A manual colorimetric procedure for measuring ammonium nitrogen in soil and plant Kjeldahl digests

Abstract

The measurement of NH4⁺‐N in soil, and plant digests is one of the greatest needs in laboratories conducting agricultural and environmental research. Many laboratories do not have access to automated equipment for colorimetric analysis of soil and plant digests. The objective of this research was to modify an automated colorimetric analysis procedure for determining NH₄+‐N in soil and plant digests for manual use, and compare the proposed technique with the standard distillation‐titration technique. The modified procedure is based on the color reaction between NH₄ ⁺‐ and a weakly alkaline mixture of Na salicylate and a chlorine source in the presence of Na nitroprusside. Wavelength scans indicated a very well defined peak for determinations at 650 nm. Time scans showed that color development in the manual procedure was rapid, 12 to 40 minutes depending on temperature, and that the color development remained stable for at least 120 minutes. Regression analysis of the results from 18 soil and 20 plant tissue sample determinations by distillation‐titration and the proposed method indicated NH₄ ⁺ ‐N recoveries of 99% or higher. The results obtained using the colorimetric procedure were very similar to the values obtained by distil ling and titrating the digests for both soil and plant samples as indicated by the large coefficients of determination (R² = 0.99).     

Measurement of available soil phosphorus under conventional and no‐till management

Abstract

The objective of the investigation was to compare the predominant forms of P in fields of an acid Matapeake soil under no‐till and conventional‐till management. The fields, which differed in extent of contact between soil and fertilizer P, also differ in forms of P. Fertilizer P remained in the uppermost layer of no‐till fields and was, therefore, not in as close proximity to the plant (corn) roots as P was in conventional‐till fields. Nevertheless, fertilizer P in the no‐till fields underwent only limited conversion to forms less available to plants and thus, in part, may have accounted for similar plant uptake rates of P in no‐till and conventional‐till fields.

One method used to analyze P in the Matapeake soil was the double‐acid‐extraction method. This method is used by several state soil‐testing laboratories of the eastern and southeastern United States, where acid soils like Matapeake are common. The double‐acid‐extraction method underestimated the soil P available for plant uptake.     

Soil and plant analysis as methods for diagnosing micronutrient deficiencies

Abstract

Soil and plant analyses can be effectively used to detect and confirm suspected micronutrient deficiencies. The numbers of laboratories offering tests for the micronutrients has increased substantially in the last 10 years. Suitable soil tests have been developed for most of the micro‐nutrients. Although plant analysis is relatively new, its use is gaining wide acceptance as an effective means of evaluating the micronutrient status of plants and plant tissue. Considerable improvement in methodology has been a primary factor in the increasing use of soil tests and plant analyses as means of evaluating the micronutrient status of the soil‐plant environment.     

A comparison of the results from three soil testing laboratories using the mehlich‐3 extractant on southeastern coastal plain soils

Abstract

Soil test values from three laboratories using the Mehlich‐3 extradant on Coastal Plain soils with a wide range in soil test levels were compared. Soil samples were collected over a four year period from four Southeastern/Mid‐Atlantic states (SC, NC, VA and DL). The results among labs were highly correlated (r > 0.9) for all elements analyzed (P, K, Ca, Mg, Mn, Zn, and Cu). Regression equations were developed to predict the soil test values among laboratories for each element. Comparisons of extractable levels for the elements shown above among the three laboratories are given.     

Rapid,Wet Oxidation Procedure for the Estimation of Silicon in Plant Tissue

Abstract

The quantification of silicon (Si) in plant samples is being requested more frequently, especially in agricultural laboratories associated with the determination of nutritional requirements of sugarcane (Saccharum officinarum L.) and rice (Oryza sativa L.). The analysis of plant material for Si can be protracted, especially if laboratories do not have access to X‐ray flourescence (XRF) instrumentation and large numbers of samples are involved. A simplified procedure using equipment considered standard in most agricultural laboratories is reported. Dry, ground plant material is subjected to nitric acid/peroxide oxidation in a low‐pressure laboratory microwave digestion system. The hydrated silica liberated from the organic matrix is dissolved in a small volume of sodium hydroxide solution also using the microwave digestion system. Silicon is measured by inductively coupled plasma atomic emission spectrometry (ICP‐AES). This method gives results that are linearly correlated with the much slower conventional techniques and avoids using hazardous chemicals (hydrofluoric acid) sometimes employed in other microwave methods.     

Quality assurance for plant tissue analysis by ICP‐AES

Abstract

A survey of 12 service laboratories using ICP‐AES for routine plant analysis reveals a variety of sample preparation and instrument calibration procedures in use. With the continued growth of ICP applications in plant analysis laboratories, a need exists for inter‐laboratory quality control.

The assurance of data quality among laboratories cannot be expected unless a standardization of preparation methods and calibration is accomplished. In the selection of a method for multi‐element determination on the same sample solution, the completeness of elemental release and sensitivity for some elements may have to be compromised.

In addition to the above survey, 8 plant samples were sent to 5 ICP laboratories that handle large volumes of plant samples with each using different preparation and calibration methods. The results for 11 elements show that the best precision among laboratories was for P, Mg, Mn, Ca and K, and the poorest precision for Al, Zn, Fe, Na, Cu and B. The imprecision noted for some elements was presumed to be caused by the diversity of preparation and calibration methods. Quality control efforts taken by this laboratory will also be given.     

A rapid steam distillation method of assessing potentially available organic nitrogen in soil

Abstract

A rapid steam distillation of assessing potentially available organic nitrogen in soil is described. It involves determination of the ammonia‐N produced by steam distillation of the soil sample with pH 11.2 phosphate‐borate buffer solution for 8 min. The method is simple and precise, and its results are not significantly affected by air‐drying or air‐dry storage of the soil sample before analysis. It is well suited for use in soil testing laboratories because it does not require extraction, filtration or transfer steps. Studies using 33 Brazilian soils showed that the results obtained by this method were highly correlated with those obtained by aerobic and anaerobic incubation methods of assessing potentially available organic nitrogen in soil.     

Evaluation of extractants for predicting availability of sulphur to mustard in inceptisols

Abstract

Mustard (Brassica juncea) is an important oilseed crop of northern India, which is widely grown in Delhi and adjoining States. This crop has a relatively high requirement of sulphur (S), and is sensitive to S‐deficiency. For predicting response of mustard to S application, several extractants have been tried with variable results. Since selection of a promising extractant for a particular soil needs careful consideration, the present investigation was planned to select the most promising extractant to predict the availability of S to mustard grown on Inceptisols of Delhi. For this purpose, a greenhouse experiment was conducted with twenty soils (two from each often important soil series from the cultivated alluvial soil belt of Delhi. Nine extractants, commonly used for estimating the availability of S, were evaluated and S in soil extract and in plant digest was estimated using the turbiditimetric method. The results indicate that the phosphate salt methods extracted comparatively more S than other extractants. The amount of S extracted by these extractants was found in the following order: KH₂PO₄‐500 ppm P>Ca(H₂PO₄)₂‐500 ppm P>0.001 M HCl>NaOAc+HOAc>heat soluble S>0.15% CaCl₂>l% NaCl> water soluble S>NH₄OAc+HOAc. Simple correlation coefficients of the amounts of S extracted by different extractants and the forms of S with the plant parameters were worked out. To determine the combined effect of soil characteristics on S extraction by different extractants, stepwise multiple regression analysis was carried out. Based on this study, the suitability of the extractants for mustard crops in Inceptisols of Delhi may be arranged as follows: 0.15% CaCl₂>water soluble S>0.001 M HCl>Ca(H₂PO₄)₂‐500 ppm>1%NaCl>NH₄OAc+HOAc>NaOAc+HOAc>KH₂PO₄‐500 ppm P>heat soluble S.     

Soil Test to Predict the Copper Availability in Pasture Soils

Abstract

The proportion of copper (Cu) that can be extracted by soil test extractants varied with the soil matrix. The plant‐available forms of Cu and the efficiency of various soil test extractants [(0.01 M Ca(NO₃)₂, 0.1 M NaNO₃, 0.01 M CaCl₂, 1.0 M NH₄NO₃, 0.1 M HCl, 0.02 M SrCl₂, Mehlich‐1 (M1), Mehlich‐3 (M3), and TEA‐DTPA.)] to predict the availability of Cu for two contrasting pasture soils were treated with two sources of Cu fertilizers (CuSO₄ and CuO). The efficiency of various chemical reagents in extracting the Cu from the soil followed this order: TEA‐DTPA>Mehlich‐3>Mehlich‐1>0.02 M SrCl₂>0.1 M HCl>1.0 M NH₄NO₃>0.01 M CaCl₂>0.1 M NaNO₃>0.01 M Ca(NO₃)₂. The ratios of exchangeable: organic: oxide bound: residual forms of Cu in M1, M3, and TEA‐DTPA for the Manawatu soil are 1:20:25:4, 1:14:8:2, and 1:56:35:8, respectively, and for the Ngamoka soil are 1:14:6:4, 1:9:5:2, and 1:55:26:17, respectively. The ratios of different forms of Cu suggest that the Cu is residing mainly in the organic form, and it decreases in the order: organic>oxide>residual>exchangeable. There was a highly significant relationship between the concentrations of Cu extracted by the three soil test extractants. The determination of the coefficients obtained from the regression relationship between the amounts of Cu extracted by M1, M3, and TEA‐DTPA reagents suggests that the behavior of extractants was similar. But M3 demonstrated a greater increase of Cu from the exchangeable form and organic complexes due to the dual activity of EDTA and acids for the different fractions and is best suited for predicting the available Cu in pasture soils.     

Assessment of soil and plant analysis laboratories in the West Asia‐North Africa Region

Abstract

Although limited amount of water is the primary constraint to agricultural productivity in the rainfed area of West Asia and North Africa (WANA), yields are also low because of the poor mineral nutrient status of soils. Yields can, therefore, be considerably increased by judicious fertilizer use. Laboratories for soil and plant analysis are essential for identifying nutrient constraints and providing a basis for efficient fertilizer use, through correlation studies to establish suitable soil testing extractants and calibration studies with crop responses. The Soils Laboratory at the International Center for Agricultural Research in the Dry Areas (ICARDA) has initiated a quality control program among the national agricultural research systems (NARS) in the countries of the WANA region. The efforts include linkages with the Wageningen International Soil Analytical Exchange Program, in‐country training courses, and a laboratory analysis manual. Continued improvement in laboratory performance is dependent upon knowledge of the capabilities of such laboratories and identification of their constraints. This presentation reports a fact‐finding survey of laboratories from 16 countries of the WANA region—mainly public, from universities and ministries of agriculture, and some private or commercial ones—based on a questionnaire about analyses, facilities, methodologies, quality assurance, personnel training, and management. Future efforts to improve the quantity and quality output from of these laboratories will address such deficiencies.     

Wildfire‐induced alterations of topsoil organic matter and their recovery in Mediterranean eucalypt stands detected with biogeochemical markers

This study addressed fire‐induced changes in topsoil organic matter (SOM) from a eucalypt plantation in Portugal over 2 years by using three complementary biogeochemical techniques: elemental analysis, analysis of biomarkers from the total extractable lipids (TLE) and solid state ¹³C nuclear magnetic resonance (NMR) spectroscopy. Direct wildfire effects included a marked decrease in soil total organic carbon (TOC) and total nitrogen (TN) content. However, both contents seem to have recovered during the 2 years. Fire also substantially reduced the TLE, producing noticeable changes in its composition. These included the thermal breakdown and cracking of n‐alkyl compounds. Ratios of short‐to‐long n‐alkanes and n‐fatty acid methyl esters (FAMEs) increased and typical carbon number predominance indices for n‐alkanes (odd‐to‐even) and n‐FAMEs (even‐to‐odd) were altered. Furthermore, the relative abundances of certain markers that are plant‐species specific were modified, especially by decreasing terpenoids such as epiglobulol, ledol and globulol, which are characteristic of Eucalyptus globulus. Other differences observed in the burnt soil were the appearance of levoglucosan, a typical marker for the thermal alteration of polysaccharides, larger relative abundances of lignin‐derived compounds (vanillin and methoxyphenols) and the presence of N‐heteroaromatic structures, which suggested the accumulation of ‘black nitrogen’. The ¹³C NMR spectra indicated that the wildfire produced a considerable increase in the aromaticity and aromatic condensation of the topsoil SOM. This was reflected in a broadening of the signal of aromatic compounds at the expense of O‐alkyl and alkyl‐C compounds. The continuation of these differences in SOM quality during the 2‐year study suggested a slow recovery of soil properties, possibly influenced by a limited recovery of the vegetation after the fire combined with the fire‐enhanced losses of soil.     

Certification of an air‐dry soil for pH and extractable nutrients using one hundredth molar calcium chloride

Abstract

The preparation of an air‐dry river‐clay soil as reference soil material for pH and extractable nutrients with a 0.01 M calcium chloride (CaCl₂) solution and the homogeneity testing are described. Recommended values for pH and the concentrations of ammonium‐nitrogen (NH₄‐N), total soluble nitrogen (N), phosphorus (P), sodium (Na), potassium (K), and magnesium (Mg) using the unbuffered 0.01M CaCl₂ are given. With respect to nitrate‐nitrogen (NO₃‐N), the sample proved not to be sufficienctly homogeneous. The certified soil sample has also been used as a sample in the International Soil‐Analytical Exchange (ISE), a continuous proficiency testing scheme. The values found by the ISE laboratories compared well with the certified values.     

Within plot variability in available soil mineral nitrogen in relation to leaf greenness and yield

Abstract

Available soil mineral nitrogen (N) varies both temporally and spatially. These variations affect field‐scale N‐use efficiency. A field study was conducted for three years to investigate spatial variability in available soil mineral N within uniform research plots in relation to leaf greenness or chlorophyll content (plant N sufficiency) and yield. Variations within the plot in available soil mineral N sampled at the 6‐ligule stage was related to N fertility: the higher the fertilizer N levels, the higher the variability. The standard deviation for the 200 kg N ha^‐1 treatment was up to five times higher than the unfertilized control treatment. The nitrate (NO₃)‐N accounted for 70 to 80% of soil mineral N in fertilized plots compared to 50 to 60% in unfertilized control plots. The variability in grain yield of individual maize (Zea mays L.) plants within a plot was inversely related to soil N fertility: the higher the fertilizer N levels, the lower the yield variability (at 100 or 200 kg N ha^‐1, yield ranged from 97 to 148 g plant¹, or 10% CV within ayear compared to ranges from 0 to 82, or 50% CV in the same year at 0 kg N ha^‐1). On an individual plant basis, chlorophyll content from the 6‐ligule stage through the growing season generally showed much smaller CV's, but had a similar trend to variations in yield. Leaf greenness from 6‐ligule stage to silking was significantly correlated with harvest yield (r>0.60, P<0.01), and both also correlated with available soil mineral N, though to a lesser degree (r>0.36). The number of fully expanded leaves prior to silking differentiated N treatments better than did single leaf chlorophyll measurements with higher yields associated with more rapid vegetative development. Our data suggest that multiple core samples are required to estimate available soil mineral N, particularly in fertilized plots that have greater spatial variability. Variability of plant‐based measures, such as chlorophyll content, could be used as an indicator of relative plant N sufficiency at early growth stages as spatial variability declined with higher soil N fertility.     

Characteristic alterations of quantity and quality of soil organic matter caused by forest fires in continental Mediterranean ecosystems: a solid-state 13C NMR study

The variable effect of different types of forest fires on the quantity and quality of soil organic matter (SOM) was analysed by comparing burnt and unburnt soils from six forest ecosystems in central Spain by organic elemental analysis and solid‐state ¹³C nuclear magnetic resonance (NMR) spectroscopy. Whole soil samples were collected 1 to 2 years after the fires and included one site affected by two fires within 2 years. The fire‐affected soils showed no common pattern with respect to the amount of additional carbon (C_add) but at all sites, the fire enhanced the aromatic‐C content. The weakest fire intensity resulted in the greatest aromatic‐C enrichment factor, EF_{I(aromatic C)} indicating the greatest local accumulation of char. The respective C_add disclosed an EF_{I(aromatic C)} to EF_{I(alkyl C)} ratio, B_char, of c.1, which supports a small degree of charring. Extensive combustion and volatilization at stronger fire intensities yielded a decrease of EF_{I(aromatic C)} and an increase in B_char. These trends are in good agreement with fire intensity and forest fuel combustibility in the various sites and therefore these indices could be used to elucidate the quality and quantity of char input that occurs during and after forest fires. No ¹³C NMR evidence for substantial inputs from non‐charred plant necromass was found for any of the single‐burn soils. The large carboxyl‐C content of C_add is evidence of the occurrence of oxidation reactions very shortly after the fire. In comparing the single and double‐burn sites, no additional char input was observed for the double‐burn site, possibly because of complete combustion of young shrubs and char remains during the second fire. The large O‐alkyl‐C portion found in C_add of the double‐burn soil is best explained by decreased litter degradation.     

AB‐DTPA cation extraction in Spanish soil samples

Abstract

Since only one extraction is required to determine a large number of nutrients, many laboratories employ universal extractants to determine the available nutrients in a soil sample. This paper compares the universal ammonium bicarbonate‐DTPA (AB‐DTPA) method developed by Soltanpour and Schwab (1977) with the traditional methods, ammonium acetate (NH₄OAc) test for exchangeable cations and the Lindsay and Norwell (1969) test for the micronutrients. Results from the analysis of 28 soils by these methods were compared. Most soils were selected from those used by the Spanish Working Group for the Standardization of Analytical Methods. In most cases, statistical correlations between methods presented good agreement for each element, but depending on the soil pH range, some elements needed two correlations. Also, when results for wet and dry soils were compared, variability was lower when the AB‐DTPA extraction method was used. We concluded that, besides being faster, the AB‐DTPA method is valid for Spanish soils, even for calcium (Ca) extraction in calcareous soils, where the ammonium acetate method fails due to excessive Ca solubilization.     

Snap bean response to soil tillage management and cover crops

Abstract

Snap beans (Phaseolus vulgaris) were grown using conventional tillage (CT) and no‐tillage (NT) soil management following either hairy vetch (Vicia villosa Roth) or rye (Secale cereale L.) in 1992 and 1993 in the mountain regions of Georgia near Blairsville. Soil bulk density and inorganic nitrogen content as well as crop dry matter production and yield were monitored. Soil bulk density of the surface (0 to 10 cm) layer under NT exceeded that under CT at planting by as much as 0.33 Mg/m³. However, growth‐limiting bulk densities (values>1.45 Mg/m³) did not occur under either tillage regime. Inorganic soil nitrogen to a depth of 30 cm at planting and at five weeks after planting was similar for the two tillage systems. However, soil nitrogen (N) tended to be greater following hairy vetch than following rye. There were no significant effects of tillage or cover crop on plant stand or plant dry weight. Total yields were generally similar regardless of tillage or cover crop. A notable exception was that early yield in 1992 was 62% greater using NT. These results indicate great potential for use of conservation tillage and cover crops in the production of snap beans in the mountain regions of the southeastern United States.     

Effects of normal and Fe‐treated organic matter on Fe chlorosis and yields of grain sorghum

Abstract

A greenhouse study was conducted to evaluate the effects of normal and Fe‐treated plant material on Fe chlorosis and yields of grain sorghum. Pigweed, guar, clover, sunflower and wheat plants grown in the field for six weeks were sprayed with a 20% ferrous sulfate solution. The plants were harvested after 48 hours, air dried, then ground to pass through a 0.5 mm stainless steel seive. Different rates of normal and Fe‐treated plant material (0, 14.8, 22.2 and 29.6 Mg ha^‐1) were added to the Pernitas fsl (Typic Agiustoll).

Chlorosis increased with increasing rates of normal plant material added to the soil. Conversely, applications of Fetreated plant material reduced Fe deficiency chlorosis in grain sorghum. The order of effectiveness of Fe‐treated plant material was: sunflower > pigweed > guar > clover > wheat. There was no significant growth response to the untreated plant material. Growth responses to the Fe‐treated plant material were: sunflower > pigweed > guar > wheat > clover. Data obtained indicate that sunflower and pigweed are good Fe‐carriers and could be used to recycle Fe in the soil to correct Fe deficiency chlorosis and increase yields     

Soil Characteristics and Mineral Nutrient in Wild Jatropha Population of India

Abstract

Mature leaves of naturally occurring Jatropha curcas plants and soils samples were collected from four different populations to determine the soil characteristics, soil‐available nutrients, and leaf nutrient contents. This study provides a reliable account of the endogenic concentrations of nutrients present in jatropha leaves. Soil manganese [diethylenetriamine pentaacetic acid (DTPA)‐Mn] was the only soil‐available nutrient significantly correlated with its content in the plant. Relationships between soil characteristics, available nutrient in soil, and their content in plant leaves were also attempted.     

An evaluation of chemical methods for extracting copper from rice soils

Abstract

Rice (Oryza sativaL. CV. Lemont) was grown on 19 soils, and eight extractants were evaluated for determining the availability of Cu to rice plants. Correlation analyses were employed as criteria for evaluating methods that would provide the best index of Cu availability. The order of removal of Cu from soils was: 0.5NHC1 + 0.05NA1C1₃> 0.5NHNO₃> 0.5 N HC1 > EDTA + NH₄OAc > 0.1NHC1 > EDTA + (NH₄)₂CO₃? DTPA‐TEA, pH 7.3 >>> 1 N NH₄0Ac, pH 4.8.

Uptake of Cu by rice plants was significantly correlated with soil Cu. Among the eight extractants evaluated, Cu extracted with DTPA‐TEA, pH 7.3 was better related to the concentration (r = 0.563 ) and uptake (r = 0.673 ) of Cu by rice plants grown on the soils with different chemical and physical properties.

A significant negative correlation was found between the concentration of Cu in rice plants and the organic matter content of the soils. Each one percent increase in the organic matter of the soils resulted in a corresponding decrease of approximately one mg/kg in the concentration of Cu in the rice‐plant tissue. Multiple regressions of extractable Cu by eight methods with soil organic matter content accounted for from 53.4 to 70.0% of the variations in the prediction of the concentration of Cu in the rice plants. Combinations of other soil chemical properties measured with extractable Cu did not significantly improve the predictability     

Boron analysis in soil extracts and plant tissue by plasma emission spectroscopy

Abstract

Nine Colorado soils were treated with sodium borate and were subjected to 3 wetting and drying cycles. These soils were extracted with hot water for boron analysis. Plant samples, including NBS standard reference materials (SRM) 1571, 1570, 1573, were dry ashed and wet digested using nitric acid. All soil extracts and plant digests were analyzed for boron using ICP‐AES and colorimetrically using the Azomethine‐H method.

A high degree of correlation (r² = .99) was found between boron determination by ICP and the Azomethine‐H method for soil extracts and plant digests. The Azomethine‐H method gave B values 9% higher than ICP‐AES on the average.

Boron levels determined by ICP were similar to NBS boron values for both the dry ashed and wet digested SRM plant samples. Boron levels determined colorimetrically were comparable to the NBS values for dry ashed SRM plant samples. Plant samples digested in nitric acid could not be analyzed for boron by the Azomethine‐H colorimetric method due to interferences resulting from nitrate complexes in the wet digest.