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SOIL QUALITY AND PESTICIDE RESIDUES ANALYSIS

Mahendra Prasad, Pushpendra Koli
  • Country of Origin:

  • Imprint:

    NIPA

  • eISBN:

    9789390512577

  • Binding:

    EBook

  • Number Of Pages:

    114

  • Language:

    English

Individual Price: 3,000.00 INR 2,700.00 INR + Tax

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This book includes the techniques of soil quality and pesticide residue analysis in field of forage science. The collection and compilation of laboratory methods and techniques from various concrete sources and has been endeavored to include as much information as could be possible. It covers latest methods and interpretations from sampling to testing platforms. Provides detailed testing protocols and quality assurance protocols. This book helps the young researchers, scientists, students of M.Sc. and Ph.D. in field of soil science and pesticide residue analysis.

0 Start Pages

Preface In the recent past soil quality has been considered as one of the most concern for food and fodder security as well as human and livestock health. The goal of maintaining soil and feed quality will not be achieve without precise analysis of soil parameters and pesticide residue. The presence of pesticide residues in animal feed and its animal products is in the focus at the present scenario in the view of WTO. The residues not only affect the public health but also cause economic losses to the livestock industry. Not only these affect the health of livestock and human beings but also affect the quality of animal products. Pesticide residues accumulate in the animals either by direct contact with pesticide or by indirect contact with environment. Pesticides are used in forage crops for disease and pest control and they leave the residues in the feed and fodder consumed by animals. Common soil analysis methods for monitoring and determining soil quality are fundamental for successful soil management programme. There are well established standard methods for soil and pesticide residue analysis. The results on soil analysis are interpreted with the background of upgrade literatures and reported for valid recommendations. These analyses may help farmers to supplement nutrient to the soil system. This book will provide a virtual link among agricultural scientists engaged in teaching, research and extension activities.

 
1 Importance of Soil Testing Soil Sampling and Processing

Soil testing involves an estimation of its available nutrient status i.e. the portion or amount of nutrient directly available in soil for subsequent uptake by crop plant. This exercise is commonly referred to as soil testing and is used to arrive at optimum fertilizer application ratio. The need for estimation of available nutrient arises because only a small fraction of what the soil contains is the total nutrient content of the soil. Soil test are calibrated by correlating them with crop response and the result from the basis for making fertilizer recommendations. Estimation of nutrient contents and forms in materials that are involved in nutrient supply and dynamics is a conical step towards planning scientific nutrient management. In this content, both soil and plant testing information comes out of the interpretation of analysis assumes a greater value when their concentrations and amounts can relate to soil fertility, nutrient availability, plant growth, yield and quality of the crop produce.

1 - 6 (6 Pages)
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2 Determination of Soil pH and Electrical Conductivity

Determination of pH is actually measurement of hydrogen ions activity in soil-water system. It is defined as negative logarithm of the hydrogen ion activity. Mathematically, it is expressed as:pH = - log a H+ The pH value of a soil is an indication of soil reaction i.e. acidic, neutral or alkaline. The nutrient availability is governed by soil reaction. It is maximum at neutral pH and decreases with increase in acidity or alkalinity. Thus, pH value gives an idea about the availability of nutrients to plants. Principle The pH is a measure of hydrogen or hydroxyl ion activity of the soil-water system. It indicates whether the soil is acidic, neutral or alkaline in reaction. Since crop growth suffers much under both very low (strongly acidic) as well as very high pH (alkaline) conditions. Now a days, most of the pH meters have single combined electrode. Before measuring the pH of the soil, the instrument has to be calibrated with standard buffer solution of known pH. Since, the pH is also affected by the temperature, hence, the pH meter should be adjusted to the temperature of the solution by temperature correction knob.

7 - 10 (4 Pages)
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3 Determination of Soil Texture by Hydrometer Method

The method is based on the Stokes law which states that the rate of fall of particles in suspension is directly proportional to their size. Accordingly, larger particle (sand) will settle first, followed by silt and clay. The resistance offered by the liquid to the fall of the particles varies with the radius of the sphere. Principle This method is based on the principle of dispersion and sedimentation techniques, employed to a given weight of soil sample. Mechanical stirring disperses macro aggregates while chemical dispersing required for micro aggregates. The mixture of dispersed soil particles in water is called a soil suspension. Sedimentation refers to the settling rates of the dispersed particles in water, which is a function of particle size and is governed by Stoke’s law.

11 - 14 (4 Pages)
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4 Determination of Soil Bulk Density

Purpose The bulk density varies indirectly with total pore space present in the soil and gives a good estimate of porosity of soil. Bulk density is of great importance than particle density in understanding the physical condition of soil. Soil bulk density is defined as the ratio of the mass of the oven dry soil to its bulk volume. Method of determination Different methods are available for bulk density determination which differ how the soil sample is obtained and its volume is determined such as core, clod and excavation methods. There are other methods for the determination of bulk density where different principles are employed, for example, radiation method. Commonly used methods are weighing bottle, core and clod method.

15 - 18 (4 Pages)
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5 Determination of Soil Particle Density

Particle density determination is based on the measurements of weight of solids and their volume. The weight of solids is obtained by weighing a sample of oven dried soil. The volume of solids is determined is determined by immersion. The method outlined here is “Pycnometer method”. Principle A given amount of dry soil when immerses in a definitive volume of water, expels air and results in the displacement of equal volume of water. The volume of soil particles is determined by measuring the volume of water displaced in the pycnometer bottle.

19 - 20 (2 Pages)
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6 Determination of Water Holding Capacity in Soil

Purpose The determination of water holding capacity in soils is important as it gives an idea of the capacity of soil to hold water for the use by crops. The light soils which do not hold such water require more frequent irrigations than heavy clay soils; well decomposed organic matter increases the water holding capacity. Exchangeable sodium and type of clay mineral also have a marked effect on water holding capacity. Water holding capacity of soils is useful for selection of soils for irrigability classification. It also helps for comparing other properties of soils.

21 - 22 (2 Pages)
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7 Determination of Water Stable Aggregates of Soil by Wet Sieving Method

Soil aggregates refers to a group of two or more primary particles which cohere to each other more strongly than surrounding particles. Under field condition, all such units also cohere to some degree with neighboring aggregates and form larger aggregates. Such aggregates form and break easily into smaller aggregates during tillage and by disruptive action of water and air. The aggregates maintaining their identity are those in which the cohesive forces among particles are greater than the disruptive forces. A quantitative characterization of aggregates is done by determining aggregate stability and size distribution of aggregates. The aggregate stability refers to the resistance of soil aggregates to breakdown by water, air and mechanical manipulations. The soil aggregates which can stand the disruptive forces of wetting by water are known as water stable aggregates. Therefore, the process of wetting, disruption of dry aggregates and screening of aggregates of different sizes should reasonably compare to the disruptive action of water and mechanical forces of tillage under wet conditions. The vacuum wetting of dry soil largely simulates the process of soil wetting in the surface layers but the immersion wetting is more comparable to the wetting of surface soil by irrigation. Similarly, sieving under water compares more closely with the disruptive action of water and other mechanical forces. The mean weight diameter (MWD) of water stable aggregates is a useful index to characterize the change in structure due to tillage. The mean weight diameter can be calculated using following equation.

23 - 26 (4 Pages)
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8 Determination of Soil Organic Carbon

Soil Organic Matter (SOM) is the seat of nitrogen in soil and its determination is often carried out as an index of nitrogen availability. The top soil (surface soil) range from 0.5% to 3.0% organic carbon for most upland soils and less than 0.5% are limited to desert soils. Soil organic matter averages about 58% carbon, it follows that soils generally range from about 2 to 6 % organic matter (% O.M. = %C x 1.724, The factor 1.724 = 100/58). There is also a close relationship between carbon and nitrogen in soils. Most organic matter average about 5% nitrogen so that the N: C ratio is 1:11.6. Therefore by multiplying the soil organic matter percentage by 0.05 an approximate value for the soil nitrogen, percentage is obtained. In soil the chief source of some of the nutrients essential for plant growth is organic matter, such nutrients are N, S and boron is also largely derived from organic matter.

27 - 28 (2 Pages)
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9 Determination of Available Nitrogen in Soil

The major part of soil nitrogen exists in complex combination in the organic compounds. It becomes available to plants after breakdown to simple form followed by mineralization. The chemical methods for determination of soil nitrogen availability involve either direct or indirect of total nitrogen or measurement of a fraction of easily hydrosable nitrogen by employing solution of dilute acid or alkali. Distillation of alkaline potassium permanganate solution has often been adopted for estimating the ox disable and reactive form of soil nitrogen. The available nitrogen in soil is determined by alkaline permanganate method as per procedure suggested by Subbiah and Asija (1956). Principle A known weight of the soil is mixed with alkaline potassium permanganate (KMnO4) solution and distilled. The organic matter present in soil is oxidized by the nascent oxygen, liberated by potassium permanganate, in the presence of sodium hydroxide and the released ammonia is condensed and absorbed in known volume of a boric acid with mix indicator to form ammonium borate, the excess of which is titrated with a standard sulphuric acid.

29 - 32 (4 Pages)
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10 Determination of Available Phosphorous in Soil

The term available phosphorus (P) refers to the inorganic form, occurring in soil solution, which is almost exclusively ‘orthophosphate’. The available P is considered to be a fairly good indicator/measure of the P supplying capacity of a soil. A knowledge of available P content of soils is important for determining its critical limit , based on soil-test-crop response calibration study. Principle In soil, phosphorus exists in the form of various types of orthophosphates. A very small fraction of these is available to plants at a given time. Available phosphorus content of soil consists mainly of Ca-P, Al-P and Fe-P. In the neutral and alkaline soils particularly, Ca-P is the dominant fraction. Organic –P fraction is also considerable amount, but is usually not include in the determination of available phosphorus. A large number of extractions, buffer solutions, acids and chelating agents have been suggested for available phosphorus from time to time. However, no single extractant appears to be suitable for all types of soils. Two types of extraction methods are more popularly adopted. Under acidic soil conditions, Bray No.1, which involves soil extraction with a solution consisting of 0.003 N NH4F and 0.025 N HCl is widely followed. The fluoride complexes Al and Fe in soil, thus releasing some bound p besides the easily acid soluble P (largely Ca-P). This extraction is suitable for soils containing less than 2% calcite or dolomite because in calcareous soils, carbonates quickly neutralize the acid, resulting in less extraction of P.

33 - 38 (6 Pages)
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11 Determination of Available Potassium in Soil

The total potassium content (K) of a soil varies from 0.05 to 2.5%. The total K is distributed in mineral form (90-98%), fixed non-exchangeable (1-10%) and exchangeable plus water soluble K(1-2). Exchangeable K represents an average of 2-15% of the sum of exchangeable bases and 1-3% of the total capacity of cationic exchange. Principle It is based on the principle of the equilibrium of the soils with an exchangeable cation mode of the solution of neutral ammonium acetate, in a given soil:solution ratio. During the equilibrium, ammonium ions exchange with the exchangeable K ions of soil.The K content in the equilibrium solution is estimated with a flame photometer.

39 - 40 (2 Pages)
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12 Determination of Available Sulphur in Soil

Sulphur (S) occurs in different forms in soil viz., sulphites, sulphates , sulphides and in organic compounds. Plants absorb S in the form of sulphate(SO4 2-) . The organic forms of S compounds become assimilable, especially following microbiological transformation into SO4 2-. The mineralization of organic sulphur in a soil depends primarily upon the N:S ratio and any SO4 2- formed may be fixed against extraction, particularly if much Fe and Ba is present or if soil is very acidic. Principle Beside some amount in the soil solution, available sulphur in mineral soils occurs mainly as adsorbed SO4 2- ions. Both CaCl2 and phosphate solutions (as monocalcium phosphate) are generally used for replacement of the adsorbed SO4 2- ions. Use of Ca salts have a distinct advantage over those of Na or Na, as Ca prevents deflocculating in heavy textured soils and leads to easy filtration. SO4 2- in the extract can be estimated turbid metrically using a spectrophotometer. Sulphur in the extract can also be measured by colorimetric method using barium chromate but the turbimertic method given below is mainly used in the soil testing laboratories.

41 - 44 (4 Pages)
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13 Determination of Extractable Calcium Carbonate in Soil

Carbonate is a natural constituent of many soils occurring as sparingly soluble, alkaline earth carbonate, chiefly as calcite and dolomite. Most carbonate minerals found in local soils are calcite and account 90% of total soil carbonates. The determination of total carbonate such as CaCO3in soil is of great interest on account of high useful ess for diagnosing soil status in terms of structure, texture, biological activity or nutrient content. In calcareous soils carbonates exert a major influence on the chemical properties. Also carbonate content is used as a differentiating criterion for some classes at the family level of soil taxonomy. Principle A qualitative rapid test for free calcium carbonate is made by adding 10 mL of diluted HCl(1:3) to about 5 g of air dry soil on a watch glass and observing the intensity of effervescence which results from the evolution of CO Based on the . degree of effervescence the amount of calcium carbonate present in the soil can be broadly categorized into “traces or negligible, low, medium, high and very high”. Soils having traces to low amounts of calcium carbonate do not pose any problem. But those showing medium to very high degree of effervescence, a separate quantitative analysis should be carried out using Puri’s rapid titration method.

45 - 46 (2 Pages)
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14 Determination of Extractable Calcium and Magnesium in Soil

Calcium (Ca) and magnesium (Mg) are the two most abundant alkaline earth cations in soils. They both occur as soluble ions in soil solution, exchangeable, non-exchangeable and in organic material. Soils from arid regions are richer in Ca (1-2% CaO), while those from humid zones have a low content (0.01-0.02% CaO). On the other hand exchangeable Mg is found in very small quantities in calcareous soils. Sometimes, in acid soils, Mg2+ represents the largest quantity of the sum of exchangeable bases. Principle The method is based on the principle that calcium, magnesium and a number of other cations form stable complexes with versenate (ethylendiaminetetraacetic acid disodium salt, EDTA) at different pH. A known volume of standard calcium solution is titrated with standard 0.01N EDTA solution using murexide (ammonium purpurate) indicator in the presence of NaOH solution. The end point is a change of color from orange red to purple at pH 12 when the whole of Ca forms a complex with EDTA. Calcium plus Mg are also present in the solution and can be titrated with 0.01N EDTA using buffer solution and a few drops Eriochrome Black T indicator. The end point is a change of color from red to blue at pH 10. Beyond pH 10, magnesium is not bound strongly to Erichrome Black-T indicator to give a distinct end point.

47 - 50 (4 Pages)
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15 Determination of Carbonate and Bicarbonate in Soil

Principle Carbonate (CO3) and bicarbonate(HCO3) ions are species of the same acid, carbonic acid. Their proportionate content is a function of pH. The CO3 starts to form as pH rises above 8.4. Carbonate and bicarbonate are generally determined in soil saturation extract by titration with 0.01 N H2SO4 to pH 8.3 and 4.5, respectively. Apparatus Required Burette, pipette, conical flask and mechanical shaker etc

51 - 52 (2 Pages)
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16 Determination of Available Chloride in Soil

Soluble chloride (Cl) concentration in the extract is determined by silver nitrate titration. This method quantifies the concentration of Cl (meq/L) in the saturation paste extract. Chloride may be determined using anion selective electrode (potentiometric). Plant tolerance to Cl can be related to its concentration in the soil saturation paste extract. The method detection limit is approximately 0.1 meq/L, dependent on the method of analysis, and is generally reproducible within ± 10 %. Apparatus Required Burette, pipette, conical flask and mechanical shaker etc

53 - 54 (2 Pages)
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17 Determination of Micronutrients in Soil by Atomic Absorption Spectrophotometer

All atoms can absorb light at certain discrete wavelengths corresponding to the energy requirement of the particular atom. When at ground state the atom absorbs light it is transformed into the excited state. It is the same atom containing more energy. This energy is measured in relation to the ground state and a particular excited state say for example in case of Na may be 2.2 eV (electron volts) above the ground state. Each transition between different electronic energy states is characterized by a different energy and by a different wavelength. These wavelengths are sharply defined and when a range of wavelengths is surveyed, each wavelength shows as a sharp energy maximum (a spectronic line). These characteristic lines distinguish atomic spectra. The lines, which originate in the ground state of atom, are most often of interest in atomic absorption spectroscopy. These are called the resonance lines. The atomic spectrum, characteristic of each element, then comprises a number of discrete lines, some of which are resonance lines. Most of the other lines arise from excited states rather than the ground state. The lines of excited states are not useful generally in atomic absorption analysis as most of the atoms in a practical atomizer are found in the ground state.

55 - 60 (6 Pages)
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18 Determination of Available Boron in Soil

Boron occurs as anion in soils and isrequired by plants in very small quantity. Water soluble B makes the estimate of its availability to plants. Total boron in soils varies from 20 to 200 mg kg-1 and available (water soluble) boron in soils ranges from 0.03 to 12 mg kg-1 respectively. The threshold value ranging from 0.1 to 0.5 mg kg-1 (water soluble B) depends upon the soil type, crops, and other factors, below which the response to applied boron may be expected. Its availability is affected by soil pH as under:

61 - 64 (4 Pages)
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19 Pesticide Residue Analysis: Overview

A pesticides residue is any substance or mixture of substances in food, agricultural commodities or animal feed resulting from the use of pesticides and includes any specified derivatives such as degradation products and impurities that are considered to be of toxicological significance. Pesticide residue analysis (PRA) may be defined as the quantitative and qualitative analyses of the representative samples drawn from agricultural field, market and environment for pesticides and their toxic metabolites.

65 - 68 (4 Pages)
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20 Instrumentation- Gas Chromatography (GC, GC-MS & GC-MS/MS)

Chromatography is a physical method of separation in which components to be separated is distributed between two phases, one of which is stationary while other moves in a definite direction. By separating the sample into individual components, it is easier to identify (qualitative) and measure the amount (quantitative) of the various sample components. There are numerous chromatographic techniques and corresponding instruments. Gas Liquid Chromatography (GLC) is the most widely used analytical technique for estimation of volatile and thermo stable type of pesticides with speed, accuracy, reproducibility and sensitivity.

69 - 72 (4 Pages)
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21 Instrumentation High Performance Liquid Chromatography (HPLC)

Although Gas Liquid Chromatography (GLC) is widely used technique for pesticide residue analysis, it has some limitations. It can analyze of volatile and thermo stable type of pesticides only because it operate at high temperature. These problems have overcome in HPLC. Although HPLC can analyze both polar as well as non-polar type of compounds but it has less sensitivity than GLC.

73 - 76 (4 Pages)
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22 Pesticide Residue Analysis in Green Fodder

Principle Acetone is used for extraction the most nonionic pesticide residue, and residue are partitioned from acetone to dichloromethane/hexane phase. After removing traces dichloromethane, final extract is made up with acetone. This extract can be determined by GC with selective detectors. Further for organochlorine and synthetic pyrethroids extract should be cleaned up using florisil column. And for determination organophosphate extract should undergo to charcoal-celite cleanup. For the determination carbamates, the extract is subjected to C-18 solid phase cartridge clean up.

77 - 80 (4 Pages)
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23 Pesticide Residue in Dry Fodder

Principle: Acetone is used for extraction the most nonionic pesticide residue, and residue are partitioned from acetone to dichloromethane/hexane phase. After removing traces dichloromethane, final extract is made up with acetone. This extract can be determined by GC with selective detectors FPD-P/NPD without cleanup. Further for organochlorine and synthetic pyrethroids extract should be cleaned up using florisil column. And for determination organophosphate extract should undergo to charcoal-celite cleanup.

81 - 84 (4 Pages)
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24 Pesticide Residue Analysis in Soil

Principle Pesticide residues are extracted from soil using a mixture of acetone/water in a soxhlet apparatus for 7-8 hours. This extract can be determined directly by GLC. Scope: This method is suitable for most OPs, OCs, SPs, and herbicides residue analysis.

85 - 86 (2 Pages)
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25 Pesticide Residue Analysis in Milk

Principle Pesticide residues in milk are derived from the intake of pesticide contaminated feed and fodder. Scope This method is suitable for most OPs, OCs, SPs, and herbicides residue analysis.

87 - 88 (2 Pages)
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26 Pesticide Residue Analysis from Concentrated Animal Feed

Scope This method is suitable for most OPs, OCs, SPs, and herbicides residue analysis. Apparatus required Homogenizer Centrifuge Nitrogen evaporator

89 - 92 (4 Pages)
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27 End Pages

Appendices Appendix I: Molecular and equivalent weight of some important compounds Appendix II: Percentage concentration, specific gravity, normality and amount needed for making 1N solution of some commonly used acids Appendix III: some important conversion factors Appendix IV: Common terms used in pesticide residue analysis Appendix V: Classification of pesticides according to toxicity, expressed as LD50 (mg/kg) Appendix VI: Chemical classification of pesticides

 
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