`
`Eton Ex. 1066
`1 of 11
`
`Eton Ex. 1066
`1 of 11
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`

`

`
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`C.
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`
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`Eton Ex. 1066
`2 of 11
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`

`

`AMERICAN PUBLIC HEALTH
`
`ASSOCIATION
`
`LABORATORY SECTION
`
`STANDARD METHODS
`FOR THE
`
`EXAMINATION
`
`OF
`
`WATER AND SEWAGE
`
`SECOND EDITION
`SECOND REPRINT
`
`AMERICAN PUBLIC HEALTH ASSOCIATION
`
`755 BOYLSTON Sum-r, BOSTON
`1915
`
`C0 816
`
`Eton Ex. 1066
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`
`Eton Ex. 1066
`3 of 11
`
`

`

`QD
`1 42.
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`\^\5
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`
`Eton Ex. 1066
`4 of 11
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`

`

`TABLE OF - CONTENTS.
`
`PREFACE To SECOND EDITION
`
`INTRODUCTION .
`
`PHYSICAL EXAMINATION
`
`CHEMICAL EXAMINATION .
`
`BIBLIOGRAPHY
`
`MICROSCOPICAL EXAMINATION
`
`BIBLIOGRAPHY
`
`BACTEEIOLOGICAL EXAMINATION
`
`BIBLIOGRAPHY
`
`REPORT OF COMMITTEE AT HAVANA MEETING
`
`INDEX
`
`PAGE
`
`14
`
`70
`
`75
`
`76
`
`77
`
`137
`
`141
`
`143
`
`iii
`
`283350
`
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`Eton Ex. 1066
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`PREFACE TO SECOND EDITION.
`The present volume is the second and revised edition of the volume issued in
`the title "Report of the Committee on Standard Methods of Water
`1905 under
`Analysis to the Laboratory Section of the American Public Health Association."
`toward standard methods of water
`A full history of the origin of the movement
`analysis and of the work of the various committees which have had that matter
`in hand since 1895 is given in the letter of transmittal of the original report.
`The
`committee having in charge the preparation of that report was continued in office
`at the Boston meeting in 1904, and it was the expressed
`after its final presentation
`opinion of those present at that meeting that progress reports
`should be made
`from time to time looking toward a revision of the standard text when such re
`of a second edition of
`The question
`vision seemed desirable.
`the report was
`definitely settled at the Atlantic City meeting in 1908.
`This task was placed in
`the hands of two new committees
`to whom were referred,
`respectively, methods
`for the chemical analysis of water and sewage, and methods for the bacteriologi
`The former committee was made up of Messrs.
`cal tests of water and sewage.
`Earle B. Phelps, Chairman; Robert Spurr Weston, Leonard P. Kinnicutt, Edward
`Bartow, and A. E. Kimberly; and the latter of D. D. Jackson, Chairman, Wm.
`J. A. Amyot, Fred P. Gorham and Stephen DeM. Gage.
`Royal Stokes,
`These
`two committees have worked quite independently in the preparation of the two
`sections of the present volume.
`The work of the Committees during the three years that have elapsed since their
`in the progress reports which have been sub
`appointment, has been contained
`mitted at the annual meetings.
`These reports have been in the nature of pro
`It has been thought best to
`posed changes in or additions to the existing text.
`these annual reports to be the actual working reports of the committees,
`consider
`and in the final
`incorporation of the committees'
`recommendations
`in the text
`of this volume to change the title of the latter so that it no longer appears as a
`Committee report.
`The changes which have been incorporated in the chemical section of the report
`have been minor changes in technique
`in certain of the determinations; a con
`of the material into what is considered a somewhat more
`siderable rearrangement
`form for use; the substitution of entirely new matter in the case of
`convenient
`notably that for nitrates in sewage, copper, and some
`a few of the determinations,
`minor determinations; a substitution of the term "non-carbonate hardness"
`for
`the rather troublesome
`term "incrustants"
`heretofore used; a method of state
`as "free," "half-bound,"
`for carbon
`ment
`dioxide
`heretofore
`reported
`and
`"bound" carbon dioxide, which statement
`it is believed brings the results of this
`determination more nearly into line with those of other mineral constituents
`now commonly expressed in the ionic form; and in the addition of certain new
`notably methods
`for manganese,
`material,
`hydrogen
`bromine
`and
`sulphide,
`The principal addition to the text, however, consists in a complete method
`iodine.
`for the so-called "mineral analysis of water," the analysis for industrial purposes
`and for use in boilers. Methods for the determination of putrescibility or rela
`
`Eton Ex. 1066
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`
`

`

`vi
`
`Preface to Second Edition
`tive stability in sewage and rapid approximate methods known as "lime value,"
`and "soda value," intended for use in connection with water softening plants to
`the relative amounts
`of these two reagents necessary
`for softening,
`determine
`have also been added; and a new table of oxygen saturation values including
`fresh and saline water and with a correction formula for altitude,
`is
`in
`corporated.
`The changes proposed by the Committee on Bacteriological Methods have
`consisted in a few minor changes in the text,
`together with the addition of much
`In order to study the various bacteria of fecal origin a study has
`new material.
`been made of the B. coli group, and this group has beep divided into four sub
`The quantitative tests for the B.
`divisions, as the text of the report will show.
`coli group have been considered, and the dilution method in fermentation tubes
`In quantitative tests for general gas-producing
`has been recommended.
`bac
`teria in water or sewage the use of liver broth has been suggested, and a number
`of comparative studies are set forth in the report concerning the rejuvenation of
`attenuated forms by this method.
`in drink
`Tests for B. sporogenes and B. typhi
`ing water are also considered, and the report ends with the consideration of the
`isolation of specific disease germs from water supplies and a careful set of direc
`of sterilization and the manufacture of various
`tions concerning
`the technique
`culture media. A list of references is appended.
`This volume on Standard Methods is presented in the belief that it represents
`It is in no
`the best methods for the various determinations that are available.
`sense the work of the committee members alone, but throughout the work of
`revision every effort has been made to obtain a consensus of opinion upon all mat
`It is believed that the procedures
`ters.
`described represent
`such a consensus
`of opinion and fairly represent
`the best practice in American laboratories.
`These,
`It must be obvious that stand
`however, are not in any sense regarded as final.
`to be useful must, while maintaining sufficient
`ard methods of this kind in order
`rigidity to serve as a satisfactory guide to laboratory procedure, be at the same
`time sufficiently elastic to be readily if somewhat slowly moulded by new devel
`to the end that the Standard Methods themselves
`opments in the best practice,
`reflect what is best in laboratory procedure rather than arbitrarily
`shall always
`fix such procedure.
`The members of the two committees wish to express their thanks to those who
`have rendered assistance in the preparation of this report, and to beg for their
`in the future work of the laboratory
`continued interest, support and co-operation
`section along these lines.
`
`Eton Ex. 1066
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`

`

`59
`
`Carbonic Acid —Oxygen
`When the water is alkaline to phenolphthalein, bicarbonates are
`present only when this alkalinity is less than one half that by methyl
`See Table 8, page 39.
`Then the bicarbonate
`red or erythrosine.
`alkalinity is equal to the total alkalinity by methyl red or erythro
`sine minus twice the alkalinity by phenolphthalein. When this
`difference is expressed in terms of calcium carbonate,
`the bicarbo
`nate, carbonic acid as bicarbonate, and half bound carbonic acid
`are determined from it by the factors given above.
`
`CARBONATE
`
`in
`
`(C03), AND BOUND
`
`(CO3), CARBONIC ACID AS CARBONATE
`CARBONIC ACID.
`Carbonate is computed as 1.2 times the alkalinity expressed
`terms of calcium carbonate, as determined by phenolphthalein.
`Carbonic acid as carbonate is computed as 0.88 times the same.
`Bound carbonic acid is computed as 0.44 times the alkalinity ex
`pressed in terms of calcium carbonate as determined by methyl
`red, lacmoid, or erythrosine.
`It should be noted that half bound carbonic acid is equal to one
`half the bicarbonate carbonic acid and that the bound is the sum
`of the carbonic acid as carbonate and one half that as bicarbonate.
`DETERMINATION OF DISSOLVED OXYGEN.
`There are three methods in use for the determination of atmos
`pheric oxygen dissolved in water, viz., those of Winkler,71 Thresh72
`Each of these methods has its own particular field of
`and Levy.73
`usefulness. All are capable of giving sufficiently accurate results.
`The Winkler method is in the most common use in this country,
`and possesses the advantage of requiring only simple and not read
`It is therefore recommended as the stand
`ily breakable apparatus.
`ard method.
`The method of Thresh is perhaps slightly more accurate than
`the Winkler method, but the apparatus is not so well adapted to
`For certain purposes, however, as,
`field work.
`the
`for example,
`it
`determination of dissolved oxygen before and after incubation,
`than the Winkler method, because the apparatus
`is more practical
`allows the taking of representative samples direct
`from bottles or
`other containers.
`What is true of the disadvantages of the Thresh method is also
`true to a great degree of the Levy method. With both of these
`5
`
`Eton Ex. 1066
`8 of 11
`
`

`

`60
`
`Oxygen
`
`methods the samples are taken in a special, stoppered, separatory
`funnel.
`Winkler Method Reagents. — 1. Manganous sulphate solution: Dis
`solve 48 grams of manganous sulphate in 100 c.c. of distilled water.
`2. Solution of sodium hydrate and potassium iodide: Dissolve
`360 grams of sodium hydrate and 100 grams of potassium iodide in
`one liter of distilled water.
`3. Sulphuric acid.
`Specific gravity 1.4 (dilution 1:1).
`4. Sodium thiosulphate solution.
`Dissolve 6.2 grams of chemi
`cally pure recrystallized sodium thiosulphate in one liter of dis
`This gives a ^ solution each c.c. of which is equiva
`tilled water.
`to 0.2 mg. of oxygen or 0.1395 c.c. of oxygen at 0° C. and
`lent
`it
`760 mm. pressure.
`Inasmuch as this solution is not permanent
`should be standardized occasionally against an J5 solution of potas
`sium bichromate as described in almost any work on volumetric
`The keeping qualities of the thiosulphate solution are
`analysis.
`improved by adding to each liter 5 c.c. of chloroform and 1.5 grams
`of ammonium carbonate before making up to the prescribed volume.
`5. Starch solution. Mix a small amount of clean starch with
`cold water until
`it becomes a thin paste, stir this into 150 to 200
`times its weight of boiling water. Boil
`for a few minutes,
`then
`It may be preserved by adding a few drops of chloroform.
`sterilize.
`the Sample. —The sample shall be collected with
`Collection of
`extreme care in order to avoid the entrainment or absorption of any
`oxygen from the atmosphere.
`The sample bottle shall be preferably
`a glass-stoppered bottle which has a narrow neck and which holds
`at least 250 c.c.
`The exact capacity of the bottle shall be deter
`mined and for convenient
`this may be scratched upon
`reference
`the glass with a diamond.
`If the sample is to be collected from a tap the water shall be made
`to enter the bottle through a glass or rubber tube which reaches to
`the water being allowed to overflow for
`the bottom of the bottle,
`several minutes, after which the glass stopper is carefully replaced
`so that no bubble of air is caught beneath it.
`If the sample is to be collected from the surface of a pond or tank
`the ordinary sample bottle and a second
`two bottles shall be used,
`bottle of four times the capacity.
`Both bottles shall be provided
`with temporary stoppers of double perforation and in both cases
`a glass tube shall extend through one hole of the stopper to the bot
`
`Eton Ex. 1066
`9 of 11
`
`

`

`Oxygen
`
`61
`
`torn of the bottle and a short glass tube shall enter the other hole
`The short tube of
`into the bottle.
`of the stopper but not project
`the sample bottle shall be connected with the long tube of the larger
`In collecting the sample the sample bottle shall be im
`bottle.
`mersed in the water and suction applied to the short
`tube of the
`large bottle and enough water drawn through the hole to fill
`the
`In this way the water in the smaller bottle will be
`large bottle.
`changed several times and a fair sample secured.
`If the sample is to be taken at a depth below the surface both
`lowered to the desired depth, and if the
`bottles may be connected,
`smaller bottle is placed beneath the larger one the water will enter
`the air
`the small bottle and pass from that into the larger bottle,
`As soon as the
`escaping from the short tube of the large bottle.
`small bottle has been filled remove the temporary stopper and in
`sert the permanent glass stopper using care not
`to entrain any bub
`bles of air.
`Procedure.— Remove the stopper
`from the bottle and add ap
`two c.c. of the manganous sulphate solution and two
`proximate^'
`c.c. of the sodium hydrate-potassium iodide solution delivering both
`of these solutions beneath the surface of the liquid by means of a
`Replace the stopper and mix the contents of the bottle
`pipette.
`Allow the precipitate to settle.
`Remove the stopper,
`by shaking.
`Up to
`two c.c. of sulphuric acid and mix thoroughly.
`add about
`the procedure shall be carried on in the field but after
`this point
`the sulphuric acid has been added and the stopper replaced there
`is no further change and the rest of the operation may be conducted
`For accurate work there are a number of corrections
`at leisure.
`to be made, but in actual practice it is seldom necessary
`necessary
`to take them into account as they are ordinarily much less than the
`errors of sampling.
`Rinse the contents of the bottle into a flask,
`titrate with 5-5 solution of sodium thiosulphate using a few c.c. of
`the starch solution toward the end of the titration.
`Do not add the
`the color has become a faint yellow;
`titrate until the
`starch until
`If nitrites be present, correction must be
`blue color disappears.
`made.
`Calculation of results. —The standard method of expressing re
`sults shall be by parts per million of oxygen by weight.
`It is sometimes convenient
`to know the number of c.c. of the
`gas per liter at 0° C. temperature and 760 mm. pressure and also
`to know the percentage which the amount of gas present is of the.
`
`Eton Ex. 1066
`10 of 11
`
`

`

`62
`
`OXYGEN
`
`maximum amount capable of being dissolved by distilled water at
`the same temperature and pressure. All three methods of calcu-
`lotion are therefore here given.
`
`QWNXIJIIMII] MN
`.
`.
`.
`Oxygen in parts per million =—— -
`V
`V
`0.1395 N x1000
`139.5 N
`.
`.
`=__._—V__. =T
`Oxygen m c.e. per liter
`O
`n in
`r cent of saturation w —2M
`pe
`'
`v><o
`‘
`v0
`me
`Where N :uumber of c.c. of 1‘1: thiosulphate solution.
`V=capacity of the bottle in c.(:. less the volume of the mungmiouo sulphate
`and potassium iodide solution added (1. 03., less {our c.c.).
`0=tbe amount. of oxygen in parts per million in water saturated at the same
`temperature and pressure. See Table 12.
`TABLE 12.
`Sou-sum or 0mm In Fuel Warn um 11'! Su Win-n or Sum DIOR-II! or $11.11!?” ATVAIIDL'I. Tn-
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`Pml‘ll or m ul.‘
`(Cnlmhted by G. C. Whipple Ind M. C. Whipple from Monuments 010.1. Fox)"
`Mm
`Chlorine in Sen Water (Perla pee Million).
`' _.———._.__fl— DB [WM
`Tempultun Centigrade.
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`of! Chlorine
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`petunia.
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`12.0?
`12.14
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`11.82
`12 23
`11.52
`11.91!
`11.24
`11.119
`10.9?
`11.39
`10 70
`11.12
`10.05
`10.85
`10.21
`10.61
`9.911
`10 36
`0.76
`10.13
`0 55
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`201100
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`11.33
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`10.76
`10.50
`10 25
`10.01
`0.73
`0.57
`0.35
`0.17
`8.93
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`3 80
`8.63
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`13.41
`13.06
`12 72
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`11.70
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`10 1'3
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`10.49
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`‘Under any other barometric prenure. B. the solubility Ell]. be obtained from the corresponding Vllue in the
`table by the formula:
`_
`_
`.
`S'-Solul.nlity at Elna-B" Inehu.
`s =Solubilit3' .1 mum-29.92 inches.
`
`S’ S B S B’
`' Fo' 29.92
`
`. Go gle
`
`Eton Ex. 1066
`11 of 11
`
`Eton Ex. 1066
`11 of 11
`
`