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CIC y Bases Intercambiables
CIC y Bases Intercambiables
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GLOBAL SOIL LABORATORY NETWORK
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PARTNERSHIP
Standard operating procedure
for cation exchange capacity
and exchangeable bases
1N ammonium acetate, pH 7.0 method
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Global Soil Laboratory Network GLOSOLAN-SOP-17
GLOSOLAN
CATION EXCHANGE CAPACITY AND
EXCHANGEABLE BASES BY AMMONIUM Version number : 1 Page 1 of 17
ACETATE METHOD Effective date : 26 July 2022
VERSION HISTORY
02
Etc.
Contents
1. Introduction to CEC and exchangeable bases................................................................................. 3
2. Scope and field of application ......................................................................................................... 3
3. Principle .......................................................................................................................................... 4
4. Apparatus ........................................................................................................................................ 5
5. Materials ......................................................................................................................................... 5
6. Health and safety ............................................................................................................................ 7
6.1 Personnel Safety ....................................................................................................................... 7
6.2 Chemical Hazards ...................................................................................................................... 7
7. Sample preparation ........................................................................................................................ 7
8. Procedure ........................................................................................................................................ 7
9. Calculations .................................................................................................................................... 9
9.1 Calculations for CEC .................................................................................................................. 9
9.2 Calculation for exchangeable bases .......................................................................................... 9
10. Quality assurance / quality control ........................................................................................... 10
10.1 Precision Test ................................................................................................................... 10
10.2 Accuracy Test .................................................................................................................. 10
10.3 Quality Control Chart ....................................................................................................... 10
11. Reference documents .................................................................................................................... 12
12. Appendix I – Acknowledgments ............................................................................................... 13
13. Appendix II – List of authors .................................................................................................... 13
14. Appendix III – Contributing laboratories .................................................................................. 14
The term “exchangeable bases” or “total exchangeable bases” refers to the sum of the concentration
of the bases (calcium, magnesium, potassium, and sodium) in exchangeable form. Exchangeable
cations are those that can be exchanged by a cation of an added salt solution. Calcium is more
dominant than other cations in most agricultural soils. The minerals present in the soils govern the
dominance of exchangeable bases. In the absence of excess CaCO3, the cations Ca2+, Mg2+, and Na+
appear to be exchangeable by NH4OAc, except in certain soils containing trioctahedral vermiculites.
This method plays an important role for soil taxonomy (Soil Survey Staff, 1975) and it is widely used
for non-calcareous, neutral soils which are dominated by clay minerals with permanent surface
charges.
This method overestimates the CEC of acidic soils as additional negative charge is developed on
colloidal exchange sites after the addition of ammonium acetate solution having pH 7.
The method underestimates the CEC of soils containing carbonates or gypsum because the release of
calcium carbonates or sulfates from the soil into the ammonium acetate solution limits the saturation
of exchange sites by ammonium ions.
Caution should be exercised in using this method for soils dominated by vermiculite and mica clays
because ammonium ions are fixed between the layers of these clays. This methods thus causes the
layers to collapse and the fixed ions can no longer be exchanged by sodium ions.
In relation to the exchangeable bases, for soils with the presence of gypsum (calcium sulfate),
extraction with ammonium acetate only allows the quantification of exchangeable magnesium,
sodium and potassium, since the calcium content is affected by the excess calcium in the gypsum.
Likewise, in soils containing calcium and magnesium carbonates, extraction with ammonium acetate
only allows the quantification of exchangeable sodium and potassium, since the content of calcium
and magnesium is affected by the excess of ions from the carbonate.
Another problem arises in soils affected by salts, because the soluble cations (from the salts) are
extracted together with the exchangeable bases.
3. Principle
CEC determination is based on reference solution conditions (buffered to pH 7.0) by minimizing the
errors to obtain the data that should be accepted universally. It is the crucial step to select the proper
method as different methods give different results. Methods to determine the CEC consists of various
steps like soil pre-treatment, saturation, washings, etc.
Different methods have been developed to determine CEC, depending on the type of colloidal material
involved in the cation exchange of the soil. This SOP describes the most widely used method for
agricultural soils.
The soil is treated with 1 normal ammonium acetate solution buffered at pH 7.0 to remove
exchangeable cations from the exchange sites of the soil colloids and to saturate them with
ammonium ions. Then the exchangeable cations are quantified using different instrumental
methodologies (Atomic Absorption/Emission spectrometry using flame atomizers or Inductively
Coupled Plasma). The excess of ammonium ions in the soil samples are removed by washing with
ethanol. Then the adsorbed ammonium ions on soil sample are extracted using acidified sodium
chloride. Finally the ammonium is measured by distillation and titration.
In soils, with carbonates or gypsum, when preparing the report it is necessary to take into account and
not include Ca-Mg or Ca content in the report.
In saline soils, one of the options is to pre-wash samples with 70% alcohol to eliminate the salts
(soluble bases) and then carry out the extraction with ammonium acetate to quantify the
exchangeable cations. Another option is to perform a saturation extract and quantify the soluble basic
cations. The exchangeable bases (EB) are estimated from the subtraction of the soluble cations from
the total obtained by extraction with ammonium acetate
4. Apparatus
4.1. Reciprocal shaker, with a path that allows the complete agitation of the sample
4.11. Distillation tubes for the Kjeldahl equipment, with a nominal capacity of 250 mL
5. Materials
5.1 Deionized water/distilled water, It should have a specific conductivity not higher than 0.2
mS/m at 25 °C and a pH greater than 5.6 (or grade 2 water or type II water according to ISO
3696 and ASTM D1193-06, respectively, if this is the quality of water produced in the
laboratory).
Immediately before use, the pH should be checked to be 7.0±.1. If the pH is not 7.0, it should
be adjusted by adding diluted acetic acid or ammonium hydroxide (approximately 10% m/v).
Alternatively, the ammonium acetate solution could be prepared using glacial acetic acid and
concentrated ammonium hydroxide.
Dissolve 100 g of NaCl in 1000 mL of water. Drops of HCl are added, to adjust the pH to 2.5±0.2,
and heliantin, to identify the change in pH of the solution (through the heliantin turning red).
Dissolve 40.0 g ± 0.1 g of H3BO3 in 800 mL of preheated water at a temperature below 60 ºC.
Allow to cool to room temperature and bring to final volume of 1000 mL with water. Add 10
mL of each of these indicators (bromocresol green (50 mg in 100 mL alcohol) and methyl red
(50 mg in 100 mL alcohol). Add 1N sodium hydroxide drop by drop until the pH is adjusted to
value close to 5.0.
Spillages: Neutralize spilled acids with dilute solution of sodium bicarbonate or cover with dry sand or
other non-combustible material and place in appropriate waste disposal container.
Alcohol is a flammable liquid, and vapor and containers can build up pressure if exposed to heat and/or
fire.
Ammonium acetate is a corrosive, flammable liquid and vapor and can causes severe eye irritation
and skin burn. Thoroughly wash hands after using chemical reagents.
7. Sample preparation
On reception, examine sample status, break big lumps, and discard the big stones and the plant parts,
if any. If samples are moist, spread them on a cloth or paper or tray to dry under shade (not under
sun) where the sample will not be contaminated. If wet, dry for 2 to 3 days under shade and dry in
oven at 40oC overnight. Dried sample: disaggregate and sieve through 2 mm sieve. Repackage in
storage container and submit to laboratory for testing.
Prepare the soil sample according to the SOP Handling and Preparation of Soil Samples for Chemical
and Physical Analyses (https://www.fao.org/3/ca8283en/ca8283en.pdf)
8. Procedure
8.1 Weigh 5g of <2mm sieved soil in a 50 mL container/extraction tubes;
8.4 Centrifuge and filter the supernatant in a clean 100 mL volumetric flask with qualitative fine
porous filter paper. Repeat steps 8.2 to 8.3 two more times to obtain a total of approximately 100 mL
at the end. Fill up to the 100 mL mark with ammonium acetate and mix well. Keep the soil sample in
the 50 mL extraction/centrifuge tubes for step 8.6;
8.5 Analyze the extractant in 8.4 for Ca, Mg, Na and K by Atomic Absorption flame or plasma
spectrophotometry. Following the manufacturer’s guide: Suitable spectral lines are: Ca = 422.7 nm;
Mg = 285.2 nm; Na = 589.0 nm; and K = 766.5 nm. Ca2+ and Mg2+ are measured on dilute extracts,
whereas, extracts of Na+ and K+ analysis are only diluted if over range. And for plasma suitable
wavelengths are: Ca = 430.25 nm; Mg = 285.2 nm; Na = 588.96 nm; and K = 766.49 nm. It is suggested
to use a flame AA but an ICP-OES can also be used. The range of standards presented in table 1 is
recommended;
Table 1 – Recommended standard range
Ca Mg Na K
Flask 1 0 0 0 0 0 0 0 0
Flask 2 2 2 1 1 5 5 5 5
Flask 3 4 4 2 2 10 10 10 10
Flask 4 6 6 3 3 15 15 15 15
Flask 5 8 8 4 4 20 20 20 20
Flask 6 10 10 5 5 25 25 25 25
8.6 The samples in 50 mL extraction/centrifuge tubes from step 8.4 must be subjected to 2
consecutive washes with 50 mL 96% ethanol following the procedure in steps 8.2 and 8.3. Discard the
ethanol after each wash;
8.7 To displace the adsorbed ammonium ions ; add 33 mL of a 10% NaCl solution to the sample,
shake for 15 minutes, centrifuge and filter into a clean 100 mL volumetric flask;
8.8 Repeat steps 8.7 two more times to obtain a total of approximately 100 mL of NaCl solution
at the end. Fill up to 100 mL with NaCl and mix well;
Transfer 50 mL of aliquot NaCl extract into the distillation tube and connect to the distillation
unit. Then add 10 mL sodium hydroxide and distilled water to be automatically added to the aliquot
by the distillation unit.
Fill 25 mL boric acid into a receiving Erlenmeyer flask and place in position for distillate and
start the distillation.
9. Calculations
9.1 Calculations for CEC
Sample weight = 5 g
Extract = 100 mL
Aliquot = 50 mL
HCl concentration = 0.01 N
CEC meq/100g soil = (HCl used for sample - HCl used for blank) * HCl concentration * 100/5 *
100/50
Na Cmol(+)/kg soil = (Sample concentration in mg/l - blank concentration in mg/l) x 100/1000 x 1/10
x 1/22.99 x 1000/5 x dilution factor
K Cmol(+)/kg soil = (Sample concentration in mg/l - blank concentration in mg/l) x 100/1000 x 1/10 x
1/39.098 x 1000/5 x dilution factor
100/1000 conversion to L
1000/5 conversion to Kg
Modify by Revision Approved Date Validated Date
Compare results with the target precision for the analyte concentration (table of expected precision
as a function of analyte concentration by AOAC – see table 2).
Table 2: Expected precision (repeatability) as a function of analyte concentration.
for Out of Control Signals (+/- 2 SD). If Out of Control Signal/Trend is observed, identify root cause,
develop corrective and preventive actions.
Blakemore, Leslie Clifford. "Methods for chemicalanalysis of soils." NZ Soil Bureau Sci. Rep. 80 (1987):
72-76.
Chapman, H.D.,1965 "Cation-exchange Capacity,", in C.A. Black (ed.), Method of Soil Analysis, Part 2:
Chemical and Microbiological Properties, Am. Soc. Agron., Madison, Wisconsin. pp. 891-900.
Kalra, Y.P., Maynard, D.G., 1991. Methods Manual for Forest Soil and Plant Analysis. Northern Forestry
Centre, Edmonton, Alberta.
Sumner, M. E., & Miller, W. P. (1996). Cation exchange capacity and exchange coefficients. In
“Methods of Soil Analysis, Part 3. Chemical Methods” (D. L. Sparks, Ed.), Soil Sci. Soc. Am. Book Ser. 5,
pp. 1201–1229. Soil Sci. Soc. Am., Madison, WI.
GLOSOLAN would also like to thank the experts who were part of the Review Panel and who ensured
the finalization of the SOP, all the laboratories that provided inputs for the harmonization of this
method, all the experts from the GLOSOLAN Technical Committee who technically reviewed this SOP,
and Ms. Magdeline Camille Vlasimsky (University of Gent) for proofreading it.
• Soil and Water Resources Centre, Directorate of Agricultural Researches, Ministry of Science
and Technology, Iraq
• KIMIA AB environmental and agricultural consulting laboratory, Islamic Republic of Iran
• Kuwait Institute for Scientific Research, Kuwait
• Lebanese Agriculture Research Institute, Lebanon
• Soil Characterization Lab - AUB, Lebanon
• LABOMAG, Morocco
• National Institute of Agricultural Research - INRA, Morocco
• Homs lab - GCSAR, Syrian Arab Republic
• DRS/DGACTA, Tunisia
GLOSOLAN
GLOBAL SOIL LABORATORY NETWORK