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North Carolina State Library
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TWENTY-FIFTH ANNUAL REPORT °<?
OF THE
NORTH CAROLINA
AGRICULTURAL EXPERIMENT STATION
OF THE
COLLEGE OF AGRICULTURE AND MECHANIC ARTS
FOR THE
YEAR ENDING JUNE 30, 1902.
INCLUDING
TECHNICAL AND SCIENTIFIC PAPERS AND
BULLETIN No. 181.
RALEIGH, N. C.
RALEIGH:
Edwards & Broughton, State Printers.
1903.
N. C. COLLEGE OF AGRICULTURE AND MECHANIC ARTS.
THE NORTH CAROLINA
AGRICULTURAL EXPERIMENT STATION
UNDER THE CONTROL OF THE
TRUSTEES OF THE A. AND M. COLLEGE
S. L. Patterson, ex officio Chairman, Raleigh.
J. B. Coffield Evei etts.
E. L. Daughtridge Rocky Mount.
Wm. Dunn New Bern.
C.N. Allen ... _ . Auburn.
J. S. Cuningham Cunningham
A. T. McCallum Red Springs.
J. P. McRae Laurinburg.
P. B. Kennedy Daltonia.
W. A. Graham Machpelah.
A. Cannon Horse Shoe.
Howard Browning .. Littleton.
J. R. Joyce Reidsville.
G. E. Flow Monroe.
J. C. Ray Boone.
Geo. T. Winston, LL. D . President of the College.
STATION STAFF.
B. W. Kilgore Director.
W. A. Withers Chemist.
W. F. Massey Horticulturist.
C. W. Burkett Agriculturist.
Tait Butler Veterinarian.
G. S. Fraps Assistant Chemist.
H. P. Richardson . Poultryman.
B. F. Walton Assistant in Field Experiments.
B. S. Skinner Farm Superintendent.
A. F. Bowen ...Bursar.
The Director's office is in the Agricultural Building, Raleigh ; the experi-ment
grounds and laboratories being at the Agricultural College just west of
town and on the street car line.
Visitors will be welcome at all times, and will be given every opportunity
to inspect the work of the Station. Bulletins and reports are mailed free to all
residents of the State upon application.
Address all communications to
THE AGRICULTURAL EXPERIMENT STATION,
RALEIGH. N. C.
TABLE OF CONTENTS.
PAGE.
Board of Trustees and Experiment Station Staff - _ . . 2
Letter of Transmittal 5
Letter of Submittal _
.
6
Report of the Director _ 7
Report of the Chief of the Agricultural Division 13
Report of the Chief of the Chemical Division 15
Report of the Chief of the Division of Horticulture, Botany and Ento-mology
18
Report of the Veterinary Division 29
Financial Statement for the year ending June 30, 1902 30
Papers-
Nitrification in Different Soils 31
Determination of Sulphur in Plants 42
Determination of Sulphur and Chlorine in Plants _ 44
Solubility of Barium Sulphate in Ferric Chloride, Aluminium Chloride
and Magnesium Chloride _ 50
Sulphur Content of Some Vegetable Materials 54
Determination of Pentosan-Free Crude Fiber 59
Press Bulletins
—
Cabbage Snakes ...<V. _..'._'_ Q^J^U.. 63
Anthracnose or "Black Rust" of Cotton 1 64
Bulletin-
Number 181, Silk Culture.
LETTER OF TRANSMITTAL,
Raleigh, K C., June 30, 1902.
To His Excellency; Charles B. Aycock,
Governor of North Carolina.
Sir :—I ha,ve the honor to transmit herewith the report of the oper-ations
of the Agricultural Experiment Station of the North Carolina
College of Agriculture and Mechanic Arts, for the year beginning
July 1/1901, and ending June 30, 1902.
Very respectfully, S. L. Patterson,
Chairman Board of Trustees.
LETTER OF SUBMITTAL.
The North Carolina Agricutural Experiment Station,
Office of the Director,
Raleigh, 1ST. CL, June 30, 1902".
Hon. S. L. Patterson, Chairman Board of Trustees.
Sir :—I Lave the honor to submit herewith the report of the opera-tions
of the North Carolina Agricultural Experiment Station of the
North Carolina College of Agriculture and Mechanic Arts, for
the year ending June 30, 1902.
This report is made in accordance with that portion of Section 3 of
the Hatch Act of the Congress of the United State®, relating to the
agricultural experiment stations and their maintenance in the several
States and Territories, and which requires said stations "annually, on
or before the 1st day of February, to make to the Governor of the
State or Territory in which it is located, a full and detailed report of
its operations, including a statement of receipts and expenditures."
Trusting that this report will prove satisfactory, I am,
Very respectfully, B. W. Kilgore,
Director.
TWENTY-FIFTH ANNUAL REPORT
OF THE DIRECTOR OF THE
N. C. AGRICULTURAL EXPERIMENT STATION
For the Year Ending June 30th, 1902.
By the Director.
CHANGES IN THE STATION STAFF.
The present Director assumed charge of the work of the: Station at
the beginning of this fiscal year, July 1, 1901, in accordance with the
action of the Board of Agriculture, in charge of the Experiment Sta-tion,
as recorded in the report, of the Director of the Station for the
previous year.
Shortly afterwards Prof. 0. W. Burkett, of the New Hampshire
Agricultural College and Experiment: Station, was made Professor of
Agriculture in the college, and Agriculturist to the Station ; Dr. Tait
Butler, of the Kansas Agricultural College and Experiment Station,
was elected Veterinarian to the Station ; Mr. H. P. Richardson, of the
New Hampshire College, was put. in charge of the poultry work, and
Mr. B. F. Walton, a former graduate of the North Carolina Agricul-tural
College, was made Assistant in Eield Experiments, to perform,
in part, the work done by Mr. A. Rhodes, who' resigned to accept the
position of Horticulturist to the Georgia Normal and Industrial
School.
WORK IN THE AGRICULTURAL DIVISION.
Practically no experimental work was found in operation in the
Agricultural Division of the Station on July 1, 1901. It was, there-fore,
necessary not only to plan and put in operation an entirely new
set of experiments to deal with our important agricultural problems,
but new land had to be prepared on which to conduct the experiments.
This necessarily delayed operations., and will still longer delay the
obtaining of results of field experiments for publication in bulletin
form, .as this class of work, to be of the greatest value, must not only
be carefully planned and carried out, but must be continued for a
number of years, so as to make reasonably sure of the accuracy of the
conclusions. A start was made at once, and a field of about sixty-five
(65) acres has been cleared in part* and laid out in twentieth and
tenth acre and larger plats for our permanent work in agricultural
lines.
The Type of Soil.—The field experiments are on the ridge to the
North Carolina State Library
Raleigh
8 TWENTY-FIFTH ANNUAL REPORT, 1902.
southwest of the college buildings, the soil being a fairly good type of
what is generally known as gray land. It is a sandy loam, six to ten
inches deep, underlaid by stiff red clay. In the soil survey work of
the Bureau of Soils of the United States Department of Agriculture
this soil is designated "Cecil Sandy Loam."
Experiments with Cotton.—Forty-seven one-twentieth-acre plats of
this land are devoted to experiments with cotton, in testing flat as
compared with ridge culture, and frequent in comparison with infre-quent
cultivation ; in comparing a number of the varieties of cotton as
to productiveness, time of maturity, and length and strength of fiber
;
in growing cotton in a, number of rotations with corn, grains and le-guminous
crops, including peas, vetch and Burr clover ; in determin-ing
the yield of cotton with similar total amounts of fertilizer, but with
widely varying proportions of nitrogen, phosphoric acid and potash,
and with varying applications, to see what is the most profitable! quan-tity
of fertilizer to use to the acre. Tests are also included with cot-ton
in different width rows and different distances in the rows.
These experiments were planned by the Director and Agriculturist
and are practically a duplication of tests in progress for the past three
years on two types of sandy soils in the eastern part of the State. A
similar set will be started next spring on the red clay lands in the
Piedmont section of the State in Iredell County, the idea being to
obtain and bring together the results of these tests relating to cotton
culture on the several type soils and sections of the State, with the
view of being then better able to suggest; and help1 introduce varieties,
culture methods, fertilization, and rotations that are best suited to our
different soils and sections. The experiments away from the main
Station at Raleigh are being conducted by the State Department of
Agriculture, and are so arranged as to fit into and supplement the
Station work. In this way the two institutions, working according to
one general experimental plan, hope to eventually cover reasonably
well the broad field of agriculture in the State. It is certainly in
need of every possible assistance and deserving of the most powerful
efforts.
Experiments with Corn.—Similar tests to those referred to above
are being conducted with corn, and in addition, experiments as to
time and methods of planting have been added by the Agriculturist.
This work with corn is also< being repeated away from the main
Station and along with the tests of cotton.
Grasses and Legumes for Pasture and for Hay.—Ninety to one
hundred different grasses and legumes and combinations of these for
pasture and for hay are being tested on small plats here, and on the
sandy soils of the eastern part of the State, and next spring the same
series will be put out in the Piedmont section. After a few years'
tests we hope to be able, by bringing together the results obtained on
REPORT OF DIRECTOR. 9
the different type soils, to recommend the grasses and legume® best
suited to different localities.
Beef Production.—Past and present high prices of beef lend attrac-tiveness
to the beef industry. Last winter the Station obtained in
Missouri, through the assistance and courtesy of the Director of the
Missouri Experiment Station, thirty-nine head of thoroughbred and
high-grade beef animals of the Aberdeen-Angus breed, for the use of
the Station, Department of Agriculture!, and for a number of farmers
in the State. Sixteen head of these were kept by the Station as a
nucleus of a beef herd. It is the purpose of the Station to make beef
production and dairying and grass and forage plant production lead-ing
lines of its work. To this end and to develop' as fully and rapidly
as possible all phases of the strictly agricultural lines of the State, the
Agriculturist has been given every assistance the Station could afford
and as fast as it could be used to advantage toward bringing this
about.
Poultry Work.—The poultry interests of the State are more im-portant
than ever before, and the inquiries which come to the Station
on this subject, are frequent, intelligent' and deserving of the best
attention. Considerable additions have been made to the equipment
of the poultry plant in the Avay of incubators, brooders, and stock of
good breeds and breeding. To deal with the questions relating to the
breeding, care and handling of poultry requires skill and experience.
It is our purpose to put this phase of Station work on the highest
plane it can afford.
WORK IN THE HORTICULTURAL DIVISION.
The report of the Horticulturist gives in considerable detail the
work which has been carried on during the past year. The main
questions under investigation have related to the growing of peaches,
plums, pears and apples, the Station having a, considerable number of
trees of the different varieties of these several fruits. It also has a
large number of varieties of grapes and strawberries under test, and
has conducted experiments during the year with tomatoes out of doors
and under glass, with potatoes, sweet corn, etc. An effort is being
made to introduce the culture of the newer and higher priced kinds of
bulbs in the eastern part of the State.
The Horticulturist's time is perhaps taken up more largely than
any other Station worker, outside of the Director, with correspond-ence
with the farmers of the State.
WORK IN THE CHEMICAL DIVISION.
The investigations in the Chemical Division of the Station are gen-erally
more technical than those conducted by the other workers.
The work the past year has been principally in continuation of experi-
10 TWENTY-FIFTH ANNUAL REPORT, 1902,
nients already begun, and relate mainly to the study of the rat© at
which nitrogenous fertilizer materials nitrify and become available
for plant food in different soils. Quite a difference has been found
in the action of different soils, which is attributed to the presence' or
absence of bacteria in some and not in others. This work will be con-tinued
with a view to determining definitely the cause
? and should it
be found that bacteria, are responsible for the difference, it will be
interesting to follow the matter further and see if it will be possible or
profitable to handle different soils so as to get into them bacteria of
the most beneficial kinds. This would be a similar experience to that
with which we are all now so familiar as regards the necessity of
special bacteria in connection with the growth of leguminons crops.
The chemical work has also shown that sulphur is present in plants in
much larger proportion that has been heretofore supposed, and that
it, in fact, is as abundant in many cases as phosphoric acid, which
makes it desirable to make a closer study than ever has been done in
regard to the effect of sulphur as a fertilizer for different crops and
soils. Other work in the Chemical Department has been in the study
of methods for the analysis of various materials.
Papers of a more or less technical nature, giving the results of
chemical work, are included in this report, as follows
I. Nitrification in Different Soils.
II. The Determination of Sulphur in Plants.
III. The Determination of Sulphur and Chlorine in Plants.
IV. The Solubility of Barium Sulphate in Ferric Chloride, Alum-inium
Chloride, and Magnesium Chloride.
V. The Sulphur Content of Some Vegetable Materials.
VI. The Determination of Pentason-free Crude Fiber.
WORK IN THE VETERINARY DIVISION.
By far the greater portion of the time of the Veterinarian has been
occupied in work relating to> the extermination of the cattle tick, or
the inoculation of cattle, to render1 them immune against tick or Texas
fever when put on tick-infested pastures. Twenty-two head of the
Northern cattle purchased last winter were thus inoculated. One
animal died from the fever produced by this treatment, the rest hav-ing
lived and done well, though they are carrying large numbers of
ticks. The data obtained in this work will be used when further
added to for a bulletin on the subject.
The beef cattle brought from; the North have attracted so much at-tention
that a large number of requests have come to the Station for
similar ones, and we are now arranging to purchase a further lot for
farmers in different, parts of the State, who have already placed their
orders for animals. It would be unsafe to put cattle obtained north
of the tick line on tick-infested pastures, on account of the heavy loss
REPORT OF DIRECTOR. 11
from death, which would certainty follow. To aid farmers in this
matter the Station; is offering to inoculate free cattle obtained beyond
the tick line>, and which are subject to the fever.
farmers' institutes.
The Station has aided the Commissioner of Agriculture in con-ducting
Farmers' Institutes by sending members of the staff whenever
called on by him for this duty. We consider this a most valuable
phase of agricultural work—one which should be encouraged and ex-tended
in every way possible.
PUBLICATIONS.
On account of there being no' completed work at the beginning of
the fiscal year and very little in progress at that time, no results have
been available for publication during the year, except from the Chem-ical
Division, which has furnished a. number of papers, already re-ferred
to in this report, and occurring elsewhere in it. These might
have been issued as one or more technical bulletins, but it has been de-cided
to make the annual report the medium for distributing and pie-serving
this class of investigations, reserving their publication in bul-letin
form1 until the work has progressed and been tested sufficiently
to warrant deductions that, are susceptible of application by the
farmer.
Only one Bulletin, has been issued
—
iSTo. 181—Silk Culture, by Gerald McCarthy.
And three press Bulletins—
No. 1—Silk Worm Feeding Chart.
Eo. 2—So-called "Cabbage Snakes/'
No. 3—Anthracnose or "Black Bust" of Cotton.
Press Bulletins on timely subjects and containing matter of imme-diate
interest and usefulness to the farmers are being issued fre-quently
now, and it is proposed to make them a feature of the Station
publications. They do and will contain concise information most
frequently asked for by farmers in their correspondence with the
Station.
CORRESPONDENCE AND CONCLUSION.
The large number of letters of inquiry which come to' the Station
covering the various: phases of farm, operations show that our farmers
are interested in the Station and its work, and are looking to it for
assistance in their farming matters.
It is our hope and purpose to make the Station more and more in-dispensable
to the farmers of the State as the years go- by. They are
invited to treat it! as their own and to come to it for help on all mat-ters
relating to their work. We shall be glad to advise with them re^
12 TWENTY-FIFTH ANNUAL REPORT. 1902.
garding their operations, and shall in like manner be glad to have
theni suggest and advise with us in the conduct of our and their ex-perimental
work.
REPORTS OF HEADS OF DIVISIONS AND FINANCIAL STATEMENT.
The reports of the heads of the several divisions of the Station's
work and the financial statement follow:
REPORT OF THE AGRICULTURAL DIVISION. 13
REPORT OF THE AGRICULTURAL DIVISION.
Prof. B. W. Kilgore, Director.
Sir :—The work of the past year in the Division of Agriculture has
been primarily along preparatory lines for investigations. The first
thing done in the division, after assuming the duties of Agriculturist^
was the selection of suitable grounds for experimentation and the
separation of twentieth and tenth-acre areas for plot experiments.
A site was selected early in the season for permanent! work and now
about 400 plots are available and being used the present year.
AGRONOMY AND PLANT PRODUCTION.
The four hundred plots used for investigation in agronomy and
plant production are employed in the following lines of work
:
1. Soil improvement by means of leguminuous crops and ferti-lizers.
2. Method of culture, 'varieties and fertilization for cotton.
3. Method of culture, varieties and fertilization for com.
4. Testing of varieties!, methods of culture and fertilization for
cow peas.
5. "Wheat culture in relation to cow peas.
6. Forage crops and grasses.
The work in these several lines is of a permanent nature and outr
lined to cover a series of years. The work will be" enlarged so as to
cover all new questions arising from the investigations now begun.
WORK WITH POULTRY.
The poultry plant is. a permanent feature of the Station, and in the
change of location and enlarged conditions of the work, the division
will be enabled to carry on work of considerable importance in egg
production, the raising of fowls in practical and economical ways,
feeding rations for poultry, comparing incubators, fertility of eggs,
etc.
For successful work in poultry raising, range must be provided.
The fact is clearly proved that close confinement makes poultry rais-ing
unprofitable.
FEEDING HORSES AND MULES.
During the past year the division has" conducted feeding experi-ments
with the college horses and mules. A great many feeding
stuffs have been compared and the effect of feed and labor on weight
recorded. At the end of the feeding period, which is twelve months
in length, the result will be presented in bulletin form.
14 TWENTY-FIFTH ANNUAL REPORT, 1902.
BEEF PRODUCTION.
The division, believing the beef industry of growing importance in
this State, early in the year secured a nucleus beef herd, for investiga-tion
in breeding, raising and managing beef cattle under Southern
conditions.
An Aberdeen-Angus bull and two heifers of pure breeding, and
several high-grade heifers of the same breed, were purchased.
The division will make its investigation along the lines of raising
beef animals, comparing some of our breeding stuff for beef produc-tion,
comparing the well-bred with the native stock, and the adapta-bility
of beef raising to the agriculture of the State.
THE DAIRY INDUSTRY.
Since a good part of the manufactured dairy products used in the
State is brought from other States, it follows that the dairy industry
is one of great and growing importance. This is doubly so on account
of the marvelous development of manufacturing interests in the State.
The division is giving careful attention to dairy education. The im-provement
of dairy stock and the production of milk and butter. The
whole college herd, of fifty cows-, are used in this investigation. The
lines being considered are: The cost of producing milk and butter
with Southern feeds and under Southern conditions ; the milk and
butter capacity of dairy cows ; comparison of feeding stuffs raised in
the State, etc.
A careful record of each cow^ is being kept. The milk of every
cow at every milking is recorded and sampled for determination of
butter contents. Other phases of dairying are also being studied.
Respectfully submitted, Charles W. Burkett,
Agriculturist.
REPORT Or THE CHEMICAL DIVISION. 15
KEPOET OF THE CHEMICAL DIVISION.
Prof. B. W. Kilgore, Director.
Sir :—I havei the honor to submit the following report of the work
of the Chemical Division for the year ending June 30, 1902 : .
PLANT NUTRITION.
Minimum Requirements of Plant Food for Crops.—These experi-ments,
which were begun in 1S9 9, and which are referred to in re-ports
of the Station previous to this, have been continued during the
year.
Studies in Nitrification.—The work of this division during the
year previous* led toi the belief that in different soils may be found
different nitrifying organisms. T'01 test this theory ammonium, sulph-ate
and cotton-seed meal were submitted to nitrification in eleven
soils of various sources, both with and without, the additon of calcium
carbonate. The soils came from North Carolina, Florida, Massachu-setts
and Rhode Island. The results of the work show that in some
soils nitrification of ammonium! sulphate took place more rapidly and
in others less rapidly than cotton-seed meal, thereby serving to con-firm
the theories advanced to explain the results of our previous work.
An article containing the result of this work is submitted herewith.
A report of the work was read before the Association of Official Agri-cultural
Chemists at its meeting in 1901, and appears in the printed
report of the proceedings of that, meeting. It- also appears in the
Journal of the American Chemical Society for 1902, pages 528
to 534.
Since the completion of the work referred to we: have treated
chabazite with an ammonium salt and subjected the product after
washing to' nitrification by various soils in comparison with am-monium
sulphate and cotton-seed meal. The soils used by us nitri-fied
ammonium sulphate less rapidly than cotton-seed meal, but in
every case the ammonia fixed by the chabazite was nitrified more
rapidly than either of the other1 nitrogenous materials. Some- further
experiments, along this line are in progress.
COMPOSITION OF PLANTS.
Sulphur in Plants.—It has been customary heretofore to estimate
the amount of sulphur in plants from the analysis of the ash. In
making an investigation of the method for determining sulphur, it
was ascertained by this division that a large parti of the sulphur in
plants was driven off by burning and did not appear in the ash. In
consequence of this the sulphur1 content of various plants has been
*24th Annual Report, pp. 8, 9, and 13-24.
1G TWENTY-FIFTH ANNUAL REPORT. 1902.
estimated too low and the importance of that element, so far as
quantity is concerned, at least, has been under-rated.
The number of samples analyzed was as follows:
Cotton-seed meal 10
Cotton-seed hulls 6
Cotton-seed kernels . . . . 2
Lint cotton 3
Tobacco 4
Kernels . . . . 2
Peas 6
Corn 8
Beans 18
Peanuts 3
Onions 1
As a result, of this work it has been found that instead of sulphur
being present in plants in almost insignificant quantities, in some
cases it is present in very much larger quantities. ; in many cases sur-passing
that of phosphoric acid, lime, magnesia, and even potash.
METHODS OF ANALYSIS.
Determination of Sitlphur in Plants —As stated above, it has
been found that much of the sulphur in vegetable materials
is driven off by burning, and does not remain in the ash.
consequently, the sulphur found in the ash does not truly represent the
amount present in the entire plant. This division proposes a method
which is described in an article submitted herewith, together with the
experiments connected with the work. The result of this work is re-ported
in the Journal of the American Chemical Society, pages 24,
346, and to the Association of Official Agricultural Chemists, (See
Proceedings 1901.)
Determination* of Chlorine in Plants.—The object of our work was
to devise a satisfactory method for the determination of chlorine in
plants. A report of the work is submitted herewith.
Solubility of Barium Sulphate.—In the work on the determination
of sulphuric acid in soils, Mr. C. B. Williams, Assistant Chemist in
the North Carolina Department of Agriculture, found that consider-ably
more barium sulphate was obtained, when the iron and alumi-mium
had been previously precipitated from the soil solution. As
the precipitation of the barium sulphate takes place in the presence
of these salts, the accuracy of the determination of sulphur depends
upon the solubility of barium sulphate. A paper embodying the
results of tins investigation accompanies this report. The same
REPORT OF THE CHEMICAL DIVISION. 17
paper has appeared in the American Chemical Journal [£7, 288
(1902)].
Determination of Pentosan-free Crude Fiber.—When crude fiber
is determined in feeding stuffs according to the methods of the Asso-ciation
of Official Agricultural Chemists, it contains pentosans in ad-dition.
To remedy this difficulty, a determination should be made
of the pentosans in crude fiber, or there should be a method for ob-taining
a crude fiber which should be free from pentosans. Atten-
1 ion has been called by this Division to a method devised by J. Konig
for obtaining pentosan-free crude fiber. Tests of the method were
made with satisfactory results. A paper containing the results of
this investigation accompanies this report. The same was read be-fore
the Association of Official Agricultural Chemists at its meet-ing
in 1901, and is to be found in the printed report of the proceed-ings'
of that meeting.
CONCLUSION.
I desire to express my high appreciation of the work of Dr. G. S.
Fraps, Assistant! Chemist.
Very respectfully, W. A. Withers,
Chemist.
18 TWENTY-FIFTH ANNUAL REPORT. 1902
REPORT OF THE HORTICULTURAL DIVISION.
Prof. B. W. Kilgore, Director.
Dear Sir :
I have pleasure in reiporrting that the plantation of fruit trees is in a
very thrifty condition, and so far has not been troubled by attacks of
insects, except the ever present Curculio. The peaches and plums,
most of them, bore their first fruit this, season. This is true: of the
Japanese and American plum varieties. The; domestic sorts of
European origin have not yet fruited. Plums of the varieties fruited
seem to, come to. normal size and perfection where they did not rot.
The rot was quite bad with some sorts. The Burbank plum rotted
bodily, though the cropi set wa,s a full one. It is evident that spray-ing
with fungicides must begin with the plums at an early stage in
the season and before any swelling of the buds, as the fungi seem to
gain entrance by the blossoms. I hope to have better success in
checking the rot. another season, The plums and peaches were sprayed
with arsenite of lead as a, check to the Curculio. If the spraying had
been repeated more: frequently there would doubtless have, been better
results. Another1 season I shall use the jarring method, and the
gathering of bitten fruit: and insects, as well as the arsenite. The
arsenite of lead has the advantage that it does not injure the foliage
of peaches as Bordeaux mixture and Paris green are certain to do.
One row of peaches most exposed to the sun was sprayed all over
with whitewash for the purpose of retarding the bloom by whitening
the shoots, thus reflecting the heat. Though rain came directly after
washing, the whitewash on many of the trees remained sufficiently to
show that it did have some effect in retarding the bloom, as the trees
were somewhat later than others, down the slope, north of them. In a
general way I have to report, that the peaches in our red clay soil here
do not seem to attain the size or have the color that they do on lighter
soil elsewhere in the State. From the lack of characteristic color it is
hard to recognize varieties with which I am perfectly familiar. I
have noticed this fact elsewhere in the neighborhood of Raleigh, and it
lead's to a, serious doubt as to whether the growing of peaches can ever
be made a commercial success, here. A few rows of the peach trees
have been left uncultivated, but the ground liberally manured. This,
too', is for the purpose of testing the effect on the retarding of the
bloom in spring, since it has seemed that trees well cultivated in the
early season start into bloom' sooner than those in. uncultivated land.
REPORT OF THE HORTICULTURAL DIVISION. 19
I>y manuring these trees have nuaide fully as good a growth as those in
cultivated ground. In fact, the growth of all the trees is as strong as
there can be any wish for. The pear and apple orchard is doing well.
These were cultivated all through the early part of the season, and
then peas were planted in rows between the trees, and these were cul-tivated
till July, when cultivation stopped, in order that the trees may
fully mature their growth.
GRAPES.
Two years ago, by the courtesy of the Georgia Station, I received
cuttings of 300 varieties of grapes. These were rooted, and last year
were planted in a small vineyard for trial. Last year the season was
against them and the land very poor and unmanured. Hence, the
growth was small. This season they have been well manured and
have had a topi dressing of nitrate- of soda, and have been kept to' a
single cane. The growth has been fine and they will be ready for the
trellis the coming spring. I propose to use the same shelter trellis
that I found so successful at Southern Pines. This, is a modification
of what is called the Munson trellis, and it. is found that there is far
less tendency to rot on such a trellis. The trellis is made by setting
stout posts along the- rows ten feet apart and nailing strong cross
pieces to the tops: four feet from the! ground. Three wires are
stretched, one along the tops of the posts and the others at each end 01
the three-foot cross pieces. The arms- are then taken along the cen-tral
wire: and the fruiting shoots hang over the outer ones and form a
complete shelter to1 the fruit beneath. My experiments years, ago
showed that a board coping over a trellis was just as effective! in pre-venting
rot as the most careful spraying, and this method of training
has some' of the effect, of the board coping. Two' rows, of peas have
been planted between the rows of grape vines for the purpose of fur-nishing
organic matter to the soil.
TOMATOES.
The experiments in growing1 tomatoes under glass were continued
the past winter1
. Heretofore I have been forcing the tomatoes in
large pots. The past season I planted them, in a solid bed in the centre
of the greenhouse. This bed was made of a well-prepared compost of
rotted sods and manure, and had a, top' dressiing of stable manure after
the plants were set. But two varieties were planted—Maule's Ear-liest
and the Dwarf Champion. Twenty-six plants of each were set.
The growth was all that could be desired, and the. crop was a good one.
A heavier crop would have been had, had the blossoms, been more
regularly fertilized with pollen. As there are at that time no insects
to help in this, the setting of the blooms must be done by hand. 1
had to depend for this largely on the help1 of inexperienced students.
20 TWENTY-FIFTH ANNUAL REPORT, 1902.
and after the plants got. very tall it was. not done as fully as it should
have been, and many very small tomatoes resulted. The plants were
trained to single stems, and grew nearly ten feet high during the
season. From the 26 plants of Maule's Earliest we. gathered 268
pounds of tomatoes, and from the 26 plants of Dwarf Champion 142
pounds of fruit. The Dwarf Champions were largely overshadowed
by the more rapid growing plants of Maule's Earliest, and if the
whole; bed had been set, with them the result, would have: perhaps been
better. The fruit of Maule's Earliest is inclined to be rough and
wrinkled, while that of Dwarf Champion is uniformly smooth. The
Earliest would be a first-class forcing tomato if it could be bred into a
smooth shape. The result showed that if we had a house: properly
suited to the tomato:, which the college houses are not, the winter
forcing of tomatoes, can be made a profitable business, and when our
market growers fully realize and learn what can be done in our sunny
climate under glass, the business will develop: greatly. In the open
ground I have: grown this season 26 varieties of tomatoes. This fruit
has now been brought, to such a, degree of perfection that there is little
to. choose between the leading varieties. My plantation was. more for
the purpose of observing the1 degree of resistance of the' varieties to
the Southern Blight, and to select seed fromi resistant sorts. The re-sults
this season have been rather of a negative character, since the
land in which the plants were set has: probably never before been
planted in tomatoes, and is not, as yet infected with the Blight bac-teria,
so: that, no disease has appeared. This very fact, however,
shows the importance of avoiding land where tomatoes: or potatoes
have recently been grown. It. has long been noticed that the1 small
plum-shaped tomatoes are uniformly resistant to the Blight,. In hope
of getting some of this resistant quality in tomatoes, I have saved seed
from some: of the finest of the- larger tomatoes crossed with these: small
and resistant, ones, and will use these: in our work another season.
LETTUCE.
The growing of frame lettuce: during the winter under cloth and
olass has developed to such an extent in the eastern part, of this State
that it was thought, that some' experiments: with fertilizers for this
crop would be valuable. It was planned to1 make this experiment in
frames covered with glass. There were two lines, of frames with 24
and 18 sashes, respectively. The sashes are: the ordinary hot-bed
sashes, 3 by 6 feet each, and the plot® were arranged to take two
sashes each. For the purpose of getting an unaltered soil the frames
were excavated and a soil collected from1 a thin, poor piece of wood-land
mixed with washed sand was filled in the place of the soil re-moved.
This soil was found to- be exceedingly deficient in all the
elements of fertility. The following plan of fertilization was adopted,
REPORT OF THE HORTICULTURAL DIVISION. 21
placing the normal application of nitrogen, phosphoric acid and
potash at 100 pounds per acre, N in the table standing for 100 pounds
per acre of nitrogen, P for phosphoric acid, and K for potash, in same
amount
Plot
3,4,6
FIRST FRAME.
1. K P.
2. K. N.
3. N. P.
4 N P. K.
5. Ns P. K.
6. O.
7. N. Ps. K.
8. N. P. Ks.
9. 2.N. P. K.)
10. i (N P. K.)
11. N P. K. L
12. N. P. K. L. S
SECOND FRAME.
Plot 1. N. P.K. and stable manure.
2. N. P K.
,7,8,9 N. P. K.
5. O.
The plots 3, 4, 6, 7, 8, 9 were intended for a, variety test, but the
plants failed, and only one variety, the Big Boston, was used. This
is the variety most commonly grown by the market growers. The re-sult
of this experiment seems to show that in our clay soil commercial
fertilizers alone will fail to make' good lettuce. The. crop in these
frames was; very slow! in growth, and the product of all the plots was
inferior, and sold for less than half the price obtained for first-class
lettuce. The average weights of all the heads was four ounces, while
jjlants raised from the same seed, sown at the same time, but treated
in a commercial way, made heads weighing .... pounds and over,
and were sold and the frames, replanted before any of this lettuce was
headed. The frames in my home! garden were filled with a well
rotted compost of sods and stable manure, and a complete fertilizer
applied in addition at rate of one ton per1 acre. In our clay soil here
well rotted stable manure is essential to the production of fine lettuce
in winter. The plots having some stable manure made better lettuce
than the others, but the: manure ivas of too coarse and fresh a condi-tion
to give the best results. A tabulated statement of these plots
will be given in bulletin on this work. It is found that, with glass
sashes and mats to cover them in very severe weather1 we can grow as
good lettuce, or better, than the growers in the eastern part, of the
State get under their cloth covers. In the long run the glass is the
cheaper of the two, and when our growers find out. the value of glass
fully they will abandon the use of cloth.
The variety tests planned for the lettuce were not carried out be^
22 TWENTY-FIFTH ANNUAL REPORT, 1902.
cause of the partial failure of the fertilizer crop, and the fact that it
occupied the frames during the entire winter. I am planning for a
very complete variety test of lettuces during the coming winter, as it
is of the greatest importance to our market growers to' find the variety
best suited to their work. From results gotten in my home garden I
am of the opinion that no one variety will be found suited for the
entire season from December till May. A rather1 smaller and earlier
variety, like Rawson's Hothouse lettuce, will be best for the December
and Christmas market-, a plentiful supply of plants of the Big Boston
being in the meantime provided for the immediate replanting of the
frames. This crop will come off in March, and after this there is a
strong demand for Southern lettuce that should be met during April,
when the price is apt to be higher than at any other time. For this
crop we have found a, large wrinkled leaf variety, similar to the; Han-son,
and called the Wonderful, which is admirably suited. If frames
are set with this, and only protected by cloth or glass in the most
severe weather, simply enough to prevent their being killed, they will
come on at the right, time and will make immense heads of great
solidity, weighing from two to four pounds. I ami inclined to- think
that our market, growers will find this about the most; profitable crop.
The Wonderful lettuce is not suited to; the winter heading crop, as it
will not head well till spring. But, for the spring crop during April
it promises to be the best, so far1 as our experiments have gome. With
a specially prepared compost and heavy additional fertilization it is
hoped to demonstrate the value of the three-crop system of growing
frame lettuce in the South. The first sowing of seed will be made as
usual the third week in August, and other sowings of Big Boston and
Wonderful from first to middle of September. By the use of glass
sashes and mats the crop of winter frame lettuce can be grown suc^
cessfully in any part, of the State east of the Blue Ridge as success-fully
as in the market garden region of the Eastern section. I esti-mate
that it will require an expenditure of $4,000.00 to cover an acre
with frames and glass sashes, and that the first winter and spring
crop' will pay for1 the sashes and frames, while the cost of cloth cov-ered
frames is fully $500 per acre, and the cloth has to be renewed
every two years, and sometimes in one season, while the sashes are
good for twenty years, at: least, if taken care of. I have now sashes
that have been in use for thirteen years and are still in good shape.
Hence, in the long run I think the market growers will find the glass
not only better than cloth, in giving a better1 product, but cheaper.
For covering the sashes in very cold nights I ami using at the Sta-tion
mats made of broomsedge, woven on strands of tarred twine.
These were made by the students and farm hands, and have been in
use two winters, and are still good. I have also1 in my private garden
REPORT OF THE HORTICULTURAL DIVISION. 23
mats bought in New York. These are. six feet square and are made
of two thicknesses of burlaps with waste wool quilted, between. These
I find to keep: out frost completely, and with their protection I had
hyacinths, tulips, narcissus, violets and freesias in bloom, during the
winter in my frames.
This fact opens up another prospective industry for Eastern North
Carolina. Roman hyacinths, violets and narcissus are forced in the
North extensively in steam and hot-water heated greenhouses. Here
we can produce just as good flowers in a simple frame, covered with
glass, and as our florists get many cut flowers from the North all win-ter
in good shape after having been cut and sent to' the commission
merchants; in New York, it, would be perfectly easy, with the present
means for1 transportation, to pack and ship the cut flowers to New
York and other Northern, .cities during the winter, where our growers
could afford to sell at far lower prices than the Northern growers can.
The forced bulbs used in the heated houses North are worthless after
the forcing, while those grown more naturally in the frames really in-crease
in value, as they can be left to fully mature while the sashes
are removed to extra frames for later use. The uses that can be
profitably made in our climate of a simple frame and sash are innum-erable,
and the use of glass opens up a business, the profit of which
our growers can as yet have no' conception.
ROSES.
During the season of 1901 I planted and grew some thousands of
roses of various kinds in the open ground for one: of the Northern
dealers. The plants were sent, here already rooted and were set, in
rows for cultivation by horse power. The crop was dug and shipped
in the fall of 1901. Though there was a heavy loss of plants from
the first shipment, having been sent too early, and being caught by a
hard freeze just after setting, the result showed that a, gardener here
could make a fair1 profit by growing these contract roses.
The business of producing field-grown roses is gradually coming to
the South, since with our longer season we can produce a, better plant
than the Northern growers, and there is a tendency among the larger
dealers and growers there to have their roses grown in the South.
But the profit in this business would be far greater if the growers
here would prepare to propagate the plants at home and then go, on
the market at regular rates with their stock. The roses we grew
during the year past were grown for $2.00 per 100, the Northern
house paying the freight both ways. The regular trade prices for
these roses varies from! $50 to> $150 per thousand, according to the
value of the variety. Hence, it is easy to see that a, grower with
plenty of stock plants here, and facilities under glass for propagation
can make a larger profit than by growing on contract. And here the
4 TWENTY-FIFTH ANNUAL REPORT, 1902.
simple sashes and frames come into play again. With a single house
for rooting the cuttings they can be potted into' small pots, and win-tered
in the frames ready for the spring planting, or for sale during
the winter as young pot plants. This opens up a business, in which
large capital can be safely and profitably invested, and at least, one
^Northern firm has bought land in the South and is erecting houses
and frames for this purpose. Intensive horticulture, is just in its
infancy in the upper South. Our growers have learned the profit
there is in the slight, protection of the plant cloth, and little by little
they will grasp, the opportunity for enlarging their1 operations by the
the use of glass.
IRISH POTATOES.
In the section about Raleigh there has seemed to^ be a, particular
difficulty in the way of getting profitable crops of early Irish potatoes,
and the result is that nearly all the early potatoes sold in our market
are brought here from the South or the eastern part of this. State. I
endeavored to make a, small variety test., using two of the older
varieties, the Early Rose and Early Ohio, for comparison with a
number of newer sorts. They were planted in the best, soil we have
for the potato, a, soil well suited to the crop. I used in the furrow
under the potatoes a fertilizer composed of dried blood, sulphate of
potash and acid phosphate, these being the materials at hand. The
mixture was calculated to contain 4 per cent nitrogen., 8 per cent
phosphoric acid and 7 per cent potash. This was used at rate of
1,000 pounds per acre, One peck of each variety was planted, and
the weights of the crop' are given below. The growth in the early
part of the season was fine, until the hot and dry weather set. in, and
but for this the crop1 would have: been a very fine! one. The' plants
were sprayed twice with arsenate of lead, which cleaned up the beetles
and their larvae. No Bordeaux was used, and little or no blight was
observed. Like the tomatoes, the potatoes were on land which had
probably never been used for the cropi before:. Hence, the freedom,
from blight. The earlier varieties., it will be seen, made a larger crop
than the later ones, as these were more seriously damaged by the
drought and heat on land of a peculiarly thirsty nature.
REPORT OF THE HORTICULTURAL DIVISION. 25
Variety.
Early Ohio
Early Reel Bose
Early Rose
Thoroughbred
Commercial
Freeman
Bovee
Sir Walter Raleigh ._.
Junior Pride
Early State of Maine.
Total
Comparative
Earliness.
Weight
Crop.
of
Pounds.
1 148
2 130
2 160
3 200
5 110
4 98
5 285
5 186
4 150
4 160
1,627
The vield of the entire plot was at the rate of 108 bushels per acre,
not a large crop, but showing that in suitable soil here we can
grow a profitable crop of early potatoes and can sell them readily in
the local market, in a season1 of normal moisture and temperature.
SWEET CORN.
There has always been a. serious difficulty in getting an early sweet
corn with stamina; sufficient to succeed in, this climate. The later
varieties of Sugar Corn give fair crops, but it is very hard to get an
early one that is of any value here. The trouble arises largely from
the fact, that our people regularly get. seed of the sweet corn from the
seedsmen, and this seed is. produced in the North and is not. accli-mated
here. We planted this spring the following varieties in order
to> get completely cross, fertilized seed, from which we may developi by
selection a variety that will be early enough and which will grow well
here. Some years agoi I undertook this by crossing the Learning and
the Mammoth sugar corn. This was selected for seven years, till I
finally had a well fixed variety of fairly good and early corn, which
made a sufficient growth of stalk and had! good-sized ears. The fault
of this variety was a shallow grain and large cob-. Still, it. was well
suited to' our conditions. After leaving Southern Pines. I had no
place for the corn, and soi the crop was distributed all over the State,
with the notice that, no more would be grown here and that the re-cipients
would have to take care of it. I believe that this corn is no
longer in existence, and I now propose to select and grow a. pure, sweet
corn without, any cross of field corn, and hope that in a few years I
may be able to select and Hx such a variety as will have sufficient
growth and produce a fairly early crop for table use. Such a corn is
26 TWENTY-FIFTH ANNUAL REPORT, 1902.
badly needed by our market growers, who now depend mainly on such
varieties as Adams' Early for the early market, though this is not a
sugar corn, but a small early Dent variety. The varieties planted
this season for crossing were: First of All, Cory, Early Sheffield,
Early Champion, Stabler's Early, Mammoth Cory, Maule's XX,
Nonesuch, Black Mexican, Kendall's Early Giant, Perry's Hybrid,
Improved Giant, Metropolitan, Mamie's Mammoth, Zigzag Ever-green,
Stowell's Evergreen and Everbearing Egyptian.
The varieties most promising for this climate, and the ones that
should be used here in breeding by selection for a variety for our use
are the following: Country Gentleman, Zigzag Evergreen, Mam-moth,
Maule's Mammoth and Stowell's Evergreen. These will all
do fairly well in favorable soil, when grown from Northern seed, and
when carefully selected here will doubtless improve in adaptation to
the climate. I should have included in the above list the Egyptian, a
large corn of sturdy habit, that has been developed in Maryland, and
is perhaps at present better1 adapted to our climate than any other.
THE PRODUCTION OF FLOWERING BULBS FOR FLORISTS.
For many years the growers in Eastern North Carolina have been
supplying the markets, of New York and London with nearly all the
tuberose bulbs used by the florists of America and Europe. Owing
to> the fact that, there is a smaller demand for these than formerly, the
price has fallen so that the business is not as profitable as it once was.
Hoping to introduce the culture of other bulbs, which are, now im-ported
in immense quantities, from Europe and Bermuda, I began
several years ago to experiment in the culture of these bulbs here, and
especially with the Bermuda Easter Lily, which is now imported to
the extent, of about a million dollars worth annually. I was enabled
to do this through the liberality of the Northern dealers, who are in-terested
in the development, of the culture here, and sent me quanti-tis
of bulbs for trial. Last year, finding the soil at the Station farm
unsuited to this work, I determined to continue the experiments, at
my own expense on better soil in my home garden. With some bulbs
I have had fairly good success, but with the most important one, the
Easter Lily, I have not, as yet produced as fine bulbs as I could wish,
and I have found that the local conditions in this part of the State
will render the culture uncertain. Our soil dries out too rapidly and
the bulbs are stunted by drought- On the level black soils in the
eastern part of the State, such as are used so successfully for the
growing of strawberries, I feel sure that the lilies will be a success.
A paper which I presented at the meeting of the Society of American
Florists at Asheville this summer, attracted attention,, and it is hoped
that further experiments will be made in the eastern part of the State,
for which I can furnish a large amount, of sets for planting this fall.
REPORT OF THE HORTICULTURAL DIVISION. 27
In Southeast, Virginia a company with abundant capital has started
in the business of growing bulbs, and is being successful with the
same kinds thati I have succeeded with here, but I am not informed
whether they have grown the Bermuda Lily with success. All that is
needed in Eastern North Carolina is the investment of capital in the
work and the employment of skilled men to attend to it.
CANTALOUPES.
Some years ago> the town of Rocky Ford, Colorado', came into note
by reason of the excellence of the; cantaloupes grown there. The bus-iness
has increased there to a, large extent and hundreds of car loads
of Rocky Ford melons are sent East, and sold at paying prices. The
seedsmen put the Rocky Ford melon in their catalogues as a new
variety. It was soon found, however, that, it is simply the old Netted
Gemi melon, varied by soil and climate, and it became a matter of in-terest
to study the variations produced by climate on this melon. The
Department, of Agriculture at Washington asked me to undertake the
culture of this melon and send them samples' for chemical analysis, as
they proposed to have them grown in a variety of climates for this
purpose. The unfavorable season last, year wias against the success of
any melon, owing to the continual wet. weather. Hence, the Depart-ment
has asked that the experiment be continued, and I have again
planted this melon from seeds sent by the Department, but after re-peated
plantings have a poor stand of plants, and I am inclined to
believe that the Rocky Ford growers have palmed off some poor seed
on the Department. Enough will bo produced for the purpose den
sired, I suppose, and I shall look for the result of the analysis with
interest.
FOOD CROPS.
Having to support, a, team of horses, it became necessary to add
some forage to our regular1 work. A portion of land was sown last
fall to winter oats and hairy vetch, which has made a fairly good
crop1
, notwithstanding the fact that there was some winter killing of
the oats. I have planted also cow peas,, some of which were planted
as early as the' first of May and some later, and the sowing will be
continued after the oats grown for hay have been cut. The early
ones have been planted in rows and are to be cultivated, and it may
possibly be found that, this is the best way to grow) them, as less seed
is needed. The results will be given hereafter, as the late ones will
be broadcasted.
BOTANICAL.
In the line of botanical work my efforts have been confined to the
identification of plants sent in by correspondents. These have been
28 TWENTY-FIFTH ANNUAL REPORT. 1902
mainly grasses, and the number of specimens sent shows that our peo-ple
are taking more interest every year in the native grasses. I have
in every case written carefully and fully in regard to the specimens
sent, and have endeavored to advise in regard to culture, etc.
ENTOMOLOGICAL.
A great many correspondents send me specimens of insects for
identification and advice. In most cases I have been able to make an
intelligent, reply, but am glad to know that the Station now has the
services of an expert Entomologist.
Respectfully submitted, W. F. Massey,
Horticulturist.
REPORT OF THE VETERINARY DIVISION. 29
KEPOKT OF THE VETERINARY DIVISION.
Prof. B. W. Kilgore, Director.
Dear Sir :—I beg to submit the following report of tlie work done
by the Veterinarian of the Experiment Station during the past year.
The work has been confined to a study of the problems involved in
the extermination of the cattle tick (Boophilns Annulatus) and inocu-lation,
for the prevention of Texas or tick fever. Twenty-two head
of Northern cattle have been inoculated and placed upon tick-infested
pastures. They are all living and doing well. The temperatures of
these animals were taken once and twice daily for two months, and
the effect of the disease upon the number of red corpuscles in the
blood observed.
It is proposed to continue .this work and extend the observations
upon the blood of cattle the first summer after inoculation, as com-pared
with that of cattle immunized in the natural way. When the
work has been completed and sufficient data obtained the results will
be. offered for publication.
Yours respectfully, Tait Butler,
Veterinarian.
30 TWENTY-FIFTH ANNUAL REPORT, 1902.
North Carolina Agricultural Experiment Station in account with The
United States Appropriation, 1901-1902.
DR.
To Receipts from the Treasurer of the United States as per appropria-tion
for fiscal year ended June 30, 1902, as per act of Congress ap-proved
March 2, 1887 $15,000.00
CR.
By Salaries $8,203.77
Labor _ 1,585.45
Publications 80.82
Postage and stationery ... 117.60
Freight and express __ 250.30
Heat, light, water and power _ 9.03
Chemical supplies _ _
62 16
Seeds, plants and sundry supplies 190.42
Fertilizers 90.42
Feeding stuffs _ -._ 568 27
Library.... . . 12.97
Tools, implements and machinery _ 270.08
Furniture and fixtures 20.50
Scientific apparatus , 49.00
Livestock 2.890.87
Traveling expenses 58 55
Contingent expenses 210.00
Building and repairs 329. 79
Total .. ..$15,000.00
We, the undersigned duly appointed auditors of the Corporation, do hereby
certify that we have examined the books and accounts of the North Carolina
Experiment Station for the fiscal year ending June 30, 1902; that we have
found the same well kept and classified as above, and that the receipts for the
year from the Treasurer of the United States are shown to have been
$15,000.00 and the corresponding disbursements $15,000.00, for all of which
proper vouchers are on file, and have been by us examined and found correct,
thus leaving nothing.
And we further certify that the expenditures have been solely for the pur-poses
set forth in the Act of Congress approved March 2, 1887.
(Signed) S. L. Patteeson,
B. W. KlLGORE,
(Seal.) Auditors.
Attest: A. F. Bowen,
Custodian.
Nitrification in Different Soils.
By W. A. WITHERS, A.M., Chemist, and G. S. FRAPS, Ph.D , Assistant Chemist.
In a previous bulletin of this Station (No. 176, November, 1900)
were published the results of the nitrification of different fertilizer
materials in a pasture soil. The order1 of nitrification in the soil used
was dried blood (most nitrified), cotton-seed meal, dried fish, tankage,
bat guano, bone and ammoniumi sulphate. Excluding: the ammonium
sulphate, this is the order of availability of the nitrogen in these
fertilizers, as measured by vegetation tests, and solubility in per-manganate
of potash. When calcium1 carbonate was added to the soil
the nitrification was. greatly accelerated, and the order1 became dried
blood, cotton-seed meal, dried fish, bat guano, tankage, ammonium
sulphate, bone.
Results of two experiments by other workers were cited, in one of
which ammonium sulphate was nitrified to a greater extent than dried
blood and other materials tested, and in the other the ammonium
sulphate was nitrified less than oil cake, fish guano and dried blood,
whether calcium carbonate was added or not.
In view of the general opinion held in regard to the value: of am-monium
sulphate as a fertilizer, these results may seem extraordinary.
It is probable, however, that plants can assimilate ammonium: salts as
well as nitrates, just as they can get carbon from sugar as well as from
carbon dioxide.
The following explanation was advanced for the results of the ex-periments
just cited
There are three possible ways to account for the slow rate of nitrification of
ammonium sulphate.
1. Ammonium sulphate may hinder the action of the nitrifying organisms.
This explanation will not account for the beneficial action of calcium carbonate.
The assumption that ammonium sulphate hinders the action of the nitrifying
organism would explain the low rate of nitrification of ammonium sulphate that
we have obtained. It would also explain the results of Boname, according to
which ammonium sulphate is nitrified very slowly indeed the first and second
months, and very rapidly the third. In direct contradiction to the above
hypothesis, however, would stand the experiments of Muntz and Girard.
These difficulties might be explained away by supposing that the ammonium
sulphate affects the nitrifying germs less in some soils than in others, either on
account of the different character of the soils (power of fixing ammonia, etc.),
or the presence of different kinds of nitrifying organisms
2. The second explanation for the slow rate of nitrification of ammonium sul-phate,
compared with the other materials, is that the nitric and sulphuric acids
formed are detrimental to the nitrifying organisms, being neutralized only in
part by the bases of the soil. When calcium carbonate is added, it neutralizes
the acids, with consequent acceleration of the change. This explanation is prof
bably applicable, but does not explain all the facts, for, if so, the addition o
32 TWENTY-FIFTH ANNUAL REPORT, 1902.
calcium carbonate would remove the unfavorable conditions, and place ammo-nium
sulphate at the head of the list—which it does not do.
3. The third explanation is, that different soils contain different nitrifying
organisms, some of which convert organic matter directly to nitrites, while oth-ers
change ammonium salts to nitrites more readily. The nitrites are then con-verted
to nitrates. In soils containing the first kind of organisms, and few of
the second, organic matter would be converted to nitrites more rapid y than
ammonium salts would be, as was the case in the experiments of Boname, and
those here described. In soils in which the second class of organisms predomi-nate,
ammonium salts would be nitrified more rapidly than organic com-pounds.
This hypothesis would explain all the experiments here cited.
It appears very probable that all three of the explanations given above apply,
and that all three are in operation, one exerting a greater influence in some soils
than othei s.
It was our object, to test the last hypothesis, and the results of the
experiments will here be detailed.
Since the bulletin above alluded to was printed, the following addi-tional
work has come to our notice
P. Bonanie (Exp. Sta. Record, 12, 836), in continuing experi-ments
of previous years, obtained the following results:
TABLE I.
Nitric Nitrogen (in Mgr.) in 100 Gkams Soil.
Jan. 24. March 4.
Soil Alone
Ammonium Sul phate .__
Dried Blood
Fertilizer
Ammonium Sulphate and Lime
Dried Blood and Lime
Fertilizer and Lime
27.
50.
94.
66.
131.
73.
On May 20th the soil to which! ammonium) sulphate and lime had
been added contained as much nitric nitrogen as that which had re-ceived
blood and lime.
This is another case in which ammonium salts are nitrified less
rapidly than dried blood.
PLAN OF WORK.
The object of the work was to study the nitrification of ammonium
sulphate and cotton-seed meal in different soils, in order to see if the
soils would behave differently toward these substances.
The samples of soil was sifted through a coarse sieve, and the quan-tity
of cotton-seed meal or ammonium sulphate containing 0.8 gram
nitrogen was intimately mixed with 500 grams of the soil. The mix-ture
was then placed in precipitating jars and kept in a dark closet.
NITRIFICATION IN DIFFERENT SOILS. 33
When: calcium carbonate was added the amount was exactly enough
to combine with all the nitric acid and sulphuric acid which would be
formed if the ammonium sulphate were completely nitrified. The
amount ol water in the soils was about 15 per cent; at suitable periods
one or more jars in each set was weighed, and the estimated loss of
water was replaced in all the jars. The average moisture in the dif-ferent
sets is given in Table II.
At the end of three weeks, as a, rule, the nitrates were leached out
with 1000 c. c. water, and determined by the Tiemann-Schulze method
in an aliquot, portion of the filtrate. In each case correction was
made for the nitrates in the soil to which no nitrogen had been added.
DESCRIPTION OF SOILS.
The soils used were as follows
:
1667.—Pasture soil from the farm of this college; a light loam,
containing humus, and not acid to" litmus.
1668.—Heavy clay soil from the farm of this college, contains no
humus, possesses low fertility, and is slightly acid to litmus.
1669.—Black garden soil from the Florida Experiment Station;
contains much humus, and is acid to litmus,
1670.—Soil from the Massachusetts Hatch Experiment Station.
This soil has been used: in plot, experiments for some time, being from
a plot in field CI, fertilized with sulphate of ammonia., muriate of
potash, dissolved bone black, and stable manure, since 1891. This is
the plot giving the least satisfactory growth, especially upon lettuce,
beets, spinach and onions. It contained little humus, and was acid to
litmus.
1674.—Soil from the Rhode Island Experiment Station. This
soil has: been used in plot- experiments. Is slightly acid to litmus;
contains humus..
1675.—Sandy soil from the test farm of the North Carolina De-partment
of Agriculture, at Red Springs ; contains little humus.
1676.—Soil from the Rhode Island Experiment Station. This
soil is from a series of plots, which have been in use for some time, to
test the effect of lime on an acid upland soil. Plot 23 fertilized with
ammonium sulphate for some years.
1677.—Same as 1676. Plot 25 fertilized with ammonium sul-phate
and lime.
1678.—'Same as 1676. Plot 27 fertilized with sodium nitrate.
1679.—Same as 1676. Plot 29 fertilized with sodium nitrate and
lime.
1680.—Sandy soil from the test farm of the North Carolina De-partment
of Agriculture at Tarboro.
3
34 TWENTY-FIFTH ANNUAL REPORT. 1902.
NITRATES IN SOIL.
Table I shows the amount of nitrates found at the end of the nitri-fication
period in the soils to which no ammonium sulphate or cotton-seed
meal had been added, i. e., the blanks.
TABLE II.
Mgr. Nitrates per 500 Grams Soil at the End of Three Weeks
Alone. With CaCO,. Alone. ^WithCaCOg-
1667 10.4
2.5
2.2
14.0
8.4 ..
1676
16-7
1678
1679
1680
18.5
14.5
7.3
3.1
1.8
1668
1669
1670 4.5
16.3
1.2
6.5
1674 17.7
1675
5.0
EXTENT OF NITRIFICATION.
Table III contains; the percentage of nitric nitrogen from ammonr
ium sulphate and from cotton-seed meal respectively. It also* gives
the temperature and water content of the soils.
It will be noted that, nitrification was much more active in the first
four soils, in which their temperature was 23 to 30 degrees, C, with
an average of 26 degrees. The nitrification is very much less active
at 19-20 degrees O.
TABLE III.
Nitrification in Soils.
1667 Pasture soil, (N. C.)
Ammonium sulphate
Cottonseed meal
% ammonium sulphate
y2 cottonseed meal
Ammonium sulphate and cottonseed meal
1668 Clay soil (N. C.)
Ammonium sulphate
Cottonseed meal
% ammonium sulphate
1669 Garden soil (Fla.)
Ammonium sulphate
Moisture
Average.
10.5
Temperature.
Extremes.
25-30°
13.0
13.0
25-30°
25-30°
Mean.
Per cent nitrified.
Alone. With
CaCOs
7.2
32.4
27°
57.2
43.6
71.8
43.0
22.3
0.6
10.1
0.2
11.6
-1.1
43.2
15.
NITRIFICATION IN DIFFERENT SOILS.
TABLE III—Continued.
1 Moisture Temperature. Per cent nitrified.
Average. Extremes. Mean. Alone. With
CaCOs.
17.3 41.5
1670 Soil, (Mass.) 15.0 23-28° 26°
Ammonium sulphate 2.2
14.8
0.5
45.7
32.6
Ammonium sulphate and cottonseed meal
1674 Soil, (R. I.) 1 10.7 20-26° 22°
2.1
3.4
2.3
4.9
16.5
10.9
Ammonium sulphate and cottonseed meal 1.3
8.0 19-24° 20°
Ammonium sulphate „ __ .0
.0
.0
Cotton seed meal _ _ .0
1676 Acid soil (R. I.) — — 12.2° 18-23° 19°
Ammonium sulphate . .0
—1.9
1.5
Cottonseed meal _ . —1.3
3^2 ammonium sulphate. . .. 1.5
% cottonseed meal 0.6
1677 Acid soil limed (R. I.)- - 11.7 18-23° 19° .0
1.0
1.8
Ammonium sulphate __ _ _ 5.6
Cottonseed meal _ __ _ _ .____ _. 6.2
1678 Acid soil (R. I.) 12.
1
18-23° 19°
Ammonium sulphate . .0
.0
0.6
Cottonseed meal _ _- . _ _ . .0
1679 Acid soil limed (R. I.) _ . . 12.5 18-23° 19°
1 , Ammonium sulphate _ ._ _ _ 1.2
2.9
3.0
Cottonseed meal ___ ._ _ .
1
10.6
1680 Tarboro soil (N. C.) ... . 9.5
i
19°-24° 20°
Ammonium sulphate. .. .0
1.3
—1.3
Cottonseed meal 1
—0.8
^ ammonium sulphate ...
1
.. J 0.8
Yz cottonseed meal ... _ _ _ 1 4.5
f
36 TWENTY-FIFTH ANNUAL REPORT, 1902
KO REDUCTION OF SULPHATES.
When the previous work on nitrification was reported to the Asso-ciation
of Official Agricultural Chemists, inquiry was made whether
any hydrogen sulphid was detected. In several series of the experi-ments
herei reported tests were made for sulphids in two ways. A
strip of paper moistened with lead acetate was placed over each jar,
and the soil extract was acidified and heated to boiling, a piece of lead
acetate paper being placed in the neck of the flask. In no case was
any hydrogen sulphid found by either method. Insoluble metallic
sulphids would not be detected by this method.
EFFECT OF CAECIUM CARBONATE.
The addition of calcium carbonate to the soil always resulted in an
increase in the percentage of nitrates formed, if nitrification took
place at all. This is true of the nitrogenous compounds already in
the soil, as well as of ammonium sulphate and cotton-seed meal. The
increase is greater with ammonium sulphate than with cotton-seed
meal. The greatest increases in the nitrification of cotton-seed meal
when calcium carbonate is added, are from 100 to 366, 100 to 340,
and 100 to 240. With ammonium sulphate, the increase is 100 to
800, and 100 to 2,100, and in some soils • nitrification takes place
when calcium carbonate is added, and does not take place without it.
Calcium carbonate accelerates nitrification, even when the soil has
been limed, as may be seen by referring to the Rhode Island soils.
With ammonium sulphate the increase is from 100 to 560 and 100 to
250 in the limed soils, and with cotton-seed meal 100 to 366 and 100
to 340.
EFFECT OF LIMING AN ACID SOIL.
Four soils in Table III show the effect of liming acid soils. In the
two acid soils practically no nitrification takes place, while in 'be
limed acid soils some nitrification takes place, though not a great
amount. It is probable that more nitrification would have taken
place had the temperature at which the experiment was conducted
been above 19 degrees.
EFFECT OF THE APPLICATION OF FERTILIZERS.
Soils 1677 and 1679 show the effect of the application of different
fertilizers to the same soil. In 1677, a. limed acid soil, to which other
fertilizing elements and ammonium sulphate had been applied for a
number of years, nitrifies 5.6 per cent of ammonium sulphate, in the
presence of calcium carbonate ; the same soil which received its nitro-gen
in the form of sodium nitrate, nitrified only 3 per cent of am-monium
sulphate under the same conditions.
It is probable thai the continued application of ammonium sulphate
NITRIFICATION IN DIFFERENT SOILS 37
to a soil, will increase its power to nitrify that salt, provided other
conditions are fulfilled, especially if bases are provided.
VARIATIONS IN THE NITRIFYING- POWER OF SOILS.
Aii important result of these experiments is tx> show clearly that
different soils possess different powers of nitrification. In making
comparisons of the soils, we must, remember that some of the nitrifi-cation
tests were conducted at a different temperature from the others,
and the results can not all be compared one soil with another.
The first three soils were nitrified under the same conditions, and
at the same time. Their power to nitrify ammonium sulphate is in
the ratio 7:0.6:0, and cotton-seed meal, 32:0:17. Mixed with cal-cium
carbonate, the ratios become 57 :12 :16 and 44 :0 :42 respectively.
These soils exhibit a great variation in their action towards am-monium
sulphate and cotton-seed meal, and this even under conditions
made favorable by the addition of calcium carbonate. Some of the
soils nitrify ammonium sulphate more; rapidly than cotton-seed meal
;
others nitrify a greater percentage of the nitrogen in cotton-seed, meal
during the same period. We also have a soil which does not nitrify
cotton-seed meal, but nitrifies ammonium sulphate.
Such variations as these are exactly what we expected to find.
EFFECT OF INCREASING THE RATIO OF SOIL TO FERTILIZER.
The main series of experiments, was carried out with a mixture
containing 0.3 gram nitrogen to 500-gram soil. Some other experi-ments
were conducted with half this quantity of nitrogen to the same
amount of soil. The general result of dilution, is to increase the
quantity of nitrates formed ; though this is not always the case. It is
possible for the percentage nitrified tx> be increased under such condi-tions,
though the actual amount of nitrates formed is less. This is
illustrated by soil 1667; the percentage of nitrification in the soil
with full and with half quantities of nitrogen is as 57 :72, but the
actual amount of nitrates formed are as 57:36.
DISCUSSION OF RESULTS.
We will now consider the bearing of these experiments on the ex-planations
previously put forward.
(1) Ammonium sulphate may hinder the action of the nitrifying
organisms.
Additional evidence in favor of this hypothesis is afforded by the
fact that the progress of the nitrification is more rapid when the
quantity of ammonium sulphate is reduced.
The organisms seem to thrive more, vigorously when less ammon-ium
sulphate is present. In two cases a decrease in the quantity of
38 TWENTY-FIFTH ANNUAL REPORT, 1902.
ammonium sulphate had no effect, but very little nitrification took
place in these) soils.
Again, supporting this hypothesis, is the fact that less nitrification
takes place when ammonium sulphate and cotton-seed meal are mixed
than with either separate.
This hypothesis can not explain, however, why ammonium sulphate
is nitrified to a greater extent, than cotton-seed meal in one soil, and to
a less extent in another.
(2) The nitric and sulphuric acids formed are detrimental to the
nitrifying organisms, being; neutralized only in part by the bases of
the soil. It is a well known fact that the organisms which nitrify
ammonium salts' to nitrous acid thrive best in a. medium that is
slightly alkaline. This explanation has been generally accepted for a
long time and requires little discussion.
(3) "The third explanation is, that different soils contain different
nitrifying organisms, some of which convert organic matter directly to
nitrates, while others change ammonium; salts to nitrates more
readily." If this explanation is justified, we may expect to find soils
in which ammonium sulphate is nitrified to a greater extent than
cotton-seed meal, and others in which the cotton-seed meial is nitrified
to a greater extent.. This is exactly what we have found. In soils
1667, 1668, 1670 and 1676 the ammonium sulphate is nitrified more
rapidly than the cotton-seed mieial, in the presence of calcium carbon-ate,
while in soils 1669, 1677 and 1679 the contrary is the case. In
soil 1669, 41.5 per cent of the nitrogen in cotton-seed meal is nitri-fied,
and only 15.8 per cent of that in ammonium, sulphate; in soil
1679 3 per cent for ammonium sulphate, and 10.6 per cent for cotton-seed
meal.
The experiments here recorded seem to justify the preceding ex-planations.
THE NITRIFYING ORGANISMS.
The prevailing view in regard to the conversion of organic nitrogen
to nitrites seems to be that the organic matter must first be converted
to ammonia, then the ammoniai is converted into nitrites, and the
nitrites are next changed, into' nitrates.
If this view is correct, then it is in opposition to 'the explanation we
have put forward, that different soils contain different nitrifying
organisms, some of which convert organic matter1 directly to nitrites,
while others change ammonium salts to nitrites more readily.
The pure nitrous organism is capable of nitrifying organic sub-stances,
according to Warington,1 Frankland and Stutzer. On ob-taining
the organism in a pure state, experiments were at once started
by Warington in solutions containing urea, urine, asparagine and
J Jour. Chem. Soc, 59, 507 (1891]
NITRIFICATION IN DIFFERENT SOILS. 39
milk, with suitable organic salts. Out of the 8 asparagin© solutions
7 showed very distinct nitrification ; of the 8 milk solutions. 5 showed
distinct nitrification ; of the 8 urine solutions 6 showed decided nitrifi-cation,
and of the 8 urea solutions 3 nitrified.
"These experiments should be regarded as preliminary only, as the
course of nitrification has not been studied, or any quantitative experi-ments,
made. That the pure nitrousi organism can attack nitrogenous
organic bodies is, I think, fully proved. The nitrification has, how-ever,
been especially in the case of asparagine and milk solutions, de-cidedly
sluggish. The contaminated milk culture has nitrified to a
greater extent ' han the corresponding pure culture. It is quite possi-ble,
therefore, that other organisms may render considerable service
in the process of nitrification, by making a preliminary attack upon
organic matter."
On the other hand, V. Omelianski l has made a number of experi-ments,
and concludes tha'. pure cultures of nitrifying bacteria are
incapable of nitrifying organic nitrogen. Nitrogen in this form
must first be converted into' ammonia by the action of other micro-organisms
before the nitrifying organisms, can utilize it. It is
claimed that the opposite conclusions reached by Frankland, Waring-ton
and Stutzer and his associates were based upon inaccurate obser-vations.
It is possible that Warington and the others, are wrong, and that the
pure nitrous organism can not nitrify organic nitrogen. It is also
possible that the organism isolated by Warington is different from
the one isolated by Omelianski. At any rate, it is impossible to assert
with certainty that the nitrous organism can not nitrify organic
matter.
It would not be surprising, however, if the nitrous does not nitrify
organic nitrogen. The conditions under which it is separated from
other organisms and a, pure culture prepared are favorable to the
development of an organism, which nitrifies ammonium salts, and any
organism which can not oxidize inorganic nitrogen, and can not grow
in such a solution, is necessarily excluded. The method of Wino-grodski
as used by Omelianski 2 consists in first growing the organism
in a solution of ammonium sulphate, sodium chloride, potassium
phosphate, magnesium, sulphate, and iron sulphate in water, to' which
magnesium carbonate is added, for three or four generations, and
finally in a similar mixture in gelatinous silicic acid. Such a medium
is unfavorable for thie development of the nitrate batcerium (which
oxidizes nitrites to nitrates:) , and if the. organisms developed in it do
not oxidize organic nitrogen to nitrites, it is no evidence that organ-isms
which have that power do> not exist.
i Exp. Sta. Record 12, 115 abs. (1901).
2 Central-Blatt of Agr. Chem., 29, 565 (1900), abs.
40 TWENTY-FIFTH ANNUAL REPORT. 1902.
The nitrifying bacteria of Frankland and of Warington were also
separated by growth in an inorganic medium.
It has been found that the nitrifying organisms will not grow on
gelatine. Of over a hundred species of bacteria separated by culture
on gelatine, not one has been certainly found to possess the power of
nitrifying. Some other medium than gelatine must be used.
It is believed that there are different species of nitrifying bacteria.
In attenuated cultures from soils from different parts of the world
Winogrodski l observed several kinds of microbes, some of which were
isolated, and were found to retain under culture their power of
oxidizing ammonia, but to lose after a few generations the power ol
oxidizing nitrites. It is probable that the nitrous organisms consti-tute
a group, of which each soil contains a particular species.
According to E. Chuard,1 nitrifi cation in turf earth differs essen-tially
from that taking place in arable soils. The- addition of chalk,
potassium carbonate, or calcium sulphate exerts a retarding action on
the nitrifying process. Whether the difference is due to the action of
a different organism, or whether the process of nitrification is differ-ent
from that obtaining in arable soils has not yet been determined.
SUMMARY.
( 1 ) Calcium carbonate exerts a decided accelerating influence upon
the nitrification of cotton-seed meal and ammonium sulphate, espe-cially
the latter.
('2) In some soils a greater percentage of nitrogen is nitrified in
the form of ammonium sulphate than in cotton-seed meal; in other
soils the contrary is the case, even in the presence of calcium car-bonate.
Other soils exhibited little nitrifying power, under the con-ditions
of the experiments.
( 3 ) Three of the factors which produce this result are probably as
follows
(a) The presence of ammonium sulphate may hinder the action of
the nitrifying organisms.
(b) The acids formed may be a hindrance when no base is present
to neutralize them.
(c) Different soils may contain different classes of nitrifying
organisms, some of which oxidize ammonium salts more readily, while
others prefer organic compounds.
(4) We have found no evidence on record tending to show that
organisms do not exist in the soil which nitrify organic compounds
directly. It has been show that gelatine and agar-agar are unsuitable
mediums for the growth of nitrifying bacteria. All nitrous bacteria
heretofore d escribed have been grown in inorganic mediums, which
i Jour. Chem. So. (abs.), (iO, 1545 (1891).
NITRIFICATION IN DIFFERENT SOILS. 41
would be essentially unfaivorablei to organisms which prefer organic
compounds to ainmcmium salts.
(5) Whatever the explanation, the fact that different soils behave
differently toward ammonium sulphate and cotton-seed meal, is of
considerable scientific and practical importance.
This work will be continued.
ACKNOWLEDGMENT.
The authors wish to make acknowledgment to Director H. J.
Wheeler, of Rhode Island; Chemist H. K. Miller, of Florida; Agri-culturist
W. P. Brooks, of Massachusetts, and State Chemist B. W.
Kilgore, of North Carolina., for their kindness in furnishing us with
samples of soil; and to Dr. F. L. Stevens, Professor of Biology, in
this college, for his kindness in reading the manuscript.
%r>
The DetermiQation of Sulphur in Plants/
By G. S. FRAPS, Ph.D., Assistant Chemist.
In a previous paper l the author called attention to the loss of
sulphur in preparing ash of plants. The conclusion reached was that
"the sulphur obtained when the ash was burned by itself is from 4
to 100 per cent less than when burned with calcium acetate. Wheth-er
the calcium acetate retains all the sulphur or not, is a point which
requires further study." The facts which will be presented here
show that the calcium acetate does, not retain all the sulphur.
The object of the work was' to compare the calcium acetate method
with some method by the use of which we could be reasonably certain
that all the sulphur contained in the plant in inorganic or organic com-bination
would be retained and determined. A great difficulty is
that a very small amount of sulphur is contained in a large quantity
of plant material. The Liebig method (fusion with potassium
hydroxide and a small amount of potassium! nitrate in a silver dish)
and ttie Oarius method (heating in a sealed tube with fuming nitric
acid) were considered, but offered difficulties on account of the large
quantity of organic material to be handled. The following method
was finally adopted for trial:
Fifteen grams material were placed in a, flat porcelain dish of
about 2-^0 c. c. capacity, 35 c. c. of nitric acid (cone.) added, and the
mixture heated gently until the action had moderated. One gram
potassium nitrate was then added, and the mixture evaporated to a
thin paste, transferred to a, platinum dish, evaporated on a water-bath,
and ignited to an ash. After heating for1 some time, the ash
was dissolved in dilute hydrochloric acid, the solution evaporated
to dryness, and the residue dried thoroughly to render silicia in-soluble.
It was moistened with a little dilute hydrochloric acid,
evaporated, and again dried. The residue was moistened with about
5 c. c. of hydrochloric acid, taken up with about 50 c. c. of boiling
water, filtered and sulphuric acid determined in the filtrate by the
usual method.
A blank determination with the reagents proved them to be free
from sulphur. The sulnhur (as sulphur trioxide) found by this
method compared with the others is given in the following table :
l Jo. Am. Chm. Soc. 23, 190 (1901).
* This article appeared in the April number of the Journal of the American Chemical
Society [24, 346 (1902) ]
THE DETERMINATION OF SULPHUR IN PLANTS. 43
Sulphur Trioxide in Plant (Air-dry)
In ash
(usual way).
Per cent.
In calcium
acetate ash.
Per cent.
Nitric acid
method.
Per cent.
Wheat bran 0.221 0.368
Cotton-seed meal .___. .___ 0.343 0. 920
Green rape 1 1.02 1.25 1.63
Wheat bran 0.00 0.14 0.30
Corn silage 0.20 0.24 0.43
Timothy bay _ __ _ ... 0.15 0.17 0.28
It is evident, that the calcium acetate method does, not give cor-rect
values, for sulphur.
It is not believed that the loss of sulphur is due to volatilization
of sulphates, but to- the escape of organic sulphur compounds which
are not burned or oxidized. Most of the sulphur in a, plant is not
in the form of sulphates, but is in an organic form, and it is not
surprising that it is lost under1 the conditions. The same would be
true of chlorine, which is probably much more difficult to retain than
sulphur.
The following modification of the nitric acid method just de-scribed
has been found more convenient,. It, calls for the use of a
smaller quantity of material, and leaves out the' platinum dish, which
is liable to be damaged under1 certain conditions.
Five grams material are placed in a 3J inch porcelain evaporat-ing
dish, 20 c. c. of concentrated nitric acid added, and the mixture
heated cautiously on the water-bath until all danger of overflowing
has passed. It, is then partly evaporated, 10 e. c. of a, 5 per cent, solu-tion
of potassium nitrate added, the mixture evaporated to dryness and
ignited, at, first gently, then under a, blast-lamp, until the residue is
white. It is then dissolved in hydrochloric acid, evaporated to dry-ness,
and heated for some time in an air-bath to, render silica insolu-ble.
The residue is taken up in water with the addition of a little
acid, filtered, and the sulphuric acid precipitated with barium chh>
ride, etc., in the usual way. (This method was adopted as a pro-visional
method by the Association of Official Agricultural Chem-ists,
November, 1901).
Since the preceding article was written, it has been found more de-sirable
to use calcium acetate in place of potassium nitrate. With it
the ash does not fuse, and is very much more easily burned free
from carbon.
The Determination of Sulphur and Chlorine
in Plants.
By G. S. FRAPS, Ph.D., Assistant Chemist.
The preceding article contains an account of the work on the de-termination
of sulphur which was done up to last November. The
study of the methods of determining sulphur has since been con-tinued,
and results of the study are given in this article. The de-termination
of chlorine in plants was also undertaken, with the re-sults
to be: described later on in this paper.
METHODS FOR SULPHUR STUDIED.
The following methods for the determination of the total sulphur
in plants were tested
(1) Nitric Acid Method.—Five grams material is placed in a 3 1-2
inch porcelain evaporating dish, 20 cc. of nitric acid (cone.) added,
and the mixture heated cautiously on the water-bath until all danger
of overflowing has passed. It is then evaporated partly, 10 cc, of a
5 per cent solution of potassium nitrate added, the mixture evaporated
to complete dryness, and ignited, at first gently, then under a blast
lamp until the residue is white. It is then dissolved in hydrochloric
acid, evaporated to dryness, and heated for some time* in an air-bath
to render silica insoluble. The residue is taken up in water with the
addition of a little acid, filtered, and the sulphuric acid precipitated
with barium chloride in the usual way.
As has been stated in the preceding article, this method gives good
results. It has a, disadvantage, however, in that the ash produced is
easily fusible, acts upon the porcelain dish, and is ignited free: of
carbon with great difficulty. It was to> overcome this objection that
the modification described below was tested.
(2) Nitric Acid Method Modified.—The modification consists in
the use of a solution of calcium acetate containing 0.56 gin. OaO., in
place of the 20 cc. of potassium nitrate solution. The ignition takes
place much more easily, the ash does not fuse, and is more easily
burned free of carbon than when potassium! nitrate is used.
(3) Boiling with Nitric Acid.—An attempt was made to destroy
the organic matter by boiling the material with nitric acid, which, I
understand, is the method used for meats in the nutrition investiga-tions
of the Office of Experiment Stations. The method did not suc-ceed
with vegetable materials. Several experiments were made, but
in no case was all organic matter of the vegetable materials destroyed,
DETERMINATION OF SULPHUR AND CHLORINE IN PLANTS. 45
even when 5 grams material was boiled to dryness with 100 cc. nitric
acid, in a kjeldahl flask. As it would, therefore, be necessary to wash
the residue from the flask into a dish, and ignite with the addition of
potassium nitrate or calcium acetate!, to' remove organic matter, this
method would differ from the two preceding only in that a larger
quantity of acid is used, and the digestion with the acid is more pro-longed.
The method was not further examined.
(4) Fusion with Caustic Soda.—This is the standard method for
determining sulphur in non-volatile organic compounds. The method
as tested was as follows
Five grams material in a nickel crucible was saturated with 40 cc.
of a solution of 150 grams sodium hydroxide in 800 cc. water, evapo-rated
to> dryness, and fused with the addition of a, little sodium perox-ide.
The fusion requires care to prevent the material from overflow-ing
the dish, and the whole process is somewhat long. The melt was
dissolved in water, neutralized and acidified with hydrochloric acid,
evaporated to dryness and heated to render silica, insoluble, filtered,
and the sulphuric acid precipitated from the filtrate, the volume of
which was about 200 cc. The sodium hydroxide and sodium perox-ide
contained a large quantity of sulphates—about 0.1 gram in the
quantity used in the determination was found in the blank determina-tion.
The results with this method are decidedly low. The low re-sults
may possibly be due' to the solubility of barium sulphate in
sodium chloride, about 38 grams of the latter salt being present in the
solution from which the barium sulphate was precipitated, or it may
be due to the error caused by impurities in the reagents.
(5) Esclika's Method.—This is the method usually used for the
determination of sulphur in coals. As applied to plant materials it
was as follows:
Five grams material was intimately mixed, in a platinum dish,
with 7
1/2 grains of a mixture of 2 parts magnesium oxide to one of
dried sodium carbonate. The mixture was heated, stirring fre-quently,
and the temperature raised slowly until all carbon appeared
to be burned off. The mass was transferred to a beaker with about
50 cc. water, 150 cc. of saturated bromine water added, and boiled
five minutes. It was allowed to settle, decanted through a filter,
boiled a second and a third time with about 30 cc. water, and washed
thoroughly. The filtrate was made acid with hydrochloric acid,
boiled until bromine was expelled, and then precipitated with barium
chloride in the usual way.
The results by Eschka's method were too low.
RESULTS OF WORK.
The analytical results by the different methods are given in the
following table (Table 1). The figures in each case are corrected
46 TWENTY-FIFTH ANNUAL REPORT, 1902.
for the sulphur in the reagents, found by a blank determination. The
blank was very low in the case of the two nitric acid methods ; in the
Eschka method it was equivalent to 0.0058 gram barium sulphate
in the quantity of the reagents used for each test. As has already
been stated, the fusion method gave results much too low, and the
blank was high, being 0.1103 gram barium sulphate.
TABLE I.
Percentage of Total Sulphur (as S03 ) by Different Methods
Nitric Acid
Method.
Nitric Acid
Modified.
Eschka
Method.
Corn _._. ___. _ ... 0.249 0.287 0.238
0.244 0.286 0.208
Mean 0.247
0.481
0. 287
0.480
0. 223
Peas 0.297
0.533 0.312
0.503 0.313
Mean . __..-. . . _ _ 0.518
0.369
0.480
0.427
0.307
Millet 0.451
0.376 0.434 0.460
0.400
Mean 0.382 0.431 0.456
The results of this study may be summarized as follows:
(1) The nitric acid method, modified by the use of calcium acetate
in place of potassium nitrate, is decided to be the best method.
(2) Eschka's method gave low results.
(3) Fusion, with caustic soda as here described, gives low results.
It is a very tedious operation.
DETERMINATION OF CHLORINE.
The writer has already called attention to the fact that chlorine,
as well as sulphur, will be lost in burning plant substance to an ash
by itself. It will appear later that the loss is due to decomposition
of the chlorides by the heated organic matter.
LOSS OF CHLORINE.
Chlorine was determined in a number of substances in two ways,
namely, in the ash as prepared in the usual way, and by fusion of the
plant material with sodium hydroxide, a method which will be
described in full later on in this paper.
The results of the determination are as follows (Table 2) :
DETERMINATION OF SULPHUR AND CHLORINE IN PLANTS. 47
TABLE II.
Percentage of Chlorine in Plants.
Com
Peas
Peas, No. 2
Oats
Oats, No. 2
Peanuts
Cotton seed meal-..
Cotton seed hulls. ..
Linseed meal
Millet
Corn silage, dry
Green rape, dry
Green peas, dry
Sweet potatoes, dry
Timothy hay
Ash
Method.
NaOH
Method.
trace 0.040
0.005 0.008
0.001 0.012
0.005 0.097
0.001 0.056
0.008 0.017
0.008 0.032
0.005 0.013
0.010 0.029
0.120 0.187
0.310 0.607
1.261 1.290
0.160 0.205
0.341 0.362
0.864 0.888
It is evident that a considerable proportion, of the chlorine in
plants may be lost in burning them! to an ash, particularly when there
is only a small quantity of chlorine present in the plant.
The cause of the loss is shown by the work of Davies, reported in
the Journal of the Society of Chemical Industry, 20, 98. (1901).
He experienced similar losses when sugar, starch or filter paper1 was
ignited with sodium chloride. The alkalinity of the ash was evidence
that no base had been lost, and if the sodium chloride was added after
the sugar had been charred, and the ignition then completed, no loss
took place. That is to say, the loss took place during the initial
stages of the combustion, and not during the time the carbon was
being burned off, and was probably due to the decomposition of the
chlorides by the hot vapors from the organic matter1
. Extracting the
material with hot water after charring, and then completing the
combustion, can therefore have no effect on the lossi of chlorine, since
it takes place before the extraction. When sodium carbonate equiva-lent
to five per cent of the organic matter was added to the material,
the loss of chlorine was prevented.
DETERMINATION OF CHLORINE IN PLANTS.
Three methods for the determination of chlorine in plants were
tested.
48 TWENTY-FIFTH ANNUAL REPORT, 1902.
(1) Ignition of the Material ivith Calcium Acetate.—Five grams
substance was moistened with 20 cc. of a solution of calcium acetate
containing 0.56 gram calcium oxide, evaporated to dryness, and
ignited. The ash was dissolved in nitric acid, filtered and chlorine
determined in the filtrate by the Volhard method. On account of
the very small quantity of chlorine present in many of the sub-stances,
a gravimetric method could not be used as the precipitate
would not coagulate. The results by this method are low (Table
ni).
(2) Fusion with Sodium Hydroxide.—Five grams substance was
mixed thoroughly with 10 cc. of a solution of grams caustic soda
in 200 cc. water, evaporated to dryness, and finally fused. A nickel
crucible was used for a portion of the work, silver crucibles for the
remainder, due care being taken to prevent the silver from being
detached from the crucible. It is better to use nickel crucibles, as
there is always a little danger of small particle® of silver being de-tached.
The melt was dissolved in water, neutralized with nitric
acid, filtered, and chlorine determined in the filtrate by the Volhard
method.
The method yields satisfactory results, but it is long, and the cruci-bles
wear out rapidly. (Results in Table III).
(3) Ignition with Sodium* Carbonate.—Five grams substance in a
platinum dish is impregnated with 20 c. c. of a 5 per cent solution of
sodium carbonate, evaporated to dryness, and ignited as thoroughly
as possible. The residue is extracted with hot water, filtered and
washed. It is returned to the platinum dish, ignited to an ash, dis-solved
in nitric acid, and filtered into the previous filtrate. This is
made acid with nitric acid, and the chlorine determined by the
Volhard method.
In one or two cases, the filtrate from the first extraction was yellow
from organic matter. It was returned to> the dish with the charred
residue, evaporated to dryness, and ignited. The residue burned
very readily to> a, white1 ash.
This method is recommended.
RESULTS OF WORK.
The results by the three methods are contained in Table III:
DETERMINATION OF SULPHUR AND CHLORINE IN PLANTS. 49
TABLE III.
PERCENTAGE OF CHLORINE IN Pj.ANTS
Calcium Ace-tate
Method.
Caustic Soda
Method.
Sodium Carb.
Method
0.0021 0.040
0.040
0. 027
0. 026
Millet .. .... - - - - 0. 148 0. 165
0.171
0.188
0. 194
0.201
0. 206
0. 187 0. 191
Corn silage 0. 400 0.616 0. 610
0.081
0. 599
0.032 0.020
0.010 0.013 0.017
0.215 0.197 0. 228
0.212 0. 230
Oats 0. 034 0.056
Timothy hay 0.870 0.914 0. 897
0.878 0.911
0.872
0.888 0. 905
The sodium carbonate method gives as accurate results as the
method of fusion with caustic soda, and as it is shorter and easier,
it is to be recommended for use.
SUMMARY OF RESULTS.
(1) The nitric acid method, modified by the use of calcium
acetate in place of potassium nitrate, is to be recommended for the
determination of total sulphur in plants.
(2) Eschka's method, and the method of fusion with caustic soda
and sodium peroxide as described in this paper, gives* low1 results.
Boiling with nitric acid in a kjeldahl flask is not to be recommended.
(3) Loss of chlorine takes place in the ignition of plant materials
to> ash, probably due to decomposition of chlorides, and not to their
volitilizatdon.
(4) The method of igniting the material with sodium carbonate
is recommended for the determination of chlorine in plants. (This
method was adopted as a provisional method by the Association of
Official Agricultural Chemists, October, 1902).
Since this paper was written, Dr. H. 0. Shermon has published
results which show that the nitric acid method, described in the
above paper, gives low results.
4
The Solubility of Barium Sulphate in Ferric
Chloride, Aluminium Chloride, and
Magnesium Chloride/"
By G. S. FRAPS, Ph.D., Assistant Chemist.
In working on the determination of sulphuric acid in soils, Mr.
0. B. Williams, Assistant Chemist to the North Carolina Depart-ment
of Agriculture!, found that considerably more barium sulphate
was obtained when the iron and aluminium had been previously pre-cipitated
from the soil solution. 1 This led to the following work.
The latest determinations of the solubility of barium sulphate
which have been made are those of R, Fresenitis and E. Hintz,2 in
which the solubility was determined in pure water, 2.5 and 10 per
cent ammonium chloride, 2.5 per cent sodium chloride, 10 per cent
nitric acid, and 10 per cent hydrochloric acid, alone, and in the
presence of an excess of sulphuric acid or barium chloride.
In regard to the effect of ferric salts, aluminium salts, and mag-nesium
salts upon its solubility, we have few data, Fresenius states
that its solubility in water is increased by the presence of magnesium
chloride, and Lunge 3 states that it is soluble in ferric chloride. As
the precipation of barium sulphate sometimes takes place in the pres-ence
of these salts, the knowledge of its solubility is important in
analytical work.
METHOD OF WORK.
The method used was similar to that adopted by R. Fresenius, 4
barium chloride being used in place of barium hydroxide.
A solution of barium chloride was prepared, 100 cc. of which
was found to give 0.0952 and 0.0945 gram barium sulphate, i. e.,
1 cc. = 0. 95 milligram BaSO 4 A solution of sulphuric acid was
prepared, 100 cc. of which gave 0.1206 and 0.1204 gram barium
sulphate, or 1 cc. = 1.2 milligrams barium sulphate.
Preliminary tests were then made upon solutions of ferric chlo-ride,
aluminium chloride, and magnesium chloride. Four hundred
cc of the solutions were placed in precipitating jars and sulphuric
acid and barium chloride solution were added in the proper propor-tions
to make 10 milligrams barium sulphate. The solution was
allowed to stand twenty-four hours, and if no precipitate appeared
i His results are not yet published.
-' Ztschr. anal. Chem., 35, 170 (1896).
e Ibid., 19,431.
• Loc. cit.
* This article appeared also in the American Chemical Journal [27, 288 (1902)].
SOLUBILITY OF BARIUM SULPHATE. 51
10 milligrams more of barium sulphate were added, and so oil until
a precipitate appeared.
More exact tests were then made, based upon the results of the
preliminary tests. In making: these tests, the solution was allowed
to stand forty-eight hours instead of twenty-four, as it was found
that precipitates sometimes appeared during the second twenty-four
hours. Much smaller quantities of barium sulphate were added
each time, and the very faintest trace of appearance of barium sul-phate
was watched for. It was found that if the stirring-rod was
rubbed against the sides of the vessel the barium sulphate separated
out at this point more rapidly and more readily than elsewhere, and
could be easily seen. In making up the solutions of the various salts,
allowance was made for the quantity of water which would probably
be added with the barium, chloride and sulphuric acid.
RESULTS OF WORK.
The solubility of nascent barium sulphate in the solution of
chlorides of different concentrations is given in the following table.
Xeither barium chloride nor sulphuric acid was present in excess in
any case.
Solubility of Barium Sulphate.
Amount of
salt per
Milligrams BaS0 4 dissolved per liter.
liter.
Grams. FeCl 3 . A1C1 3 . MgCl 2 .
1
.2y2
5
10
25
.50
100
58
72
115
123
150
160
170
33
43
00
94
116
170
175
30
30
33
33
50
50
50
i
Comparing these figures with the results of Fresenius with other
salts, wei find that barium sulphate is much less soluble in 10 per cent
ferric chloride, or aluminiuin chloride, than in 10 per cent nitric
acid, or hydrochloric acid. It is also more readily soluble in a 10
per cent solution of ammonium chloride than in ferric chloride or
aluminium chloride, of the same strength, though less soluble in 2.5
per cent ammonium chloride.
52 TWENTY-FIFTH ANNUAL REPORT, 1902.
SOLUBILITY IN PRESENCE OF BARIUM CHLORIDE.
Tiie solubility of barium sulphate in ferric chloride and alumi-nium
chloride in the presence of barium chloride in excess was tested
in the same way as before. The results are as follows. In each
case 12.5 milligrams barium sulphate per liter were present (5 mil-ligrams
in 400 c. c.) :
With 5 grams aluminium chloride and 7.5 c. c. of barium chloride
(1 : 10) per liter present, the solution became) turbid in an hour.
With 10 grams aluminium chloride and 20 c. c. barium chloride
the solution became turbid in an hour.
With 25 grams aluminium chloride and 12.5 c. c. barium chloride
a very faint precipitate appeared in forty-eight hours.
With 5 grams ferric chloride, 7.5 c. c, bariuin chloride, a slight
precipitate appeared, in twenty-four hours.
With 10 grains ferric chloride, 20 c. c. bariuin chloride, a slight
precipitate appeared in twenty-four hours.
With 25 grams ferric chloride and 12.5 c, c. bariuin chloride, a
very faint precipitate appeared in forty-eight hours.
Comparing these results with those of Fresenius, we find that, in
the presence of bariuin chloride, bariuin sulphate is less soluble in
ferric chloride, or aluminium chloride, than in a 10 per cent, or 2.5
per cent, solution of ammonium, chloridei, or in a 2.5 per cent solution
of sodium chloride, or nitric acid, or hydrochloric acid.
It must be remembered that all these tests were made at the
temperature of the laboratory. The results might have been some-what
different had the work been carried on at the temperature usual-ly
used for the precipitation of barium sulphate.
The Sulphur Content of Some Vegetable
Materials.
By W. A. WITHERS. A. M., Chemist, and G. S. FRAPS, Ph. D., Assistant Chemist.
It has been assumed by most writers and workers in agricultural
chemistry, that the ash of a, plant contains all the sulphur and chlorine
of the plant, and numerous calculations have been based upon this
assumption, in spite of the fact that from time to time work has been
published tending to show1 that this assumption is erroneous. Recent
articles by one of us1 prove that the sulphur content of an ash is
no indication whatsoever of the amount of sulphur in a plant. This
point needs to be emphasized until it is clearly recognized and gener-ally
accepted. Determinations of sulphur (and of chlorine) in ashes,
so far as they are considered to throw any light upon the composition
of the plant, have no value at all, and may as well be discarded. Un-known
quantities of sulphur and chlorine have been volatilized, and
what, is left, behind bears no relation to what was in the plant.
Inasmuch as the sulphur1 content of plants has been generally
under-estimated, it becomes a matter of somei importance to ascertain
the amount which is. really present. This, is the object of the present
paper; we will communicate, the results of the determination of the
true sulphur content, of certain vegetable materials..
The method used for determinating total sulphur is that described
in a recent article 2 by one of us, using equal parts of calcium acetate
and potassium nitrate, however, instead of potassium nitrate alone.
The ash is: more easily burned completely in this case.
COTTON-SEED MEAL.
Ten samples of cotton-seed meal, from different sources, were an-alyzed.
One sample was from Sea Island seed, and contained a
large quantity of hulls. It is excluded from the average.
The results for the nine samples are as. follows: (For individual
analyses see tables at end of this article).
S (as SO 3 ) in Meal.
Average 1.10
Maximum 1.30
Minimum 0.92
Sea Island 0.63
1 See preceding articles in this Report.
Jour. Am. Ch. Soc, 123, 19 (1901) ; 24, 346 (1902).
*This Report, and Jour. Am. Ch. Soc, 24, 346 (1902).
54 TWENTY-FIFTH ANNUAL REPORT, 1902.
The fertilizing constituents of cotton-seed meal, as calculated from
204 analyses of the ash, arei as follows
l
Phosphoric
Acid. Potash. Soda. Lime. Magnesia. Sulphuric
Acid.
Average
Maximum _
2.88
4.62
1.26
1.77
3.32
0.87
0.29 •
0.73
0.03
0.43
1.25
0.27
0.95
1.26
0.48
0.19
0.40
Minimum 0.07
According to the above table, the meal contains less sulphur (as
S03 ) than phosphoric acid, potash, soda, lime or magnesia. But
the ash retains, on an average, only onehsixth of the sulphur, and
there is then really present in cotton-seed meal more sulphur than
either soda, lime, or magnesia, and the sulphur content is not far be-hind
the potash content.
OTHER COTTON SEED PRODUCTS.
Six samples of the hulls were analyzed, with the following re-sults:
(See tables at end).
S (asS0 3 ) in hulls.
Average 0.176 per cent.
Maximum 0.292 per cent
Minimum 0.089 percent.
The results of eight ash analyses' give the following constituents
of the hulls
Phosphoric
Acid. Potash. Soda. Lime. Magnesia. Sulphuric
Acid.
0.25
0. 56
0.09
1.02
1.32
0.36
0.02
0.02
0.01
0.18
1.09
0.13
0.26
0.35
0.16
o.os
Maximum 0.09
Minimum 0. OS
In this case the ash retains nearly one-half of the sulphur. The
sulphur content is not very far behind the phosphoric acid.
Two samples of cotton-seed kernels contained 0.755 and 0.720 per
(•(Mil of sulphur (as SO,), respectively.
Three samples of lint cotton contained (average) 0.135 per cent;
maximum 0.155 and minimum: 0.107 per cent. Calculated from
the ash of one sample (containing 0.144 per cent), the percentage of
sulphur as SO., was 0.043, or not quite one-third the true value.
The Cotton Plant, U.S. Department of Agriculture (1896)
SULPHUR CONTENT OF SOME VEGETABLE MATERIALS. 55
OATS.
Determinations of total sulphur, and sulphur in the ash, were made
in six samples, with the following results: (See tables at end).
SO 3 . Total. In Ash.
Average __ _ . _. _ . _ 0.491
0.5L4
0.447
0.050
Maximum
Minimum
0.069
0.014
The ash contains a little over one;-tenth of the total sulphur. The
average ash analysis of oatsi, according to Wolff, is as follows:
Phosphoric Acid 0.55 percent.
Potash 0.42 per cent.
Soda 0.10 per cent.
Lime , 0. 10 per cent.
Magnesia 0.18 per cent.
Sulphuric Acid 0.04 percent.
We find, however, that more sulphur, instead of less, is present
than potash, soda, lime or magnesia.
COWPEAS.
Thirteen samples (mostly different varieties) were analyzed with
the following results: (See tables at end of this article).
S0 3 . In Plant.
Calculated from
S0 3 in Ash.
0.466
0. 531
0.419
0.076
0. 139
Minimum.. .. . . 0.034
The ash contains not quite one-sixth of the total sulphur.
CORN.
Eight samples of corn were examined. The ash of corn (which
was tested for sulphuric acid in each; case) contains only a very small
amount of sulphuric acid, less than a milligramme of barium sul-phate
being found. A niiligramme of barium sulphate corresponds
to 0.0068 per cent S03
in the plant,
The sulphur content of the corn (grain) was: (See also> tables
at end of this article).
50 TWENTY-FIFTH ANNUAL REPORT, 1902.
Average __.
Maximum
Minimum _
0.338 percent.
0. 389 per cent.
0.302 percent.
The ash contains less than a fiftieth of the total sulphur.
According to Wolff, the composition of corn is
Phosphoric Acid 0.55 percent.
Potash 0.33 percent.
Soda 0.02 percent,
Lime 0.03 percent.
Magnesia 0.18 per cent,
Sulphur (as SO*) 0.01 percent.
The sulphur in corn is, however, greater in quantity, instead of
less, than potash, soda, lime, or magnesia.
TOBACCO.
Four samples of tobacco were analyzed, with the following re-sults
:
so a .
Average __.
Maximum.
Minimum.
In Plant.
0. 502
0. 650
0.288
alculated from
SO* in Ash.
0. 425
0. 587
0.240
The ash contains 85 per cent of the total sulphur
PEANUTS.
Three samples of peanuts, hulls and all, gave the following results
so 3 . Ii Plant, In A 3h.
Average
Maximum _ . __
0.471
0.508
0.433
0. 13!)
0.180
Minimum - _.-- . _ . _ _ __ . 0.117
The ash contains less than a third of the total sulphur.
A sample of sweet potatoes (dry) contained 0.159 per cent sulphur
as SO, ; the percentage calculated from that in the ash was 0.107.
A sample of onions contained 0.264 per cent, and calculated from the
ash content, the percentage is 0.115.
SULPHUR CONTENT OF SOME VEGETABLE MATERIALS 57
SUMMARY AND CONCLUSIONS.
( 1 ) As an average of a number of analyses, we find that the ash of
plants contain only a portion of the total sulphur, as follows
Cotton-seed MeaL.
Cotton-seed Hulls.
Oats
1-6.
1-5.
1-10.
Cowpeas 1-6.
Corn 1-50.
Peanuts 1-3.
Tobacco 4-5
(2) Plants contain much more sulphur than has hitherto been
considered to be the case. Corn and oats contain- more sulphur than
potash, soda, lime or magnesia. It. is probable that sulphur plays
a more important part in plant nutrition than has been suspected.
(3) The sulphur content of an ash is no indication as to the amount
of sulphur in the plant. Conclusions reached in regard to the sul-phur
content of a plant by ash analyses are entirely valueless.
TABLES OF
Sulphur
ANALYSES.
AS (SO s ).
No. SO3
Per cent. 1 No.
i
SO 3
Per cent.
1646 Cottonseed Meal
Cottonseed Meal
Cottonseed Meal
0.95
1.16
1.22
l.BO
1.08
1.10
1.06
1.10
0.92
1693
1694
1696
1697
1698
1699
1700
1716
1717
1717
0. 172
1681 0.197
1682 Cottonseed Hulls
Cottonseed Hulls _ _
0. 089
1683 Cottonseed Meal 0. 292
Cottonseed Meal
Cottonseed Meal .
1684 Maximum
1685
0. 292
0.089
1686 Cottonseed Meal._. _ Average
Cottonseed Kernels
0.176
1688 Cottonseed Meal 0.755
1689 Cottonseed Meal__ _. _ . 0. 720
Maximum
.
Lint Cotton
Lint Cotton _ .
1.30
0.92
1.10
0. 155
Minimum _ _ _ _. __ _ _ 0.107
Average _ _ . 0.144
Sea Island Meal
Cottonseed Hulls
0.63 Lint Cotton in Ash __ -_ 0.043
1691 0.154 Average
0.152
0. 135
1692 Cottonseed Hulls
58 TWENTY-FIFTH ANNUAL REPORT, 1902.
Sulphur as (S0 3 ).
No. Total
so :1 .
In Ash.
1709 Oats 0.447
0. 503
0.051
1715 Oats 0. 069
1733 Oats 0.510
0.514
0.481
0.053
0.062
0.052
1734 Oats __. - -
1735 Oats
1736 Oats 0.494
0.514
0. 014
Maximum. . . 0.69
Minimum. . 0.447 0.14
0.491 0.50
1710 Cow Peas 0. 481 0. 082
1712 Cow Peas 0. 439 0.095
1713 Cow Peas 0. 487 0.139
1718 Peas var. Greasy __ 0. 427 0. 049
1719 Peas Red Ripper__„ 0.462 0.054
1720
1721
1722
Peas Black Eye
White
Peas White Yellow
Eye
Peas Red CrowdtT-
0.477
0. 487
0. 485
0. 065
0.077
0.038
1723 Peas Lady 0.459 0. 036
1724 Peas Black Prolific 0. 448 0. 079
1725 Peas Unknown 0. 452 0.112
1726 Peas Large Black __ 0.419 0. 087
1727 Peas Southdown . 0.531 0. 079
Maximum
, Minimum
! Average
0.531 0. 139
0.419 0. 034
0. 466 0.76
No.
1711
1712
1729
1730
1731
1732
1737
1738
1705
1706
1707
1708
1728
1739
1740
1741
1742
Total
so 3 .
In Ash.
Corn
Corn . .__
0.302
0. 335
0.301
0.348
0.343
0.332
0. 356
0.389
Trace.
Corn
Corn
Corn . .
Corn _
Corn .. _
Corn __ _. .
Maximum _ 0.389
v 0.301
0.338
Minimum
Average
Tobacco
Tobacco
Tobacco
Tobacco
0.642
0.288
0.650
0. 430
0. 496
0.240
0. 587
0.377
Average 0.502 0.425
Sweet Potatoes
Onions
Peanuts
0.159
264
0.433
0. 472
0.508
0.471
0.107
0.115
0.117
0.180
0.120
Average 0. 139
The Determination of Pentosan-pree Crude
Fiber.
By G. S. FRAPS, Ph.D., Assistant Chemist.
Until a few years ago, the only demand made upon the method of
determining crude fiber, which is an entirely arbitrary method, was
that the crude fiber should not contain appreciable amounts of nitro-genous
compounds. A method was chosen which would give the
minimum of nitrogen-content of the fiber, always considering, of
course, its convenience, accuracy and adaptability to give concordant
results in the hands of different analysts.
In the last few years a determination has been introduced into our
scheme of analysis for1 foods which brings us to the necessity of mak-ing
further demands upon our crude fiber determination. The intro-duction
of the pentosan determination compels us to require of the
crude fiber, that it should not contain appreciable quantities of
pentosans, or else we will be obliged to make two pentosan determina-tions,
one of total pentosans, and one of pentosans in the crude fiber.
Applying this requirement: to> the official method for the determina-tion
of crude fiber, we find it lacking; the crude fiber obtained con-tains
pentosans, often in considerable quantity. The following fig-ures
are quoted from a great many available:
TABLE I.
Pentosans in 100 Parts Crude Fiber.
Bulletin 172, N. C. Station (1900):
Timothy hay,No.II 14.4
Crabgrass hay,No.II 13.4
Green rape, No. I 7.7
Rice bran 8.3
J. Konig, Analyst 88, 47 (1898):
Rye straw 18.4
Pea straw 15.0
Clover hay _ 12.7
Wheat bran 2.8
We have, then, two alternatives ; to adhere to this method, and de-termine
pentosans in the crude fiber when necessary, or to seek for a
new method, by which a pentosan-free crude fiber is produced.
KONIG' S METHOD.
In a paper read before the Association of Official Agricultural
Chemists, last year, the writer directed attention to the method of J.
Konig for determining pentosan-free crude fiber. This consists sim-
60 TWENTY-FIFTH ANNUAL REPORT. 1902.
ply in heating or boiling the substance with glycerol containing sul-phuric
acid, and determining the weight of the residue.
For description, see Analyst 23, 47, or Exp. Station Record 9,
1021.
Kellner, Herring and Zafm (Exp. Station Record 11, 705) tested
this method and decided that it was an improvement over the method
at present in use.
C. Beck (Exp. Station Record 12, 611) did not come to such a
favorable conclusion. He found the method to give somewhat vary-ing
results, but concluded that, it may be particularly useful for
fodders, but for finely ground grain feeds the other method is most
reliable. He found it difficult to keep the temperature between
131-133 degrees.
Konig replies to Beck that it is easy to keep the temperature right
if glycerol of exactly 1.229 sp. gr. is used, and if the flame is made so'
small that the liquid just boils, and only a few drops condense.
DESCRIPTION OF METHOD.
During the past summer, the writer has made some study of
Konig's method, and the following is a full description of the method
finally adopted
DETERMINATION OF CRUDE FIBER.
(a) Glycerol-Sulpliuric Acid.—Determine the specific gravity of
the glycerol by means of a specific gravity balance, or pincnometer,
and calculate the per cent of glycerol it contains by the following
table: (A hydrometer will not give correct results for the specific
gravity of glycerol.)
TABLE H.
Sp.gr. at 15.5°. Per cent.
1.2674 100
1.2647 99
1.2620 98
1.2594 97
1.2-567 96
1.2540 95
1.2518 94
1.2486 93
Sp.gr. at 15.5°.
1.2460
1.2433
Per cent.
92
91
1 2406 91
1.2380 89
1.2353 88
1.2327 87
1.2300 86
Should the temperature not. be 15.5 degrees, a correction may be
made by adding 0.00058 for each degree above 15.5 degree.
Dilute the glycerol to exactly 1.229 sp. gr., and make up a solution
20 grams concentrated sulphuric acid (1.84) in a liter of glycerol.
(b) The Determination.—Place 3 grams substance in a 500 cc.
Erlenmeyer flask, add 200 cc. of glycerol, and connect the flask with
an inverted condenser, the tube of which passes only a short distance
beyond the rubber stopper into the flask. Heat to boiling, and boil
very gently for an hour, shaking the flask from time to time to wash
down the particles which adhere to the sides of the flask. The boil-
THE DETERMINATION OF PENTOSAN. 61
ing' should take place in such a manner that only a few drops of water
are formed in the condenser. Prepare a, thin layer of asbestos in a
two-inch Hirsch funnel, and on this place a perforated platinum disk.
Filter the glycerol through this, using a suction pump, wash with hot
water, them with alcohol, and with a mixture of equal volumes of
alcohol and ether. The alcohol is necessary, not only to remove fats,
but to remove certain products not soluble in water, formed by the
action of the glycerol-acid upon the feeding stuff. Transfer to a
platinum dish, dry, weigh, incinerate completely. The loss in weight
is crude fiber.
PRECAUTIONS.
A primary necessity is to have the glycerol of the required density.
A comparatively slight variation in density causes an increase or de-crease
in its boiling point, with corresponding decrease or increase in
the quantity of crude fiber left.
On account of the nature of the glycerol, it is necessary to filter it
as hot as possible and before it cools. Cold glycerol, even if diluted
with water, filters with very great slowness. The method of filtra-tion
recommended is that found best after making trials of several
other ways. These were
(1) Dilution with water and nitration while hot, as recommended
by Konig. Very often this filtration requires a long time, and always
longer than the method recommended.
(2) Dilution with alcohol. Filtration takes place rapidly, and
this method may be used in difficult cases.
No difficulty will be had with the method described after a little
practice. The author has weighed out a set of samples, digested,
filtered, and washed the crude fiber, in three hours.
SESULTS.
The results: obtained are satisfactory. It is much easier to' obtain
concordant: results by this method than by the official method. The
following are determinations made:
TABLE III.
Crude Fiber by Konig's Method.
Timothy hay 27.40 per cent.
do 27.65 per cent.
do 27.32 per cent.
Corn bran 10.09 percent.
do 9. 80 per cent.
do 10.19 percent.
do 10.41 per cent.
Timothy hay, No. 2 31.95 per cent.
do 31.60 percent.
do 32.04 per cenl.
Sheep dung 34.33 per cent.
do 33.74 per cent.
The work of Konig and others has shown that the crude fiber so
obtained is practically free from1 pentosans.
It must be observed that, the method does not, seem applicable to
62 TWENTY-FIFTH ANNUAL REPORT. 1902
cotton-seed meal. Two or three times as much apparent crude fiber
is obtained as there should he.
Some determinations were made with this method by Mr. W. F.
Pate, a graduate student. The glycerol he used was a little more
concentrated, and he boiled the mixture more vigorously. The re-sults
obtained by him were 3.5 to 4.9 per cent lower.
Although these results do not appear favorable to the method, it is
believed that a comparison of it with the official method will show
that the one method gives, in the hands of different, analysts, as con-cordant
results as the other. This will be more particularly true
when chemists have become to' some extent familiar with the new
method.
CONCLUSION.
The Konig method has the following advantages
(1) It yields a fiber practically free from pentosans.
(2) It requires fewer manipulations and less time than the usual
method.
This paper was read before the Association of Official Agricultural
Chemists in November, 1901, and the Association adopted the recom-mendation
that the Referee on Feeding Stuffs should undertake a
studv of the method.
CABBAGE SNAKES. 63
NORTH CAROLINA AGRICULTURAL EXPERIMENT STATION.
B. W. KILGORE, Director.
PRESS BULLETIN, No. 2.
CABBAGE SNAKES.
East year considerable was said in the press of the State in regard
to cabbage snakes, especially in the cabbage sections of the western
part of the State. Recently an item has been going the round of the
newspapers concerning a supposed poisonous "cabbage snake" found
iu a head of this popular vegetable by a lady in Swain County, North
Carolina. The alleged snake was sent to the North Carolina De-partment
of Agriculture for identification, and proved to be the
common and inoffensive "Hair Snake," or water worm
—
gordius
variabilis.
This is not a snake but a nematode worm which during some
part of its life is an intestinal parasite of the cabbage caterpillar,
grasshopper and some other insects. It is often found in samples of
water from shallow wells, horse-troughs and ponds. Its presence in
water indicates that the water is not fit to drink, but the worm itself
is not poisonous nor in any way dangerous to human beings. The
popular name "Hair Snake" is given to this worm on account of its
great slenderness, which has given rise to the fanciful idea that a
horse hair has been transformed into a worm or "snake." Though
this worm is often a foot in length it is never as thick as a knitting
needle. Its color in water is usually drab, but when it lives secluded
from the light it is generally white, hence the specific name,
variabilis.
Snakes properly so-called, belong to the backbone or vertebrate
series of animals ; whereas the true worms belong to the backboneless
or invertebrate series. We have no snakes as slender as a knitting
needle, or in any way resembling a slender worm. We have no nema-tode
worms which are visible to the unaided eye that are parasitic
on human beings. Neither are they venomous or poisonous. They
are, in fact, useful, in so far as they destroy noxious insects like
cabbage worms and grasshoppers. Even should such a worm be left
in a cabbage, cooking would render it unnoticeable, and as it is not
poison no one need be afraid to handle or eat cabbage on account of
the mythical "cabbage snake."
Gerald McCarthy, Biologist,
N. C. Department of Agriculture.
Note.—The Station will be pleased to identify further specimens,
and would be glad to have any assistance or suggestions that will
enable it to obtain definite information regarding cases of poisoning
from "Cabbage Snakes."
64 TWENTY-FIFTH ANNUAL REPORT, 1902.
NORTH CAROLINA AGRICULTURAL EXPERIMENT STATION
B. W. KIlGORE, Director.
AXTHRACXOSE OR "BLACK-RUST" OF COTTON.
"Black-rust" of cotton bolls is each year becoming worse in the
cotton fields of the eastern part of North Carolina. The damage is
extensive in moist seasons. It frequently amounts to one-tenth of
the crop.
"Black-rust" is a fungus disease, and the spores or germs of the
fungus are usually transmitted from place to place with and in the
cotton seeds. The fungus also attacks the leaves and stems of the
cotton plant, but this form usually causes no appreciable damage.
The spores of the fungus may, however, live over winter in the stems
crnd diseased bolls of the preceding crop.
Remedies for "Black-rust.'
v
The simplest and most effectual remedy for this disease is the
annual selection of seed from plants known to be free from the fun-gus.
This, in connection with rotation of crops by means of which
cotton will not come upon the same field oftener than once in three
years, will reduce damage by "Black-rust" to an inappreciable quan-tity.
Cotton may be sprayed like other herbaceous crops. Tor this
crop we must use a spray which will not stain the lint. The am-moniacal
carbonate of copper is the best spray to use upon cottou.
This is made by dissolving six ounces of copper carbonate in three
pints of strong ammonia and adding the resulting solution to fiftv
gallons of water. This may be sprayed on the plants by any of the
garden or orchard sprayers in common use. The Bordeaux mixture
may be used upon cotton while it is young, but is no better than the
ammoniacal carbonate, and if used after the bolls attain full growth
—and this is the time when it is most needed—the Bordeaux mixture
is liable to stain the lint.
Paris green at rate of four ounces to the barrel may be used with
the Bordeaux mixture to destr