Análisis de Suelos
Análisis de Suelos
Análisis de Suelos
as Used in the
L. A. Alban
Mildred Kellogg
INTRODUCTION
There are many methods currently in use for the testing of soils. Each
section of the country appears to favor a particular method or group of methods
and many times individual soil testing laboratories develop modifications of
these methods. Then, too, procedures have changed greatly in the last 10 to 15
years. The development of new instruments, such as the flame photometer, and
new titration procedures such as EDTA or Versene, have practically revolutionized
soil testing. They not only have made the methods more accurate but have made
them many times more rapid.
The methods for the analysis of soils as given here are those which are
currently being used in the Oregon State College Soil Testing Laboratory. They
have been selected on the basis of their reliability for predicting fertilizer and
liming needs of Oregon soils and for their adaption to use for a large volume of
soils. Changes will be made in these procedures from time to time as new methods
and techniques are developed.
PREPARATION OF SAMPLE
Soil samples are air-dried and then passed through a mechanical crusher
consisting of two rollers which turn toward each other. The soil then passes
through a 10-mesh screen. The rollers are kept clean by large brushes held
tightly against them. The soil samples are kept for at least 5 days before being
tested, especially for potassium.
METHODS OF ANALYSIS
A. Reagents
1. Standard buffer solutions to standardize pH meter
B. Procedure
1. Weigh 10 grams of soil into a 50 ml beaker or No. 250 C.R. souffle
cup. Add 10 ml of distilled water.. Stir thoroughly.
2. Let stand for at least 30 minutes, stirring two or three times.
3. Read with a pH meter using a glass electrode.
A. Reagents
1. Buffer solution - Weigh out 800 grams calcium acetate, 160 grams
p-nitrophenol, and 12 grams magnesium oxide. Dissolve in about 18
liters distilled water. Make up to 20 liters. Let settle for a
week then adjust to pH 7.0 with HC1 or NaOH.
-2
B. Procedure
1. Weigh out 10 grams of soil and place in a shaking bottle with 50 ml
of ammonium acetate solution, shake for 30 minutes.
2. Transfer to a Buchner funnel and wash with an excess of 150 to 200
ml of ammonium acetate. Potassium, calcium, magnesium and sodium can
be run on this extract by making filtrate up to a volume of 250 mis.
Filtrate is run on the flame photometer using standards from IV.
3. Wash out the excess ammonium acetate with 150 to 200 ml ethyl alcohol
and discard filtrate.
4. Change to a clean filter flask and wash the soil with 250 ml
0.1 N HC1 to replace the ammonia.
5. Transfer the filtrate from steps 4 to an 800 ml Kjeldahl flask, add
10 grams NaC1, 10 mis concentrated NaOH, and an anti-bumping disc.
6. Attach immediately to the condenser and distill approximately one-third
of the solution over into a previously placed 500 ml Erlenmeyer
flask containing 50 ml saturated boric acid solution and 1 ml mixed
indicator.
7. Lower the Erlenmeyer flask to prevent back-suction of the material and
turn off burners.
8. Titrate the NH3 with 0.1000N H2SO4.
C. Calculation
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weight of material grams
IX. BORON - Curcumin method (3)
A. Reagents
1. Curcumin - oxalic acid solution - Dissolve 0.04 gram finely ground
curcumin in 100 ml 950 ethyl alcohol by warming slightly in warm
water. When curcumin is dissolved, add 5 grams oxalic acid, dissolve,
cool, and store in refrigerator for at least two days before using.
When stored in a refrigerator the reagent should keep for a week or
two.
2. Ethyl alcohol
3. Standard boron stock solution - Dissolve 0.5716 gram of C.P. boric
acid in 1000 ml distilled water. This solution contains 0.1 mgm
of boron per ml or 100 ppm and servew as the primary base stock
solution. From this standard solution of 0.2 to 2.0 ppm B should be
made up when necessary.
B. Procedure
1. Weigh 20 grams of soil into a 125 or 250 ml boron-free flask.
2. Add 40 ml distilled water and reflwm for 5 minutes. Condensers
should be of boron-free glass.
3. Place suspension in 50 ml centrifuge tube and centrifuge for 20 to
30 minutes at 2000 RPM. Help clarify by adding 0.02 gram calcium chloride
before centrifuging.
4. If extract is colored add small amount of decolorizing charcoal and
filter.
5. Place a 1-ml aliquot of the clear solution in a No.000 Coors
evaporating dish.
6. Add 4 ml curcumin-oxalic acid solution and mix thoroughly by rotating
the evaporating dish.
7. Evaporate to dryness on a water bath at 55 0 4 300, and then continue
to bake the residue at this temperature for a minimum of 15 minutes
to insure complete dryness. Cool.
8. Treat the reaction products with 25 ml of 95% ethyl alcohol.
9. Filter through a Whatman No. 2 (or equivalent) filter paper. Filtering
can be done directly into the comparison tubes, if desirable.
10. Read in colorimeter or spectrophotometer at 540 mu.
11. Determine amount of boron from curve prepared by running a series
of standard solutions.
X. NITRATE-NITROGEN (4)
A. Reagents
1. Phenoldisulfonic acid - Dissolve 25 grams of pure (white) phenol in
150 ml concentrated H2SOL . Add 75 ml of fuming H,SOL . Mix the
solution and heat for 2 Hours at 100 0C in a boilifig Bath. Store
solution in a brown bottle.
2. Ammonium•hydroxide solution - Mix equal volumes of concentrated
NH OHand distilled water.
3. Calcium hydroxide solution - Add excess Ca(OH) to 1 liter of
distilled water. 2
4. Standard nitrate solution - Dissolve 0.7221 gram of pure dry KNO in
distilled water and dilute to 1 liter. This solution contains MO ppm
N or nitrates and serves as the base stock solution. Standard solution
of 0.5 to 10 ppm N should be made up when necessary.
B. Procedure
1. Shake 10 grams of soil with 50 ml of distilled water for 10 minutes.
Add 0.2 gram Ca(OH) 2 powder and shake for an additional 5 minutes.
2. Filter and wash with an additional amount of water.
3. Transfer 5 ml of the filtrate to a 5-ml beaker. Add 1 ml (Ca(OH)
(Ca(OH) 2
solution and evaporate to dryness on a warm hot plate. Cool.
4. Add 1 ml of phenoldisuifonic acid and rotate the beaker so that the
acid comes in contact with all of the residue.
5. Add 14 ml of distilled water and 5 ml of 1:1 ammonium hydroxide
solution.
6. Transfer the solution to a colorimeter tube and read in a colorimeter
at 420 mu.
Determine the amount of nitrate from curve prepared by running a series
of standard solutions.
XI. AID MONIUM-NITROGEN (5)
A. Reagents
1. Potassium chloride extracting solution - Dissolve 149 grams KCI in 2
liters of distilled water.
2. Nessler reagent - In a 1000 ml volumetric flask dissolve 91 grams
mercuric iodide and 70 grams potassium iodide, using as little water as
possible. Add 224 grams KOH, dilute to 1 liter, mix well and cool.
Let stand for a few days to allow any precipitate to settle. Decant
into a brown glass bottle and store for use.
3. Sodium hydroxide - tartrate solution - Dissolve 80 grams sodium tartrate
in about 500 ml of distilled water. Add 26 grams NaOH and after it is
dissolved dilute to 1 liter.
4. Gum accacia solution - Dissolve 10 grams powdered gum accacia in 195 ml
distilled water then add 5 ml Nessler t s reagent. Gum accacia may be
dissolved most readily by adding sufficient water to make a paste
and then add the balance of water while stirring. Let settle a few
days and decant into a brown glass bottle.
5. Copper sulfate solution - Dissolve 25 grams CuSO4 in 1 liter of water.
6. Standard ammonium solution - Dissolve 0.4714 gram pure ammonium sulfate
in 1 liter of distilled water. This gives a solution of 100 ppm N
as ammonium. From this stock solution standards of 0.1 to 2.5 ppm N
as ammonium can be made as needed.
B. Procedure
1. Place 10 to 20 grams of soil in a shaking bottle.
2. Add 100 ml extracting solution and 4 drops of copper sulfate solution.
3. Shake for 30 minutes and filter. Suction filtering can be used to
speed up the operation.
Note: Beyond this point tame is critical. Add all reagents to each
stele before going onto next. Read color in 15 minutes.
A. Reagents
1. Hydrochloric acid, 1 N - Dilute 860 ml concentrated HC1 to 10 liters
with distill, d water. Mix thoroughly. Standardize against primary
Na,CO.
2. Soaiud hydroxide, 1 N - Dissolve 420 grams sodium hydroxide pellets
in about 5 liters of distilled water stirring constantly to prevent
caking. Cool, then make up to 10 liters with distilled water. Mix
thoroughly. Standardize against the standard 1 N HC1.
3. Phenophthalein indicator - Dissolve 1 gram phenolphthalein in 50 ml
ethyl alcohol and add 50 ml distilled water. Place in a dropper bottle.
B. Procedure
1. Weigh out 1 gram of finely ground material into 250 ml Erlenmeyer
flask.
2. Add a known amount of 1 N HC1 (usually 25 m1). Heat on hot plate
until almost boiling. Remove, cool and wash down neck of flask with
distilled water.
3. Titrate excess HC1 with 1 N NaOH using phenolphthalein as indicator.
C. Calculations