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SOILS OF NALYSIS

Julieth Stephanía Cano Manjarres1, Laura Orozco1, Natalia Venegas, Katherine silva

Laboratorio de Química agrícola, Universidad de la Amazonia, Facultad de Ciencias Básicas, Programa de


Química, Florencia, Caquetá-Colombia.

ABSTRACT

Soil analyses contain multiple studies or tests that manage to give a very
comprehensive understanding of the soil, for its correct classification and evaluation. In this
way, a study of a soil sample was carried out to which the pre-treatment of drying, crushing
and sieving was performed, continuing with the analyses, which consisted of the
assessment of pH, texture, Organic Carbon, AI, CIC, interchangeable bases and PD,
obtaining that the soil studied was moderately acidic with a pH of 5.81, with a medium
cation exchange of 19.2meq, but with a very low level of total interchangeable bases, value
that was taken into account since these are the ones that neutralize the acidity of the soil.
For samples taken from fresh soil microbial respiration was performed, which is important
to know the fertility of the soil, finding that fresh soil at 1 Kg released 119 mg CO2,
likewise more tests were also performed as phosphoric retention and zero load point

INTRODUCCIÓN

A great variety of minerals make up the soil, this in general is a complex compound
that takes very diverse forms and can depend on several factors, mainly atmospheric
conditions, the action of microorganisms and mesofauna. (Garrido Valero, s.f). For the
evaluation of the site or the classification of the soil is important the description and/or
characterization of this, in this way it can prevent or reverse its degradation, as well as
frame the appropriate management to provide to the soils (Zuñiga-Rojas, 2009), to know
the nutrients, texture, water properties, necessary elements, hence it is necessary to
establish methodologies for the study of soils. According to this, a method to validate soil
analysis is presented in the present, one that was pretreated to a size of 2mm with sieving,
and another with fresh soil.
Garrido Valero, M. Soledad (s.f). Interpretation of Soil Analysis. Ministry of
Agriculture fisheries and food. Vargas-Rojas Ronald.(2009). Guide to the description of
soils. Fourth Edition. United Nations Food and Agriculture Organization.

Elements that are part of the plant nutrition process, such as carbon, hydrogen,
oxygen, nitrogen, phosphorus, sulfur, sodium, aluminum and/or silicon, as well as some
others that are not found in the structural composition of natural products but that are
necessary for the development and growth of these or catalyze the process, such as iron,
manganese, zinc, copper, boron, chlorine, molybdenum, which can be studied by means of
specific equipment such as the atomic absorption spectrometer. For the study of these
nutrients and/or minerals different trials were carried out within the Methodology of this
experimental. Some complementary tests were used for the understanding of soils, such as
the Uv-Vis, determines the absorbances of a sample, looking for the peak of maximum
where the analyte absorbs more light radiation and serves to analyze or check the presence
of specific organic molecules.

MATERIALS AND METHODOLOGY


The pre-treatment of the sample was based on taking the soil sample and drying it at
room temperature. Once dried, the sample was crushed and sieved at 2 mm and its
respective triplicate was made.

After pretreatment of the sample, the following parameters are evaluated: pH,
Texture, Organic Carbon (OC), Exchangeable Acid (EA), Cation Exchange Capacity
(CEC), Exchangeable Bases, Available Phosphorus (AP), Microbial Respiration,
Phosphorus Retention, Soil Zero Loading Point, Electrical Conductivity, Chlorides, n-
Value, Ignition Loss, Minor Elements, UV VIS Spectroscopy and Soil Buffering Capacity.

pH: 10 g of dry and sieved soil were weighed, then transferred to a 125 ml
Erlenmeyer and 10 ml of deionized water was added, stirred for 1 hour, and the pH reading
was recorded.

Texture: 25 g of dry soil were weighed and then 10 ml of Calgon solution plus 150
ml of distilled water were added and agitated in a three-blade mixer for 5 min. The sample
was deposited in 1000 ml plastic test tubes and brought to volume with glyph water. After
40 sg and 2 hours, temperature and density measurements were taken. Finally, calculate
percentages of sand, silts and clays.

Organic carbon (OC): 0.5 g of dry soil was weighed and transferred to a 250 ml
Erlenmeyer, then 10 ml of K2Cr2O7 and 10 ml of 98% H2SO4 were added. Two blanks
were constructed and, together with the samples, were heated for 20 min. They were
allowed to cool and then 100 ml of deionized water was added; 5 drops of ferroin indicator
were added to each Erlenmeyer and then titrated with the Fe2SO4.7H2O solution and each
value obtained was determined. Finally, the working concentration of Fe2SO4.7H2O was
determined taking into account the value obtained by titrating the blank against the volume
of K2Cr2O7 1N added to each of the samples.

Exchangeable Acidity (EA): 10 g of soil were weighed and deposited in a 250 ml


Erlenmeyer flask, 80 ml of KCl were added and shaken for 20 min, centrifuging and
filtering at the same time. After having each sample filtered, they were transferred to a 250
ml Erlenmeyer flask and 3 drops of 0.1% phenolphthalein were added, titrating the solution
with NaOH. And finally, two blanks were made as well as the standardization of NaOH
using Potassium Biphthalate.

Cation Exchange Capacity (CEC): 5 g of dry soil were weighed and deposited in a
250 ml Erlenmeyer, 60 ml of AcONH4 at pH 7 were added, and agitated for 20 min,
performing both centrifugation and filtration. To the soil contained in the centrifuge tube,
50 ml ethanol was added and shaken manually for 1 min. Then, 50 ml of 10% NaCl was
added to the centrifuge tube with manual shaking for 1 min. After centrifugation, the
sample was filtered and added back to the 250 ml Erlenmeyer to which 5 ml of 38%
formaldehyde plus 3 drops of 0.1% phenolphthalein were added. The corresponding sample
plus the two blanks used in the process were titrated with 0.1N NaOH, and the 0.1N NaOH
was also standardized.

Interchangeable Bases: The first step of (CIC) was taken into account, 1 ml of 5%
Lanthanum Chloride was added to the sample in a 250 ml bucket, which was then gauged
with deionized water. Then, it was taken to the atomic absorption and emission equipment
using the flame mode, to determine elements such as: Sodium (Na), Calcium (Ca) and
Magnesium (Mg), Potassium (K).
Available Phosphorus (PD): 2.85 g were weighed and deposited in a 125 ml
Erlenmeyer, 20 ml of extractant solution were added and shaken for 1min and filtered. A
calibration curve was constructed taking into account the parameters given by the teacher,
including the two blanks. Finally, the spectral curve was made from 600 to 800 nm to
determine the absorbance of the samples.

Microbial Respiration: 40 g of fresh soil were weighed and deposited in a beaker, 20


ml of 1M KOH was added to another beaker and the two beakers were placed in an eight
ounce screw-top container and left closed for 8 days. 20 ml of KOH at 1M were titrated
with HCl. After the 8 days the 1M KOH solutions of the soil sample and blank were
titrated.

Phosphorus retention: 0.1 ml of 10 ppm phosphorus standard aliquot was taken and
absorbance and available P concentration of the soil were determined. (This was done with
the available phosphorus aliquot). Then, 20 ml of 10 ppm phosphorus standard was taken
and 3 g of dry soil was added and shaken for 30min and centrifuged. If coloration was
obtained, a small amount of activated carbon was taken to remove the coloration. Then, 0.1
ml of colorless supernatant was taken and the absorbance and P concentration of the soil
was determined.

Soil Zero Loading Point: 4 g of dry soil was weighed. To each of the 8 plastic
bottles of 150 ml, 4 g were added, then 60 ml of deionized water and a few drops of HCl at
0.1 N were added until the pH was the same as indicated in the table provided by the
teacher, the bottles were shaken and the pH reading was taken. After 8 days, the pH was
read again.

Chlorides and Electrical Conductivity: 4.2468g of AgNO3 was weighed at 0.025N


and brought to 1L with water. We weighed 100g of dry soil and adding distilled and
deionized water made a saturated paste and let it stand for 2h. It was centrifuged for 5min.
The electrical conductivity of the supernatant and the water used was determined and the
determination temperature was taken. Then, 5ml of the extract was taken, deposited in the
Erlenmeyer and 45 ml of distilled and deionized water was added, 4 drops of 1% Potassium
Chromate were added. Finally, it was titrated with AgNO3 to 0.05N. (blank was made)
Value n: Soil moisture; the petri dish (P1) was weighed and then 40 g of soil with
field moisture was added. After some time, the petri dish was weighed together with the
wet soil sample (P3). It was dried in the oven at a temperature of 100°C for 24 h. Remove
the assembly from the oven, allow it to cool, and weigh (P3).

Loss on Ignition: A crucible was calcined at 480°C for 4 h, then the crucible was
weighed (P1), then without taring 1-2g of dry soil was weighed (P2) and calcined at 480°C
for 4h and the calcined crucible was weighed after cooling. (P3).

Minor elements: 10g of dry sample were weighed and 40ml of the double acid
solution was added, which was prepared with 98% sulfuric acid and 37% hydrochloric acid;
the samples were shaken for 30 min and centrifuged for 5min. Finally, they were filtered
and passed through the atomic absorption equipment.

UV VIS spectroscopy: 15 g of dry soil were weighed and 100 ml of 4% NaOH were
added, left in extraction for 2 h, shaken, and centrifuged. Then a 1:25 dilution was made
with distilled water. The spectral curve was read from 240 to 665 nm in 0.5 nm intervals.
The spectra of zero order, first, second, second and third and fourth derivatives were
determined.

Soil buffering capacity: 10 g of dry soil were weighed and deposited in an


Erlenmeyer flask, 25 ml of alkaline solution were added (according to conditions given by
the teacher). Each suspension was shaken for 30 min and the pH was determined.

RESULTS AND DISCUSSION

Interchangeable acidity

IA=

IA = 0,9 meq/100g ó 0,9meq 100g-1 ó¡¡ 0,9 cmolc/kg inidica catión


c

0,9 cmol(+)/kg o 0,9 cmol(+)kg-1 o 0,9cmolc/dm3 o 0,9cmol(+)dm-3


Cmol= centimol
SAI%= PERCENTAGE SATURATION EXCHANGEABLE ACIDITY
CICA = EXCHANGEABLE CAPACITY OF CATIONIC AMMONIUM ACETATE
CICA =
CICA =
CICA = 19.2 meq/100g was average according to each is between 10 and 20 meq/100g
TOTAL INTERCHANGEABLE BASES:
Ca (mg/L) : (3-9) 2,1105
5g->250mL->3mL->9mL-> 2,1105mg/L
muy Bajo según mircofertisa
1eqCa=
1eqCa= 20g
1meqCa = 0,020g
1meqCa= 20mg
Mg(mg/L) : (3-9) 0,1379
5g->250mL->3mL->9mL-> 0,1379mg/L
Lower to very low according to microfertise
1eqMg=
1eqMg= 12g
1meqMg = 0,012g
1meqMg= 12mg
K: (3-12) 0,0469
5g->250mL->3mL->12mL-> 0,0469mg/L
bajo según microfertisa
1eqK=
1eqK= 39g
1meqK = 0,039g
1meqK= 39mg
Na m/L : (3-12) 0,9704
5g->250mL->3mL->12mL-> 0,9704mg/L
1eqNa=
1eqNa= 23g
1meqNa = 0,023g
1meqNa= 23mg
GRASSROOTS RELATIONS
conditioned according to microfertisa
= = 0,025 deficiente
Total bases
1,58cmolc/dm3+0,17 cmolc/dm3+0,024 cmolc/dm3+0,84 cmolc/dm3 = 2,614 cmolc/dm3
PSI= PORCENTAJE DE SATURACIÓN DE SODIO INTERCAMBIABLE
PSI%=
PSI%= según el IGAC es inferior al 15% normal
CICE= EFFECTIVE CATIONIC EXCHANGE CAPACITY
CICE= (AI+BT)
CICE= 0,9 + 2,6
CICE= 3,5 meq/100g Bajo
SAI% = PERCENTAGE SATURATION EXCHANGEABLE ACIDITY
SAI%=
SAI%=
SAI%=

SAI%=
SAI%=
SAI%= 4,7% SATURACION DE ALUMINIO
SB%=
SB%=
SB%=13,54% normal según microfertisa
ORGANIC CO= CARBON
Is not of agronomic control according to igac
MO%= ORGANIC MATTER
MO%= CO% x 1,724
MO%= 1,85 x 1,724
MO%= 3,18% Medio bajo según microfertisa y según igac es clima cálido y esta
N%=NITROGENO
N%= MO x 0,05
N%= 3,18 x 0,05
N%= 0,159%
Ndisponible% = N% x 0,027
Ndisponible% = 0,159 x 0,027
Ndisponible% = 0,00429%
RC/N= RELACION CARBONO NITROGENO
RC/N=
RC/N=
RC/N= 11,6
FOSFORO DISPONIBLE
V inicial solcion C Solucion patron C final de P
Tubo V final (ml)
patron de P (mL) (ppm) (ppm)
Tubo ppm (mg/L) Absorbancia Abs corregida
b 0 0,0556 0
1 0,2 0,1174 0,0618
2 0,4 0,2013 0,1457
3 0,6 0,2165 0,1609
4 0,8 0,289 0,2334
5 1 0,393 0,3374
6 1,2 0,4119 0,3563

Prepare one liter of a 50 mg/L P solution from KH2PO4 (99, 5%). How much is KH2PO4
weighed?
Prepare a solution of 9.7 mgP/L. What is the aliquot to measure from the solution of 50
mgP/L?
Linear regression model y = 0.305x + 0.0021 abs= 0.305 (mg/L) + 0.0021
Coefficient of determination was R2= 0.9786 r=0.99
Report linear regression model and coefficient of determination
ml Cl-
2,85g->20mL sln->0,2mL->10mL-> 0,1933mg/L
A=

TEXTURES
Class: Sandy loam according to textural triangle
C solución patron
Tubo Absorbancia Abs Corregida
(ppm)
0 0,1315 0 0
1 0,2164 0,2 0,0849
2 0,2619 0,4 0,1304
3 0,3307 0,6 0,1992
4 0,3328 0,8 0,2013
5 0,3938 1 0,2623
6 0,4161 1,2 0,2846

Floor-less

Floored
0,8 ml tube 4, 10 ppm; A= 0,2917

1.32 -----------------100%
1,14 ------------------
Phosphoric retention = 100% - 86.3% = 13.7%
Microbial respiration
PUNTO DE CAARGA CERO DEL SUELO
c Suelo Seco a Agua Ph requerido ph (8 días) Delta pH
2mm (g) desionizada
(ml)
0 4 60 8,1 6,82
1 4 60 2,92 3,69
2 4 60 4,16 5,12
3 4 60 5,01 5,38
4 4 60 6,10 5,94
5 4 60 7,14 6,24
6 4 60 7,91 6,14
7 4 60 8,90 6,37
8 4 60 7,98 6,88

pH Δph=ph(8 días)-
No. pH inical (8días) ph(inicial)
1 2,91 3,69 0,78
2 4,16 5,12 0,96
3 5,01 5,38 0,37
4 6,1 5,94 -0,16
5 7,14 6,24 -0,9
6 7,91 6,14 -1,77
7 8,9 6,37 -2,53

CONDUCTIVIDAD ELÉCTRICA
Conductividad eléctrica muestra: 610 ꭎs/m a T° 26,7°C
Conductividad eléctrica blanco: 6,64 ꭎs/m a T° 25°C
CEcorregida : 610 ꭎS – 6,64 ꭎS = 603,36 ꭎS/m (microsimens) a 26 °C
CTS= contenido total de sales
603,36 ꭎS  0,60336 mS
CTS= Contenido de Sales totales
CTS = 0,64 x 0,60336 mS
CTS=0,38 dS/m normal según microfertisa, normal micro
CLORUROS
muestra de suelo sin sal
muestra de suelo con sal

Expresado como NaCl (mg/kg)


Muestra de suelo sin sal
58,44gNaCl ----------------- 35,45gCL
X ------------------ 7,09mgCL

Muestra de suelo con sal


58,44gNaCl ----------------- 35,45gCL
X ------------------ 222,4mgCL
NaCl
Entocnes en 100g gramos hay 36,6 mg en 100 g de NaCl

muestra de suelo con sal


VALUE N
The measurement is performed by gravimetry after drying at a maximum
temperature of 100°C, in the literature specify a maximum of 105°C. This temperature
increase, maintained for a controlled time, is high enough to eliminate the "free" forms
water and low enough not to cause significant loss of organic matter and unstable salts by
volatilization (Pansu & Gautheyrou, 2006).

Table 1 experimental data for the determination of %Hg and value n


Código NKLJ (1) P1 45,2600g P2 85,8820g P 74,5383g
3
Código NKLJ (2) P1 43,0885g P2 83,6940g P 72,6596g
3

replay 1
gravimetric humidity
Replay 2
gravimetric humidity
Average =
%Hg=38% gravimetric soil moisture.
As a result, 38% gravimetric moisture is obtained from the soil sample.
Repeatability and reproducibility are satisfactory in most soils if procedures are rigorously
followed (Pansu & Gautheyrou, 2006).

This method can be considered "destructive" for certain types of soils and analyses
as the physical and chemical properties can be transformed, therefore the samples used in
this method were not used for further analysis.

Value of n

I miss that I do tomorrow

Soil is between 0.7 and 1.0 range, soil flows with difficulty between fingers according
to USA, describes if it is very or very dry

IGNITION LOSS
The soil consists of a solid, mineral and organic phase, a liquid phase and a gaseous
phase. The physical and chemical characteristics of the solid phase result in a high
variability of water content and a variable degree of resistance to moisture removal.

This method causes partial oxidation of organic matter using moderate to high
temperatures, and the weight lost during the procedure is related to the organic content of
the soil. On the other hand, Grewal et al. (1991) showed that this procedure can cause a
structural loss of water, especially of oxyhydroxides, as well as structural changes in some
inorganic compounds therefore what is recommended according to the literature is not to
exceed 450ºC (GREWAL et al., 1991).
The experimental soil presents a percentage of mineral fraction of 86.7%, the weight lost is
13.3% related to the organic matter content.

Table 2 Experimental data for the loss-by-ignition method


Código NKLJ (1) P1 15,1555g P2 17,2863g P3 16,9952g
Código NKLJ (2) P1 17,8929g P2 19,1827g P3 19,0177g

Replay 1
%Ce=
%Ce=
%Ce=86.3%
Replay 2
%Ce=
%Ce=
%Ce=87.2%

Average =
%Ce=86.7%
%organic matter in soil= 100%-86.7%
=13.3 per cent
The accumulation of organic matter occurs in the first 20 cm of the soil, in the organic
horizons and the horizon A. Below these appear the mineral horizons B, C and in some
cases D, which very little contribute to soil fertility (Peña Venegas, 2010).

Minor elements
Cu 0.1945 mg/L Fe 2.2787 mg/l Mn 0.3388 mg/l
10g ------- 40 mL ---- 0,1945 mgCu/L
Cu( mg/kg)=
Buffering capacity of the floor
Linear regression equation y = 1.6969x - 10.651
gKOH/kgsuelo 1,6969 (pH) - 10,651
R2 = 0,9531
CT= pHBC= 1,6969gKOH/kgsuelo. pH
1.6969gKOH is needed to increase a pH unit, 1kg of soil
CONCLUSION
Finally, we can conclude that thanks to the different technical, the characterization
of the soil was achieved, where an arduous analysis was generated from data already
referenced and so to obtain specific data of the type of soil that exists in Macagual.

From the previous analysis, the soil sample of this study was moderately acidic
with a pH of 5.81, with a medium cation exchange of 19.2meq, but with a very low level of
total interchangeable bases, value that was taken into account since it is these that
neutralize the acidity of the soil.

From the previous analysis, the soil sample of this study was moderately acidic
with a pH of 5.81, with an average cation exchange of 19.2meq, but with a very low level
of total interchangeable bases, value that was taken into account since these are the ones
that neutralize the acidity of the soil, finding the level of calcium, magnesium and poasio
are very low, but the high sodium, this value is probably the one that affects the electrical
conductivity, since this is directly related to the concentration of dissolved salts, finding
that for 1 kilogram of soil there is 7.1 mg and in the form of sodium chloride presents 11.70
mg.

REFERENCES
Garrido Valero, M. Soledad (s.f). Interpretation of Soil Analysis. Ministry of Agriculture,
Fisheries and Food.
Pansu, M.y Gautheyrou, J. (2006). Medida de pH (págs. 551 - 579). Springer Berlín
Heidelberg.
Vargas-Rojas Ronald.(2009). Guide to the description of soils. Fourth edition. United
Nations Food and Agriculture Organization.
Venegas, C. P. P., & Vanegas, G. C. (2010). Dynamics of Amazonian soils degradation
processes and alternatives for their recovery. Amazonian Institute of Scientific Research"
SINCHI".

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