Chapter V: Preface: To Fourth Edition (4)

Determine and report insoluble matter, aluminium oxide (Al_{2}O_{3}), ferric oxide (Fe_{2}O_{3}), ferrous oxide (FeO), basicity ratio, and, if present, free acid as H_{2}SO_{4}. If the material is what is known as “granular” sulfate mix it well before sampling. If it is in lump form crush it to ⅛ to ¼ inch size, mix, and sample it. It is unnecessary to grind the sample to a fine powder, but it is preferable to have the particles fairly uniform in size.

INSOLUBLE MATTER.

Treat 10 grams of the sample with 100 cc. of distilled water and digest one hour at boiling temperature. Filter through a weighed Gooch crucible and wash the insoluble matter with hot water freshly boiled to free it from carbon dioxide. Dry the crucible to constant weight at 100° C., cool, and weigh. Report the percentage of insoluble matter.

OXIDES OF IRON AND ALUMINIUM.

Dilute the filtrate from the determination of insoluble matter to 500 cc. with water free from carbon dioxide and thoroughly mix the solution. Transfer 50 cc. of the solution to a 250 cc. beaker, add about 150 cc. of water and 5 cc. of concentrated hydrochloric acid, and heat to boiling. Add ammonium hydroxide in slight excess; when the solution has been almost neutralized it is convenient to add a drop of methyl orange indicator and then to add about 0.5 cc. of ammonium hydroxide after the solution is neutral to the indicator. Digest at about 100° C. for a few minutes and filter. Some analysts prefer to wash this gelatinous precipitate with hot water by decantation, and some to wash it evenly distributed over the surface of a filter paper; either method may be used. It is difficult to free it completely from impurities and it is not necessary to do so unless unusual quantities of calcium, magnesium, sodium, or potassium are present. While the precipitate is being washed do not allow it to become dry, as it then packs and can not be washed clean. After most of the water has drained drying the filter may be hastened by placing it on a sheet of blotting paper. If much iron is present completely dry the precipitate, remove it from the paper, and ignite the paper separately. Finally, blast the precipitate, with free access of air to the crucible, for five or ten minutes, cool, and weigh as oxides of iron and aluminium (Fe_{2}O_{3} + Al_{2}O_{3}).

Subtract the content of total iron, expressed as ferric oxide (Fe_{2}O_{3}), from the weight of the combined oxides and report the difference as aluminium oxide (Al_{2}O_{3}), in percentage.

TOTAL IRON.

As filter alum usually contains 0.2 to 0.3 per cent of iron use a 10 gram sample for the determination of total iron. Treat the sample with 50 cc. of freshly boiled distilled water and add 5 cc. of concentrated hydrochloric acid and 1 cc. of bromine water. Evaporate the solution to dryness, dissolve the residue in water, and wash it into a flask with sufficient water to make the volume about 50 cc. Add 50 cc. of concentrated hydrochloric acid, boil to expel oxygen, and titrate, as hot as possible, with N/20 stannous chloride.

If a 10 gram sample is used the percentage of iron (Fe) is equal to the number of cubic centimeters of stannous chloride used multiplied by 0.028, and the percentage of iron expressed as ferric oxide is equal to the number of cubic centimeters of stannous chloride used multiplied by 0.040.

FERRIC IRON.

As filter alum usually contains 0.02 to 0.04 per cent of ferric iron use a 20 gram sample. Boil 50 cc. of distilled water to expel oxygen, add 50 cc. of concentrated hydrochloric acid, and add the sample while the solution is boiling. Keep it boiling till the sample is dissolved. The flask should be kept filled with carbon dioxide during this process by dropping in occasionally small amounts of sodium carbonate. When solution of the sample is complete titrate it hot immediately with N/20 stannous chloride.

If a 20 gram sample is used the percentage of ferric oxide (Fe_{2}O_{3}) is equal to the number of cubic centimeters of stannous chloride used multiplied by 0.020.

FERROUS IRON.

The content of ferrous iron is the difference between total and ferric iron. The percentage of ferrous oxide (FeO) is, therefore, equal to 0.90 times the difference between the percentage of total iron expressed as ferric oxide and the percentage of ferric iron expressed as ferric oxide. Report the percentage of ferrous oxide (FeO).

BASICITY RATIO.

Transfer 50 cc. of the filtrate from the determination of insoluble matter to a 200 cc. casserole and dilute it to 100 cc. Boil the solution and titrate it at boiling temperature with N/1 sodium hydroxide in presence of phenolphthalein indicator. The percentage of acidity in equivalent of sulfuric acid (H_{2}SO_{4}) is equal to the number of cubic centimeters of sodium hydroxide used multiplied by 4.9. In this titration iron and aluminium are precipitated as hydroxides and any free acid is neutralized.

Calculate the percentage of sulfuric acid equivalent to the determined percentages of aluminium oxide, ferric oxide, and ferrous oxide by the following formula:

2.88 Al_{2}O_{3} + 1.83 Fe_{2}O_{3} + 1.36 FeO.

If this percentage of acid equivalent is less than that found by titration report the difference as percentage of free acid. If the percentage of acid equivalent is greater than that found by titration the difference divided by 2.88 is the percentage equivalent to the excess of aluminium oxide present. Divide this excess by the percentage of total aluminium oxide and report the quotient as the basicity ratio.

LIME.

Mix well the sample, which should contain no lumps. If foreign matter is present grind the sample to pass a 100–mesh sieve.

Place 20 grams of granulated cane sugar and 1 gram of the sample in a 250 cc. glass-stoppered bottle, tightly stopped, and mix the mass by rolling. Do not shake hard as much of the lime could thus be lost as dust. Then add 187.4 cc. of distilled water freshly boiled to expel carbon dioxide. This makes 200 cc. of sugar solution. The lime is mixed dry with the sugar and the water added later to keep the lime from lumping. After shaking the sugar solution one hour titrate 50 cc. of it with N/2 hydrochloric acid in presence of methyl orange indicator. The acid used is equivalent to the carbonate and hydroxide in 0.25 gram of the sample.

Filter the remainder of the sugar solution, discarding the first 25 cc. of filtrate. Titrate 50 cc. of the filtrate with N/2 hydrochloric acid in presence of methyl orange indicator. The acid used is equivalent to the hydroxide in 0.25 gram of the sample.

If a 1 gram sample is used the percentage of calcium oxide (CaO) is equal to 5.6 times the number of cubic centimeters of hydrochloric acid used in the second titration; and the percentage of calcium carbonate (CaCO_{3}) equivalent to the carbonate present is equal to 10 times the difference in cubic centimeters between the results of the two titrations.

SULFATE OF IRON.

INSOLUBLE MATTER.

Treat 10 grams of the sample with 100 cc. of freshly boiled distilled water cooled to 30° C. or less. When solution is complete filter through a weighed Gooch crucible, wash, dry, cool, and weigh. Report the weight of the residue, in percentage, as insoluble matter.

IRON AS FERROUS SULFATE.

Dissolve 1 gram of the sample and dilute to 200 cc. with freshly boiled distilled water cooled to 30° C. or less. Add 5 cc. of dilute sulfuric acid (1 to 3) to a 50 cc. portion of the solution and titrate with N/10 potassium permanganate. The percentage of ferrous sulfate (FeSO_{4}.7H_{2}O) is equal to 11.12 times the number of cubic centimeters of potassium permanganate used.

ACIDITY.

Shake 12.25 grams of the sample in a 150 cc. bottle with 75 cc. of 95 per cent alcohol for ten minutes. Run a blank. Filter rapidly both sample and blank and wash rapidly with alcohol sufficient to make 100 cc. of filtrate. Titrate with N/20 sodium hydroxide in presence of phenolphthalein and subtract the result of titrating the blank from that of titrating the solution of the sample. The percentage of acidity, expressed as sulfuric acid (H_{2}SO_{4}), is equal to 0.02 times the number of cubic centimeters of sodium hydroxide used.

SODA ASH.

INSOLUBLE MATTER.

Treat 5.305 grams of the sample with 200 cc. of freshly boiled and cooled distilled water. When solution is complete filter through an asbestos mat in a weighed Gooch crucible, dry, cool, and weigh. Report the weight of the residue, in percentage, as insoluble matter.

AVAILABLE ALKALI.

Dilute the filtrate from the determination of insoluble matter to 1,000 cc. and thoroughly mix. Titrate 25 cc. of this dilution with N/10 hydrochloric acid in presence of methyl orange indicator. The percentage of available alkali, expressed as sodium carbonate (Na_{2}CO_{3}), is equal to 4 times the number of cubic centimeters of hydrochloric acid used.

CHEMICAL BIBLIOGRAPHY.

The subjoined bibliography comprises the publications cited in the text of this report. The references are arranged alphabetically by authors’ names and under each author in order of dates of publication. When different pages of a single work are cited letters are used in connection with the number that refers to the work.

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phenolphthalein as indicators: _Chem. News_, Vol. 47, pp. 123–7, 1883.

Bibliography 98:

THOMSON, ANDREW. Colorimetric method for determining small quantities
of iron: _J. Chem. Soc._, Vol. 47, pp. 493–7, 1885.

Bibliography 99:

THRESH, J. C. A new method of estimating the oxygen dissolved in
water: _J. Chem. Soc._, Vol. 57, pp. 185–95, 1890.

Bibliography 100:

——. The examination of water and water supplies, p. 200, Philadelphia,
1904;

Bibliography 100a:

p. 219;

Bibliography 100b:

p. 195;

Bibliography 100c:

p. 282.

Bibliography 101:

TIDY, C. M. The process for determining the organic purity of potable
waters: _J. Chem. Soc._, Vol. 35, pp. 46–106, 1879.

Bibliography 102:

TIEMANN, FERDINAND, and GÄRTNER, AUGUST. Handbuch der Wässer, 4th ed.,
pp. 255–8, Friedrich Vieweg und Sohn, Braunschweig, 1895.

Bibliography 103:

TREADWELL, F. P. [translated by Hall, W. T.], Analytical Chemistry, 3d
ed., Vol. 2, pp. 687–688, John Wiley & Sons, New York, 1911;

Bibliography 103a:

pp. 50–3.

Bibliography 104:

TROMMSDORFF, HUGO. Bestimmung der Organischen Substanzen: _Zeit. Anal.
Chem._, Vol. 8, p. 344, 1869.

Bibliography 105:

U. S. GEOLOGICAL SURVEY. Measurement of color and turbidity of water,
Form 9–182, Washington, 1902.

Bibliography 106:

WANKLYN, J. A. Verification of Wanklyn, Chapman, and Smith’s water
analyses on a series of artificial waters: _J. Chem. Soc._, Vol. 20,
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Bibliography 107:

——. Water analysis, 10th ed., pp. 33–5, Kegan, Paul, Trench, Trübner,
& Co., Ltd., London, 1896;

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pp. 106–7.

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WARINGTON, ROBERT. Note on the appearance of nitrous acid during
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WARREN, H. E., and WHIPPLE, G. C. The thermophone, a new instrument
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WEST, F. D. The preparation of standards for the determination of
turbidity of water: _Proc. Ill. Water Supply Assoc._, Vol. 6, pp.
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WESTON, R. S. Apparatus for the determination of ammonia in water by
the Wanklyn method, and total nitrogen by the Kjeldahl method: _J. Am.
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——. The determination of nitrogen as nitrites in waters: _J. Am. Chem.
Soc._, Vol. 27, pp. 281–7, 1905.

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——. The determination of manganese in water: _J. Am. Chem. Soc._, Vol.
29, pp. 1074–8, 1907.

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WHIPPLE, G. C. The observation of odor as an essential part of water
analysis: _Public Health Papers and Reports, Am. Pub. Health Assoc._,
Vol. 25, pp. 587–93, 1899.

Bibliography 115:

——. The microscopy of drinking water, 3d ed., pp. 186–205, John Wiley
& Sons, New York, 1914.

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——, and JACKSON, D. D. A comparative study of the methods used for the
measurement of the turbidity of water: _Tech. Quart._, Vol. 13, pp.
274–94, 1900.

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——, and others. The decolorization of water: _Trans. Am. Soc. Civil
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——, and PARKER, H. N. On the amount of oxygen and carbonic acid
dissolved in natural waters and the effect of these gases upon the
occurrence of microscopic organisms: _Trans. Am. Microscopical Soc._,
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——, and WHIPPLE, M. C. Solubility of oxygen in sea water: _J. Am.
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WINKLER, L. W. Die Bestimmung des im Wasser gelösten Sauerstoffes:
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WOODMAN, A. G., and NORTON, J. F. Air, water, and food, 4th ed., pp.
72–8, John Wiley & Sons, New York, 1914;

Bibliography 121a:

pp. 85–7;

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pp. 90–1, 216, and 231;

Bibliography 121c:

pp. 106–8.

MICROSCOPICAL EXAMINATION.

The microscopical examination of water consists of the enumeration of the kinds of microscopic organisms (Plankton), and an estimation of their quantity.

It may serve any one or more of the following purposes:

(1) To explain the presence of objectionable odors and tastes.

(2) To indicate the progress of the self purification of streams.

(3) To indicate the presence of sewage contamination.

(4) To explain the chemical analysis.

(5) To identify the source of a water.

(6) To aid in the study of the food of fish, shellfish, and other
aquatic organisms.

The term “Microscopic Organisms” shall include all organisms microscopic or barely visible to the naked eye, with the exception of the bacteria. It includes the diatomaceae, chlorophyceae, cyanophyceae, fungi, protozoa, rotifera, crustacea, bryophyta, and spongidae found in water.

Fragments of organic matter, silt, mineral matter, zoöglea, etc., shall be considered as amorphous matter. The recording of amorphous matter usually serves no useful purpose and shall not be considered a part of the standard method.

_Apparatus._—1. A cylindrical funnel about two inches in diameter at the top, with a straight side for nine inches, narrowed over a distance of three inches to a bore of one-half inch in diameter, and terminating in a straight portion of this diameter two and one-half inches in length. The capacity of this funnel is 500 cc. It shall be provided at the bottom with a tightly fitting rubber stopper with a single perforation and a disk of silk bolting cloth over the hole about three eighths of an inch in diameter.

2. A counting cell consisting of a brass rim closely cemented to a plate of optical glass. The shape and size of this cell are not essential but its depth shall be one millimeter. A convenient capacity is about one cubic centimeter.

3. An ocular micrometer ruled as follows: The ocular micrometer is commonly of such a size that with a 16 mm. objective and a suitable tube length, the largest square cuts off one square millimeter on the stage.

_Procedure._—Filter 250 cc. of the water (more or less according to the clearness of the sample) through a one-half inch layer of quartz sand (washed and screened between 60 and 120 mesh sieves) supported by the disk of bolting cloth and rubber stopper at the bottom of the funnel. Suction may be applied to hasten the filtration.

Remove the stopper and catch the plug of sand and its entrained organisms in a small beaker or test tube, washing down the inside of the funnel into the beaker with 5 cc. of clean (preferably distilled) water. Agitate the mixture of sand, water, and organisms to detach the latter from the sand grains, and quickly decant the water and the organisms in suspension to a test tube. If desired the sand may then be again washed with 5 cc. water and the wash water added to the first portion.

Cover the cell partially with a cover glass, and by means of a pipette run the concentrate under the cover glass until the cell is completely filled.

Cover and place on the microscope stage in a horizontal position for examination.

Count the organisms in twenty fields, i. e., twenty cubic millimeters, estimating their areas in terms of Standard Units.

_The Standard Unit is the smallest square in the ocular micrometer, and represents an area 20µ × 20µ, or 400 square microns on the stage._

Results shall be expressed in the number of Standard Units of each kind of micro-organism per cc. and also the total number of standard units of all kinds per cc. The general directions as to significant figures given under Turbidity shall apply also to the microscopical examination.

_Caution._—Many micro-organisms, especially some of those causing odors, are so fragile that they are broken up in filtration, especially if the agitation of the filtrate is too vigorous. A direct examination of a fresh sample is therefore a useful supplementary procedure. For the same reason the concentrate should not stand long before examination. Also some organisms are carried by specific gravity to the top of the cell which should be scrutinized as well as the bottom layer each time.

It is always better to examine the micro-organisms in the field when possible, and for this purpose the sling filter has been devised consisting of a metal funnel slung to a pivoted handle, with a disk of wire gauze in the detachable lower end to support the sand. Filtration is hastened by imparting a whirling motion to the whole and utilizing the centrifugal force thus generated.

MICROSCOPICAL BIBLIOGRAPHY.

_a._ KEAN, A. L. A new method for the microscopical examination of
water: _Science_, Vol. 13, p. 132, 1889; _Eng. News_, pp. 21,
276, 1889.

_b._ SEDGWICK, W. T. Recent progress in biological water analysis: _J.
N. E. Water Works Assoc._, Vol. 4, pp. 50–64, 1889.

_c._ ——. A report of the biological work of the Lawrence Experiment
Station: _Examinations by the State Board of Health of water
supplies of Mass., 1887–90_, pt. 2, Purification of sewage and
water, pp. 793–862, 1890.

_d._ PARKER, G. H. Report upon the organisms, excepting the bacteria
found in the waters of the State: _Examinations by the State
Board of Health of water supplies of Mass., 1887–90_, pt. 1,
Examination of water supplies, pp. 579–620, 1890.

_e._ RAFTER, G. W. The microscopical examination of potable water, D.
Van Nostrand Co., New York, 1910. (Contains bibliography.)

_f._ CALKINS, G. N. The microscopical examination of water: _Report
Mass. State Board of Health_, pp. 397–421, 1892.

_g._ JACKSON, D. D. On an improvement in the Sedgwick-Rafter method for
the microscopical examination of drinking water: _Tech. Quart._,
Vol. 9, pp. 271–4, 1896.

_h._ WHIPPLE, G. C. Experience with the Sedgwick-Rafter method at the
Biological Laboratory of the Boston Water Works: _Tech. Quart._,
Vol. 9, pp. 275–9, 1896.

_i._ ——. Microscopy of drinking water, 3d ed., John Wiley & Sons, New
York, 1914. (Contains bibliography.)

BACTERIOLOGICAL EXAMINATION.