X2),  of the two methods are then compared by thet-test
to determine whether there is a significant difference in the  accuracy of
the two methods.   The t-test employed is based on the result of the
F-test.  These two tests  of hypotheses will produce one of the following
results.

                               2    2
                  Outcome 1:  cr   = cr  , n  =  MO

                               22      i
                  Outcome 2:  cr   = cr  , ^  f  \j.

                               2 /  2
                  Outcome 3:  cr   f cr  , ju  =  fj.
                               1    ij    1     ^

                               2/2      i
                  Outcome 4:  cr   f cr    H  4  /u_


    In outcome 1,  we conclude that the sample results  do not indicate
that a significant difference  in either precision or accuracy exists
between the two methods.

    In outcome 2,  we conclude that there is no indication of a significant
difference in precision between the two methods, but there is a  signifi-
cant difference in the accuracy of the two methods; specifically,  the
method whose sample mean is closer to the true value is deemed the
more accurate.  In outcome 3, we conclude that there is no indication
of a significant difference in the accuracy of the two methods, but the
method with the smaller  sample variance is the more precise.

    In outcome 4,  we conclude that there is a  significant difference in
the precision and in the accuracy of the two methods.  The method with
the smaller sample variance is the more precise, and the  method whose
sample mean is closer to the true value  is the  more accurate.

    In the second case, more than two methods are compared at a given
level of concentration with respect to precision and accuracy.  Bartlett's
 144

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Test^ is used first to test the hypothesis of equality of the unknown
variances,    is used to determine which method means  differ signifi-
cantly.   If the precision is not the same, then the Kruskal-Wallis One-
way Analysis of Variance by Ranks   is used to determine whether a
significant difference exists among  the means in order  to compare the
accuracy of the methods.

    Once again,  there are basically four possible outcomes for the
above tests of hypotheses.
                             2
           Outcome 1:  all er _ are equal, all /u. are equal

                             2
           Outcome 2:  alia . are equal, not all n. are equal

                                2
           Outcome 3:  not all o-  . are equal,  all M. are equal

                                2
           Outcome 4:  not alia  . are equal,  not all /u. are equal


    In outcome 1, we conclude that the sample results  do  not indicate
a significant  difference in either the precision or the accuracy of the
methods.

    In outcome 2, we conclude that there is no indication of a significant
difference in the precision of the  methods; however, at least one method
does differ significantly from the rest with respect to accuracy, and
Duncan's Multiple Range Test indicates which methods  differ.   For ex-
ample,  in comparing four methods, we might conclude  n-^  = ^2 and/jg =  IJL.,
but ju^  and ^ differ significantly from /Ug and /u^; or we might conclude
that jUj = iu_ = jUg , but, ju  differs significantly from ju. ,  ju_ , and ,Ug .

    In  outcome 3, we conclude that  there is no indication of a significant
difference in the accuracy of the methods,  but at least one method differs
significantly from the rest with respect to  precision.

    In  outcome 4, we conclude that  the methods differ significantly with
respect to both precision and accuracy.
                                                                 145

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                           REFERENCES

1.  Ostle, B. Statistics in Research.  Iowa State University Press.
    Ames, Iowa, 1963, p. 123.

2.  Ibid. ,  pp. 119-20.

3.  IbiH. ,  pp. 136-38.

4.  Hicks, C.  Fundamental Concepts in the Design of Experiments.
    Holt, Rinehart,  Winston.  New York, N.Y.,  1964, pp. 21-28.

5.  Ibid.,  pp. 31-33.

6.  Kramer, C.  Extension of Multiple Range Tests to Group Means
    with Unequal Numbers of Replications.  Biometrics 12: 307-310, 1956.

7.  Siegel, S.  Nonparametric Statistics.  McGraw-Hill.  New York,
    N.Y., 1956, pp. 184-94.
 146

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                           APPENDIX E.

       ANALYTICAL REFERENCE SERVICE MEMBERSHIP
STATE AGENCIES

Alabama State Department of Public Health, Montgomery
Alabama Water Improvement Commission, Montgomery
Arizona State Department of Health, Phoenix
Arkansas Pollution Control Commission,  Little Rock
Arkansas State Department of Health, Little Rock
California Department of Water Resources, Sacramento
California State Department of Public Health,  Los Angeles
California State Department of Public Health,  Air and Industrial
   Hygiene Laboratory, Berkeley
California State Department of Public Health,  Sanitation and Radiation
   Laboratory, Berkeley
Colorado  Department of Public Health, Denver
Connecticut State Department of Health, Hartford
Delaware Water and Air Resources Commission, Dover
District of Columbia Department of Public Health, Washington, D. C.
Florida Department of Agriculture, Tallahassee
Florida State Board of Health,  Jacksonville
Florida State Board of Health,  Pensacola
Florida State Board of Health,  Winter Haven
Hawaii State Department of Health, Laboratories Branch, Honolulu
Hawaii State Department of Health, Occupational and Radiological
   Health Section, Honolulu
Idaho Department of Health, Boise
Illinois Department of Public Health, Springfield
Illinois State Water Survey, Champaign
Illinois State Water Survey, Peoria
Indiana State Board of Health,  Indianapolis
Iowa State Hygienic Laboratory, Des Moines
Iowa State Hygienic Laboratory, Iowa City
Kentucky State Department of Health, Division of Laboratory Services,
   Frankfort
Kentucky State Department of Health, Radiological Health Program,
   Frankfort
Lawrence Experiment Station,  Massachusetts
Louisiana State Department of Health, New Orleans
Los Angeles County Flood Control District, California
Maryland State Department of Health, Bureau  of Environmental
   Chemistry, Baltimore
Maryland State Department of Health, Bureau  of Laboratories,
   Baltimore
Maryland State Department of Water Resources, Annapolis
Massachusetts Department of Public Health, Amherst
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Massachusetts Department of Public Health, Boston
Michigan Department of Conservation, Lansing
Michigan Department of Public Health, Lansing
Minnesota Department of Agriculture,  St. Paul
Minnesota Department of Health,  Minneapolis
Missouri Department of Health,  Jefferson City
Montana Bureau of Mines and Geology, Butte
Montana Health Department, Helena
Nebraska State Department of Health,  Lincoln
Nevada  State Department of Health, Reno
Nevada  State Department of Health and Welfare,  Las Vegas
New Hampshire State Department of Health, Concord
New Hampshire Water Supply and Pollution Control Commission,
    Concord
New Jersey State Department of Health,  Trenton
New Mexico Department of Public Health, Santa Fe
New York State Conservation Department, Avon
New York State Conservation Department, Ronkonkoma
New York State Department of Health,  Division of Air  Resources,
    Albany
New York State Department of Health,  Division of Laboratories  and
    Research,  Albany
New York State Department of Health,  Syracuse
New York State Department of Labor,  New York City
North Carolina Department of Water and Air Resources, Raleigh
North Dakota State Department of Health, Bismarck
North Jersey District Water Supply Commission, Wanaque
Ohio Department of Agriculture,  Reynoldsburg
Ohio State Department of Health, Columbus
Oklahoma State Health Department, Oklahoma City
Oregon  State Board of Health,  Portland
Pennsylvania Department of Agriculture, Harrisburg
Pennsylvania Department of Health,  Division of Air Pollution Control,
    Harrisburg
Pennsylvania Department of Health,  Water Quality Section, Harrisburg
Puerto  Rico Institute of Health Laboratories, Hato  Rey
Puerto  Rico Aqueduct and Sewer Authority,  San  Juan
Rhode Island State Department of Health, Providence
South Carolina Pollution Control Authority,  Columbia
South Dakota Department of Health, Pierre
Tennessee Department of Public Health,  Nashville
Tennessee Stream Pollution Control Authority, Nashville
Texas State Department of Health, Austin
Utah State Department of Health, Salt Lake City
Vermont State Department of Health,  Barre
Vermont State Department of Health,  Burlington
Virginia State Department of Health,  Bureau of Industrial Hygiene,
     Richmond
148

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Virginia State Department of Health,  Bureau of Laboratories, Richmond
Virginia State Water Control Board,  Richmond
Washington State Department of Health,  Seattle
Washington State Food and Drug Laboratory, Seattle
West Virginia Department of Natural Resources, Charleston
Wisconsin Department of Agriculture, Madison

MUNICIPAL AGENCIES

Albuquerque Department of Environmental Health,  Air Management
     Division,  New Mexico
Albuquerque Department of Environmental Health,  Food and Institutional
     Division,  New Mexico
Baltimore City Health Department, Maryland
Bay Area Air  Pollution Control District, San Francisco,  California
Beaumont Health Department,  Texas
Central Water Filtration Plant, Chicago, Illinois
City of Amarillo,  Water Reclamation Department,  Texas
City of Charlotte, Water Department, North Carolina
City of Cincinnati, Division of  Water Pollution Control, Ohio
City of Durham,  Department of Water Resources,  North Carolina
City of Erie, Bureau of Water, Pennsylvania
City of Long Beach,  Water Department,  California
City of Miami, Alexander Orr, Jr. Water Treatment Plant, Florida
City of Newburgh, Water Department, New York
City of New York, Food and Drug Laboratory,  New York
City of Niagara Falls, Division of Water Laboratories, New York
City of Philadelphia,  Office of  the Medical Examiner, Pennsylvania
City of San Jose, Health Department, California
City of Seattle, Water Department, Washington
City of Toledo, Division of Pollution Control, Ohio
City of Yonkers,  Bureau of Water, New York
County of Fresno, Department of Public Health, California
County of Los Angeles, Air Pollution Control District, California
Denver  Board of Water Commissioners,  Colorado
Department of Air Pollution Control, Chicago,  Illinois
Department of Public Health, Environmental Health Laboratory,
     Philadelphia, Pennsylvania
Department of Public Health, Public  Health Laboratory, Philadelphia,
     Pennsylvania
Department of Public Works and Utilities, Flint, Michigan
Department of Service and Buildings, Dayton,  Ohio
Department of Water and Power, Los Angeles,  California
East Bay Municipal Utility District, Oakland, California
Easterly Pollution Control Center, Cleveland,  Ohio
Erie County Health Laboratory, Buffalo, New York
Houston City Health  Department, Texas
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Los Angeles Department of Public Works, Playa Del Rey, California
Louisville Water Company, Kentucky
Metropolitan St. Louis Sewer District, Missouri
Metropolitan Sanitary District of Greater Chicago, Illinois
Metropolitan Utilities District, Omaha, Nebraska
Metropolitan Water District of Southern California, LaVerne
Minneapolis Water Department,  Minnesota
Monroe County Health Department, Rochester, New York
Nassau County Department of Health, Hempstead,  New York
Nassau County Department of Health, Mineola, New York
New York City Department of Air Pollution Control, New York
New York City Health Department, New York
Orange County Air Pollution Control District,  Anaheim,  California
Philadelphia Water Department, Pennsylvania
Philadelphia Water Department, Belmont Laboratory, Pennsylvania
Philadelphia Water Department, Torresdale Laboratory, Pennsylvania
Riverside County Air Pollution Control District, California
St.  Louis Public Health Laboratories,  Missouri
Salem  and Beverly Water Supply Board, Beverly, Massachusetts
San Diego County Department of Public Health, California


FEDERAL AGENCIES

Brookhaven National Laboratory, Upton, Long Island, New York
DHEW, PHS,  Bureau of Community Environmental Management,
    Cincinnati, Ohio
DHEW, PHS,  Bureau of Water Hygiene, Bethesda, Maryland
DHEW, PHS,  National Air Pollution Control Administration, Washing-
    ton,  D.C.
DHEW, PHS,  Northeast Marine Health Sciences Laboratory, Narra-
    gansett, Rhode Island
DHEW, PHS,  Northeastern Radiological Health Laboratory, Winchester,
    Massachusetts
DHEW, PHS,  Southwestern Radiological Health Laboratory, Las Vegas,
    Nevada
First United States Army Medical Laboratory No.  1,  Fort George G.
    Meade, Maryland
Fourth U.S. Army Medical Laboratory, Fort  Sam Houston,  Texas
Regional Environmental Health Laboratory (LSGHM),  McClellan AFB,
    California
Regional Environmental Health Laboratory (SGHK), Kelly AFB,  Texas
Reynolds Electrical and Engineering Company, Inc.,  Las Vegas,
    Nevada
San Francisco Bay Naval Shipyard, Vallejo, California
Sixth U.S.  Army Medical Laboratory,  Sausalito, California
Tennessee Valley Authority, Chattanooga
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Tennessee Valley Authority, Muscle Shoals, Alabama
U.S. Army Environmental Hygiene Agency, Edge wood Arsenal, Maryland
USDA, Soils Laboratory, Beltsville, Maryland
USDI,  FWQA, AWTR Research Activities, Pomona, California
USDI,  FWQA, Alaska Water Laboratory, College
USDI,  FWQA, Analytical Quality Control,  Cincinnati,  Ohio
USDI,  FWQA, Chemistry and Physics,  Cincinnati, Ohio
USDI,  FWQA, Chicago Program  Office, Illinois
USDI,  FWQA, North Atlantic Water Quality Management Office,
    Edison,  New Jersey
USDI,  FWQA, Ohio River Basin Project, Evansville, Indiana
USDI,  FWQA, Ohio River Basin Project, Wheeling, West Virginia
USDI,  FWQA, Robert S. Kerr Water Research Center, Ada, Oklahoma
USDI,  FWQA, Technical Advisory and Investigations Branch, Cincinnati,
    Ohio
USDI,  Fish-Pesticide Research Laboratory, Columbia, Missouri
USDI,  Geological Survey, Columbus,  Ohio
USDI,  Geological Survey, Denver, Colorado
USDI,  Geological Survey, Harrisburg,  Pennsylvania
USDI,  Geological Survey, Little Rock,  Arkansas
USDI,  Geological Survey, Menlo  Park,  California
Walter Reed Army Medical Center, Washington,  D. C.


FOREIGN AGENCIES

Alberta Department of Public Health, Edmonton, Alberta,  Canada
Algoma Steel Corporation, Limited, Sault Ste. Marie, Canada
British Coke Research Association,  Chesterfield, Derbyshire, England
Central Public Health Engineering Research Institute,  Nagpur, India
City's  Institute for Health Protection, Belgrade,  Yugoslavia
Ciudad Universitaria, Mexico
Department of Energy, Mines and Resources, Ottawa, Ontario, Canada
Department of Health Services  and Hospital Insurance, Vancouver,
    B.C., Canada
Department of Municipal Laboratories,  Hamilton, Ontario,  Canada
Department of National Health and Welfare, Occupational Health Division,
    Ottawa,  Ontario,  Canada
Department of National Health and Welfare, Public Health Engineering
    Division, Ottawa, Ontario, Canada
Department of National Health and Welfare, Public Health Engineering
    Division, Vancouver, B. C.,  Canada
Department of Public  Health, Sydney, Australia
Institute of Environmental Sanitation, First Section, Taipei, Taiwan,
    China
Institute of Environmental Sanitation, Division of Quality and Pollution
    Control, Taipei,  Taiwan, China
Institute Nacional de Obras Sanitarias,  Caracas,  Venezuela
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Mekoroth Water Company, Tel-Aviv, Israel
Metropolitan Corporation of Greater Winnipeg, Manitoba,  Canada
Metropolitan Water, Sewerage and Drainage Board, Sydney, Australia
National Agricultural Materials,  Seoul, Korea
National Institute for Water Research, Pretoria, South Africa
Ontario Water Resources Commission, Toronto, Canada
Osaka City Institute of Hygiene, Japan
Scientific Research Council,  Kingston,  Jamaica, West Indies
United Kingdom Atomic Energy Authority, Didcot,  Berks, England
University  of Belgrade, Yugoslavia
University  of Leeds, England
Water Commission, Jamaica, West Indies
Water Research Association,  Marlow, Buckinghamshire,  England


UNIVERSITIES

Iowa State University, Ames
Louisiana State  University, Baton Rouge
Medical College of South Carolina, Charleston
New Mexico Institute of Mining and Technology, Socorro
New York University Medical Center,  New York
Pennsylvania State University, University Park
Purdue  University, Lafayette, Indiana
Oak Ridge Institute of Nuclear Studies,  Tennessee
Rensselaer Polytechnic Institute,  Troy, New York
Rutgers University, New Brunswick, New Jersey
St. Mary's College, Winona,  Minnesota
University of California,  Department of Civil Engineering, Berkeley
University of California,  Industrial Hygiene Engineering,  Berkeley
University of California,  Richmond
University of Dayton, Ohio
University of Florida, Gainesville
University of Kansas,  Lawrence
University of Minnesota,  Minneapolis
University of North Carolina, Chapel Hill
University of Puerto Rico, Mayaguez
University of Vermont, Burlington
University of Wisconsin,  Madison
Washington State University,  Air Pollution Research Section, Pullman
Washington State University,  College of Engineering Research Division,
     Pullman
Wayne State  University, Detroit,  Michigan


INDUSTRIES

Aluminum  Company of America, Wenatchee, Washington
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American Biochemical Laboratory, Baltimore, Maryland
American Public Health Association,  Riverside, California
American Water Works Association, New York, New York
Anaconda Company,  Grants,  New Mexico
ARMCO Steel Corporation, Middletown,  Ohio
Battelle Memorial Institute, Columbus, Ohio
Bethlehem Steel Corporation,  Bethlehem, Pennsylvania
Black and Veatch,  Kansas City,  Missouri
Bio-Technics Laboratories, Incorporated, Los Angeles, California
Borg-Warner Corporation, Des  Plaines, Illinois
Bowser-Morner Testing Laboratories, Incorporated, Dayton, Ohio
Brown and Caldwell Laboratories, San Francisco, California
Calgon Corporation,  Pittsburgh, Pennsylvania
California Water Service Company, San Jose,  California
Carnation Research Laboratories, Van Nuys, California
Chrysler Corporation, Detroit,  Michigan
Culligan,  Incorporated, Northbrook, Illinois
Cyrus Wm. Rice and Company,  Pittsburgh, Pennsylvania
Dow Chemical Company, Midland, Michigan
Emery Industries, Incorporated, Cincinnati, Ohio
Fairbanks, Morse and Company Research Center, Beloit,  Wisconsin
Goodyear Atomic Corporation, Piketon,  Ohio
H. C. Nutting Company,  Cincinnati,  Ohio
Hach Chemical Company,  Ames, Iowa
Hammond-Montel, Incorporated, Elmhurst, New York
Havens-Emerson,  East Paterson,  New Jersey
Hill Top Research, Incorporated, Miamiville, Ohio
Holzmacher, McLendon and Murrell, Melville, New York
Hydro Research Laboratories, Pontiac,  Michigan
Industrial Chemicals, Incorporated,  South Bend,  Indiana
INFILCO, General American Transportation Corporation,  Tucson,
    Arizona
lonac Chemical Company, Birmingham,  New Jersey
Ionics, Incorporated,  Watertown, Massachusetts
Isotopes - A  Teledyne Company, Sandusky,  Ohio
Isotopes,  Incorporated, Palo Alto, California
Johns-Manville Research and Engineering Center, Manville,  New Jersey
Kern-Tech Laboratories, Incorporated, Baton Rouge, Louisiana
Kennecott Copper Corporation, Salt Lake City,  Utah
Monsanto  Company, St. Louis, Missouri
Moutrey and Associates,  Incorporated, Oklahoma City,  Oklahoma
Nalco Chemical Company, Chicago,  Illinois
Pacific Engineering Laboratory, San Francisco, California
Pacific Gas and Electric Company, Emeryville, California
Pan American World Airways, Patrick AFB, Florida
Philadelphia Suburban Water Company, Bryn Mawr,  Pennsylvania
Procter and Gamble Company, Cincinnati, Ohio
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Radiation Detection Company,  Mountain View, California
Ray W.  Hawksley Company, Incorporated, Richmond, California
Reynolds Electrical and Engineering Company, Incorporated, Las Vegas,
    Nevada
Roy F. Weston, West Chester, Pennsylvania
St. Louis County Water Company, University City, Missouri
Sandia Corporation, Albuquerque, New Mexico
Shell Chemical Company,  Princeton, New Jersey
Tenco Hydroscience, Incorporated,  Chicago, Illinois
Texas Gulf Sulphur Company,  Aurora,  North Carolina
Trapelo/West, Richmond, California
U. S.  Industrial Chemicals Company,  Tuscola,  Illinois
United States Pipe and Foundry Company,  Birmingham,  Alabama
W. R. Grace and Company,  Lake Zurich,  Illinois
Wastewater Analysis Corporation,  Lincoln Park, Michigan
Water Pollution Control Federation, Washington, B.C.
Water Service Laboratories, Incorporated, New York, New York
Xerox Corporation,  Webster,  New York
York Research Corporation, Stamford, Connecticut
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