A new soil test method for the determination of plant‐available cadmium in soils

Abstract

A new soil test procedure using 1M NH₄Cl was developed for the extraction of plant‐available cadmium (Cd) from soils. Five grams of soil is weighed into a 50‐mL polyethylene vial to which 30 mL of 1M NH₄Cl solution is added. The soil suspension is then shaken on a horizontal shaker for 16 h at 25°C at 180 cycles per min. The suspension is then centrifuged at 2,500g for 5 min and the supernatant filtered through a 0.45 μm nitrocellulose filter under vacuum. Cadmium in the extract is then determined at 228.8 nm on a graphite furnace equipped atomic absorption spectrophotometer. A highly significant correlation was observed between the natural logarithm (In) of 1M NH₄Cl‐extractable Cd in soils and the Cd content in the grain of durum wheat (Triticum turgidum var. durutn L.) grown on the same soils (r = 0.974, p = 3.8 x 10^‐7). In comparison with several commonly used extradants, such as ABDTPA, CaCl₂, NH₄OAc, and NH₄NO₃, the 1M NH₄Cl‐extracted Cd from soils was found to be a better index of Cd availability.     

Evaluation of methods for nitrogen‐15 analysis of inorganic nitrogen in soil extracts: I. Steam‐distillation methods

Abstract

A study was conducted to evaluate conventional steam‐distillation techniques for N‐isotope analysis of inorganic forms of N in soil extracts. Extracts obtained with 2 M KCl from 10 diverse soils were treated with: (i) (¹⁵NH₄)₂SO₄ and KNO₃, (ii) (NH₄)₂SO₄ and K¹⁵NO₃, or (iii) KNO₃and Na¹⁵NO₂. Steam distillations were performed sequentially to determine NH₄ ⁺‐N and NO₃ ^‐‐N, and were also carried out to determine (NO₃ ^‐ + NO₂ ^‐)‐N or (NH₄ ⁺ + NO₃ ^‐ + NO₂ ^‐)‐N; a pretreatment with sulfamic acid was used to determine NO₃ ^‐‐N in the presence of NO₂ ^‐‐N. Recovery of added N ranged from 95 to 102%. Significant isotopic contamination was observed in sequential distillation of unlabeled NO₃ ^‐‐N following labeled NH₄ ⁺‐N; otherwise, analyses for ¹⁵N were usually within 1% of the values calculated by isotope‐dilution equations.     

Sodium bicarbonate‐DTPA test for macro‐and micronutrient elements in soils

Abstract

Individual soil tests are used to assess plant nutrient element needs. Separate soil tests, however, are time consuming and costly. Our objective was to develop a 0.5M sodium bicarbonate (NaHCO₃) soil phosphorus (P) test in combination with 0.005M diethylenetriaminepentaacetic acid (DTPA) so macronutrient dements: ammonium‐nitrogen (NH₄‐N), nitrate‐nitrogen (NO₃‐N), P, potassium (K), calcium (Ca), and magnesium (Mg); and micronutrients: iron (Fe), manganese (Mn), zinc (Zn), and copper (Cu) could be quantified in one extraction. The NaHCO₃‐DTPA extracting solution is a combination of 0.5M NaHCO₃ and 0.005M DTPA and has a pH of 7.60±0.05. Sodium in the solution enhances the NH₄, K, Ca, and Mg extraction; bicarbonate (HCO₃) is for P extraction; DTPA chelates Ca, Mg, and micronutrients; and the water is for NO₃ extraction. Soil samples (0–15 cm depth) came from two sources. The first set was from 12 N x P dryland proso millet (Panicum miliaceum L.) experiments, conducted from 1985 through 1987 in eastern Colorado. These soils were extracted with potassium chloride (KCl), NaHCO₃, ammonium acetate (CH₃‐COONH₄), DTPA, ammonium bicarbonate DTPA (AB‐DTPA), and with the NaHCO₃‐DTPA solutions. The second set included 25 soils from Alabama, Georgia, North Carolina, and South Carolina and were analyzed only for available P with the NaHCO₃ and NaHCO₃‐DTPA methods. Simple linear correlations for macronutrient elements and micronutrients were highly significant. Critical levels for the macronutrient elements: NO₃‐N, P, and K were 27, 11, and 144 mg kg^‐1, respectively; and the critical levels for the micronutrients: Fe, Mn, Zn, and Cu were 3.9, 0.35, 0.97, and 0.24 mg kg^‐1, respectively.     

Mehlich‐I soil‐test calibration for watermelon: Cu,Zn, and Mn

Abstract

Predictive soil tests were used to detect possible need for Cu, Zn, and Mn fertilizers for the optimum production of watermelons (Citrullus lanatus (Thumb.) Masf.) in north and central Florida. Predictive Mehlich‐I soil testing indicated a possible response to additions of Mn and Cu but not to additions of Zn at three locations: Gainesville, Dunnellon, and Live Oak. Results showed no total marketable yield response to selected Cu, Zn, and Mn treatments at any of the three sites. Yields for the Gainesville, Dunnellon, and Live Oak sites were 41.5, 29.0, and 38.0 Mg/ha, respectively, well above the state average watermelon yield of 19.0 Mg/ha. Tissue analyses at the Gainesville and Live Oak sites showed Cu, Zn, and Mn levels within or above suggested sufficiency ranges. This study indicates that current University of Florida interpretations for the Mehlich‐I extractant can identify sites with adequate extractable Cu, Zn, and Mn levels, thus avoiding unnecessary fertilization. At no time were University of Florida Cu, Zn, or Mn interpretations and recommendations found to be limiting for watermelon production.     

Evaluation of some soils in South‐Western Nigeria for arable crop production

Abstract

Five representative soil profiles were excavated and examined along a toposequence at different physiographic points in Itagunmodi area of Southwestern Nigeria. The soil series identified were Ibule, Ijare, Owena, Itagunmodi, and Adio. The soils were characterized with physical, chemical, and mineralogical analyses. Ibule series was not suitable for yam and cassava production. Ijare series was marginally suitable for yam, maize, lowland rice, and cassava production. Owena and Itagunmodi series were highly suitable for yam, maize, and cassava production. However, the latter two series were moderately suitable for lowland rice. Adio series was only suitable for lowland rice production.     

Evaluation of N‐butyl phosphorothioic triamide for retardation of urea hydrolysis in soil

Abstract

Work reported showed that N‐butyl phosphorothioic triamide (NBPT) is considerably more effective than phenylphosphorodiamidate (PPD) as a soil urease inhibitor and merits consideration as a fertilizer amendment for retarding hydrolysis of urea fertilizer in soil. Studies to determine the factors influencing the effectiveness of NBPT for retardation of urea hydrolysis in soil showed that the inhibitory effect of NBPT on hydrolysis of urea by soil urease increased markedly with the amount of NBPT added and decreased markedly with time and with increase in temperature from 10 to 40°C. They also showed that the ability of NBPT to retard urea hydrolysis in 13 surface soils selected to obtain a wide range in properties was significantly correlated with organic C content (r = ‐0.70**), total N content (r = ‐0.76**), cation‐exchange capacity (r = ‐0.67* ), sand content (r = 0.61*), clay content (r = ‐0.63*), and surface area (r = ‐0.66*), but was not significantly correlated with pH, silt content, urease activity, or CaCO₃ equivalent. Multiple‐regression analyses indicated that the effectiveness of NBPT for retardation of urea hydrolysis in soil tends to increase with decrease in soil organic‐matter content.     

Evaluation of methods for determining sulphur‐35 and sulphur‐32 in the same trapping solution of Johnson and Nishita method

Abstract

A laboratory study was conducted to investigate whether the Zn‐Na acetate solution, used for trapping H₂S in the Johnson‐Nishita method (1952), could be used to quantitatively determine ³⁵S and ³²S in the same trapping solution, as the Zn‐Na acetate solution allows more sensitive S determination using methylene blue than does the bismuth sulphide colour development of H₂S trapped in NaOH solution. Results obtained using the Zn‐Na acetate solution were variable compared with those obtained from the normal procedure of using NaOH as the H₂S trapping solution, indicating that the Zn‐Na acetate solution was unsuitable, probably because of the rapid transformation of H₂S to water‐insoluble ZnS.

The applicability of methylene blue development for H₂S trapped in NaOH solution was also investigated. Results showed that ³²S could be determined quantitatively provided methylene blue colour development was conducted less than 30 minutes after the removal of H₂S‐trapping NaOH solution from the Johnson‐Nishita digestion‐distillation unit. A delay of more than 30 minutes caused a significant linear reduction (R² = 0.86 ‐ 0.92***) in methylene blue colour, indicating that H₂S in NaOH solution was readity: oxidized to other S forms which did not undergo methylene blue development.

Toluene and dioxane were compared as liquid scintillants for assaying ³⁵S activity trapped as H₂S in either NaOH or Zn‐Na acetate solution before and after methylene blue development. Before colour development, toluene improved the counting efficiency of ³⁵S in NaOH solution by 23 to 27%. After colour development, toluene improved the counting efficiency of both NaOH and Zn‐Na acetate solutions.     

Mobile Si-rich compounds in the soil–plant system and methods for their determination

Different aspects of Si biogeochemistry in the soil have been reviewed. Interaction mechanisms of monosilicic acid with aluminum, phosphorus, and heavy metal compounds have been generalized. Polysilicic acids are chemically inert substances, but they participate in the formation of soil structure. Organosilicon compounds in the soil are very little investigated. From literature and our own data, the cycle of mobile Si forms in the soil–microorganism–plant system has been suggested, which shows the main fluxes of soluble Si migration and transformation. A new classification of the Si compounds based on their physicochemical and biological activities in the soil has been suggested as well as a method for the determination of mono- and polysilicic acids in the soil matrix.     

Evaluation of an anion‐exchange membrane for extracting plant available phosphorus in soils

Abstract

Anion‐exchange resins (AER) have been used to determine plant available phosphorus (P) since the fifties and their results have shown strong relationships with plant growth and P uptake irrespective of soil properties. However, this procedure is still not widely used by laboratories because of difficulties in handling resin beads under routine conditions. New kinds and different shapes of resins are being produced each with specific characteristics that must be evaluated before use in laboratory procedures. Thus the objective of this work was to evaluate an AER manufactured in membranes reinforced with a Modacrylic fabric. These anion‐exchange membrane (AEM) sheets are commercially available, making them suitable for soil testing. The membranes were cut in pieces (1.0×7.5 cm) identified as AEM‐strips. The AEM‐strips were soaked in 0.5M HCl for a few days and transferred, after being rinsed with deionized water (DI), to 0.5M NaHCO₃ to convert them to HCO₃ ^‐ form. The AEM‐strips and resin beads in nylon bags recovered 98.4 and 98.0% of the P content in an aqueous P solution, respectively. Three eluent solutions were evaluated with different shaking times. The 0.1M H₂SO₄ and 1.0M NaCl in 0.1M HCl were equally suitable for the molybdenum blue color development without any pH adjustment, while the pH of the 0.5M HCl was too low. The elution of P from the AEM‐strips was independent of time with a 15‐min shaking being adequate for removal of all P from the strips. A comparison of soil sample preparation demonstrated that it was not necessary to vigorously grind or sieve the soil to improve the repeatability of the results. The AEM‐strips were compared with other methods (Pi impregnated filter paper, Mehlich I and Bray 1) using 32 soils from Guatemala with widely varying physico‐chemical and mineralogical properties. Phosphorus extracted by the AEM and Pi procedures (similar principle) were highly correlated and gave similar results irrespective of soil type. The acid extraction (Mehlich I and Bray 1 methods) attacked soil components (apatites) resulting in higher and inconsistent amounts of P extracted which may not be available to plants; the correlation between these methods within soils of similar properties was good, but when all soils were considered together the relationship was not significant. This demonstrated that the acid extraction method for P is not suitable for soils containing apatites, while those based on a sink for P (AEM and Pi) can be applied irrespective of the type of soil.     

Application of soil amendments to contaminated soils for heavy metal immobilization and improved soil quality—a critical review

ABSTRACT

Today, soil metal pollution has become a significant environmental issue of great public concern. This is because soil is both a major sink for heavy metal(loid)s (HMs) released into the environment, by both pedogenic and anthropogenic activities; and also a major source of food chain contamination mainly through plant uptake and animal transfer. In addition, HM contamination of soil leads to negative impacts on soil characteristics and function by disturbing both soil biological and physiochemical properties (e.g. extreme soil pH, poor soil structure and soil fertility and lack of soil microbial activity). This eventually leads to decreased crop production. Various soil remediation techniques have been successfully employed to reduce the risks associated with HMs efflux into soil. Among these, the use of low-cost and environmentally safe inorganic and organic amendments for the in-situ immobilization of HMs has become increasingly popular. Immobilization agents have successfully reduced the availability of metal ions through a variety of adsorption, complexation, precipitation, and redox reactions. Soil amendments can also be a source of nutrients and thus can also act as a soil conditioner, improving the soil’s physiochemical properties and fertility, resulting in enhanced plant establishment in metal contaminated soils. This article critically reviews the use of immobilizing agents in HM contaminated agricultural and mining soils paying particular attention to metal immobilization chemistry and the effects of soil amendments on common soil quality parameters.     

Evaluation of the NH4HCO3‐DTPA soil test for assessing boron availability to wheat

Abstract

The NH₄HCO₃‐DTPA (AB‐DTPA), 1 MNH₄HCO₃, 0.005 M DTPA, pH=7.6, was proposed as a multi‐element extractant, for evaluating macro and micronutrients availability to plants. AB‐DTPA was also evaluated as a soil test, for assessing boron availability and toxicity to alfalfa. In a pot experiment, ten soils of Northern Greece were used to assess AB‐DTPA as an extractant of available boron to wheat (Triticum aestivum L., cv. Yecora), in comparison with hot water and saturation extract. Boron (B) was added as borax (Na₂B₄O₇*10H₂O) to the ten soils, at rates equal to 0, 3, and 5 mg B kg^‐1. Wheat was grown in pots containing the boron amended soils to the stage of tillering, and dry aboveground biomass, B concentration and B uptake by wheat were determined. AB‐DTPA extractable B was significantly greater than saturation extract and similar to hot water at each B application rate, and was correlated significantly with hot water (r=0.84), or with saturation extract (r=0.48). Extractable boron by all extractants, boron concentration in wheat and boron uptake were significantly affected by the soil x B application rate interaction. In assessing B availability to wheat using AB‐DTPA as a soil test, CEC should be included in the regression equation for B concentration, or pH for B uptake. However, the corresponding adjusted coefficients of determination for B concentration (adjusted R²=0.46) and B uptake (adjusted R²=0.48) were similar or lower to those of hot water (adjusted R²=0.45 and 0.60, respectively) and the saturation extract (adjusted R²=0.70 and 0.49, respectively), when the latter two soil tests were used in the regression equations without the inclusion of any soil property.     

Evaluation of microplate and bench-scale β-glucosidase assays for reproducibility, comparability, kinetics, and homogenization methods in two soils

Enzyme assays that use fluorescently labeled substrates and microplate formats have been incorporated into laboratory protocols to improve sensitivity and reduce the time and labor involved in traditional bench-scale analyses. Microplate protocols vary, and the methods have not been evaluated systematically for comparability and reproducibility. In this study, p-nitrophenol (pNP)-based and 4-methylumbelliferone (MUF)-based microplate methods for estimating β-glucosidase activity were compared in two soils with different properties. Microplate method reproducibility was evaluated in replicate soil suspensions, and Michaelis–Menten kinetics for the microplate assays were compared to those of a standard pNP bench-scale assay. The effect of soil sample sonication on reproducibility was determined for the MUF microplate method. The MUF microplate method was reproducible in five replicate soil suspensions, but the pNP microplate method showed greater variability. The K _m Michaelis–Menten constant was significantly different in the microplate methods compared to the bench method. Enzyme activities measured by the MUF and bench methods were comparable, but the pNP microplate method resulted in more variable measurements and was less sensitive in the soils studied. Sonication of soil at an intensity of 15 W ml^?1 resulted in higher (MUF) measurements, but greater variability. The effects of high background absorbance on the reproducibility, sensitivity, and accuracy of the pNP microplate method do not support this method as a substitute for the standard bench method. A robust comparison study of the MUF microplate method across laboratories is recommended to further validate its use in comparative analyses.     

Mehlich‐1‐ and DTPA‐extractable lead in soils in relation to soil properties

Abstract

Mehlich‐1 and DTPA extractants are frequently used to predict metal availability in soils. Metal extractability by the acid or chelate extractant reflects the metal characteristics and metal‐soil interactions. In this study, samples of eight topsoils from the southeastern United States were incubated with added lead (Pb) at the rate of 40 mg#lbkg^‐1. After five months in the greenhouse, Mehlich‐1 and DTPA extractants were employed to extract Pb in both metal‐amended and natural soils. For the natural soils, Pb concentration in the DTPA extractant was always higher than that in the Mehlich‐1 extractant. This indicates that the DTPA chelate extractant is able to dissolve some Pb in soils which is not solubilized by protons. The negative correlation found between Mehlich‐1‐extractable Pb and soil clay content might result from two mechanisms: i) strong association between Pb and soil surfaces, or ii) readsorption of Pb during extraction. None of the correlations between DTPA‐extractable Pb and soil properties was significant, suggesting that the DTPA‐extractable Pb is not heavily dependent on soil properties. The DTPA extractant showed a high ability to solubilize Pb in the natural soils possibly due to a high affinity of Pb for soil organic matter.     

A computer‐assisted method for CEC estimation and quality control in a routine soil‐test operation

Abstract

Cation‐exchange capacity (CEC) of 30 Alabama soils was estimated by two different methods based or routine soil‐test results consisting of soil‐water pH, Adams‐Evans buffer pH, and Mehlich‐1 extractable cations (K, Mg, and Ca), which were obtained automatically by a computerized data acquisition system. In one method, CEC was calculated by solving a quadratic equation involving soil‐water and buffer pH's; in the other, CEC was estimated as the summation of extractable cations and exchangeable acidity. The two estimated CEC's agreed well with each other and also had the same magnitude as CEC determined by the normal NaOAc, pH 8.2 method. By averaging the two calculated values, an even closer estimation of the measured CEC was found. These calculations and comparisons can be accomplished quickly and efficiently by a minicomputer via a simple FORTRAN program.

In addition, a discrepancy between the two estimated CEC's would indicate possible errors in analytical determinations and/or the inadequacy of the soil testing procedures. Therefore, an additional means for quality control in a routine soil‐test operation can be obtained by comparing the two CEC values.     

A quick‐test procedure for soil and plant tissue nitrates using test strips and a hand‐held reflectometer

Abstract

Development of a nitrate quick‐test for use by fanners or field consultants would likely encourage the use of plant tissue and soil nitrate tests as a means to improve nitrogen management. To evaluate a quick‐test method, nitrate concentrations in plant tissue and soils were measured using commercially available nitrate test strips and a hand‐held reflectometer. The results were compared with those obtained with standard laboratory methods. Test strip accuracy and precision and reflectometer precision were determined over a 10 day period using standard KNO₃solutions and colored paper strips. Coefficients of variation ranged from 22.4 to 9.5 percent for the test strips and from 3.5 to 1.6 percent for the reflectometer. Quick‐test results were highly correlated with laboratory results for both plant tissue nitrate (r=0.87) and soil nitrate (r=0.98) concentrations. Results indicated that test strips provide a rapid, reasonably accurate and precise method to determine nitrate concentrations in both soil and plant material     

Spatial variation of soil test phosphorus and potassium,oxalate‐extractable iron and aluminum,phosphorus‐retention index,and organic carbon content in soils of Western Australia

Abstract

Spatial variation of bicarbonate soil test phosphorus (P) and bicarbonate soil test potassium (K) was studied by measuring soil test values for 40 individual soil samples collected from random locations within eight uniform 100 m by 100 m field sites in south‐western Australia. In addition, for five of the sites, spatial variation of the three P sorption indices (ammonium oxalate extractable iron, ammonium oxalate extractable aluminum, and the P retention index) and of organic carbon (C) was measured for 20 individual soils samples. Spatial variation was found to be large, with coefficient of variation (CV) exceeding 20% in most cases, and 50% in some cases. It is therefore essential to collect an adequate number of soil samples from uniform areas in paddocks in order to provide a representative composite sample to measure the soil properties.     

Amelioration of saline‐sodic soils with organic matter and their use for wheat growth

Abstract

Few reports highlight the effect of organic matter in improving the properties of saline soils. A laboratory study was conducted to determine the effect of adding farm yard manure (manure), Egyptian clover hay (clover hay), and wheat straw, at 1 and 3% of soil weight on water stability of soil aggregates (WSA), water‐holding capacity (WHC), pH, and electrical conductivity of soil extract (ECe) of a normal, saline, and saline sodic soil. After 90 and 180 days, WSA and WHC increased, while pH and ECe decreased. Soil properties improved most by adding 3% manure to all the soils. Wheat grown in these soils indicated significant differences for various growth and yield variables, especially the root growth, number and area of green leaves, and grain yield. Organic matter added to these soils increased WSA and WHC and decreased pH and Ece. The WHC had no correlation with pH, but was negatively correlated with Ece. Increased WSA caused the leaching of excess ions and reduced their toxicity, while enhanced WHC increased the availability of water to the roots and promoted growth. It is concluded that manure ameliorated salt affected soils and promoted wheat growth better than clover hay and wheat straw.     

Comparison of two methods of sample preparation for determination by atomic absorption spectro‐photometry of heavy metals in soils and sediments

Abstract

Two commonly used methods of dissolution of heavy metals in soils and sediments for atomic absorption spectrophotomety (AAS) determination were compared. Dry ashing and subsequent dissolution with 3 N HCl in a block digestor was shown to give a better estimate of the aqua regia‐soluble fraction than wet ash digestion with a mixture of HNO₃ and HClO₄ acids using reference materials. But both methods extracted significantly less than the certified total contents of most metals.

In soils and sediments from SW Spain, the amounts extracted by the block heater method were generally greater than those obtained by wet ash digestion. In agricultural soils, highly significant differences were found between the amounts of Fe, Cu, and Zn extracted by both methods, but the significance decreases if both methods are used on soils or sediments from mining areas where metal contents are likely to be from recent deposits.     

Adsorption‐desorption of zinc in mollisols and their relationship with uptake of fertilizer‐applied zinc by rice

Abstract

Zinc (Zn) adsorption in mollisols conformed to the linear form of Freundlich equation. The log K values were positively correlated with silt, clay, and carbonate contents and soil pH, but negatively correlated with sand content. Sequential desorption of adsorbed Zn in 0.05M Ca(NO₃)₂, 0.1M Mg(NO₃)₂, 0.005M DTPA, and 0.1M HCl revealed that weakly and specifically bound fractions of added Zn, which could easily equilibrate with soil solution, were low and decreased with silt and carbonate contents and soil pH. Weakly bound fraction increased with sand content. Strongly bound and complexed fraction of applied Zn was the maximum and increased with clay, soil organic carbon and carbonate contents and specific surface area, but decreased with sand content. The mineral bound fraction of applied Zn was intermediate and increased with silt, clay and carbonate contents, and soil pH and specific surface area. Zinc uptake due to added Zn fertilizer by rice crop (Y) negatively correlated with log K, but positively related to Zn content in the equilibrium soil extract and Zn desorbed in 0.05M Ca(NO₃)₂. Both log K and l/n values together explained 59.5% of the total variation in Y, while Zn content in the equilibrium soil extract, Zn desorbed in 0.05M Ca(NO₃)₂, 0.005M DTPA and 0.1M HCl collectively accounted 79.6% of the total variation in Y.     

Distribution of DTPA‐extractable Fe,Zn, and cu in soil particle‐size fractions

Abstract

To examine the distribution of DTPA‐extractable Fe, Zn, and Cu in clay, silt, and sand fractions; surface soils were collected from cultivated fields of North Dakota, South Dakota, West Virginia, Iowa, Ohio, and Illinois. Clay, silt, and sand fractions were separated after sonic dispersion of soil water suspension and analyzed for DTPA‐extractable Fe, Zn, and Cu. In general, clay had the highest and sand the lowest amount of DTPA‐extractable metals. Consequently, clay had the highest and sand the lowest intensity and capacity factors for these metals since DTPA micronutrient test measures both these factors.