Re‐analysis of the Relationship between Organic Carbon and Loss‐on‐Ignition in Soil

The suitability of loss‐on‐ignition (LOI) as an alternative to direct measurement of organic carbon (OC) has been debated for decades without resolution. The literature contains an abundance of different linear regression models to describe the LOI–OC relationship, most based on untransformed values of LOI and OC. Such regression is suspect because the variables are unable to occupy Euclidean space. Logratio transformation—based on relative rather than absolute differences—eliminates this constraint. Re‐analysis of the relationship on new and 10 previously published datasets using logratio techniques reveals that the relationship is nonlinear and that the profusion of regression models is in part a function of the range of LOI. Although LOI may offer a crude estimate of OC at high LOI levels, OC/LOI ratios when LOI is less than about 25% are too variable for reliable OC estimation, and interstudy comparisons remain dubious. Direct measurement of OC is recommended.     

Open‐vessel microwave digestion of animal waste samples for multi‐element analysis

Abstract

Wet acid digestion on a heat block or in a closed‐vessel microwave digestion system normally use half a gram to 1 gram of organic samples, but it is difficult to take a small quantity of representative sample from animal waste materials due to their heterogeneity. This study investigated an alternative microwave digestion system to prepare animal manure samples for plant nutrient analysis. Two types of solid animal manure and two reference plant samples were digested with an open‐vessel microwave digestion system and with the conventional nitric/perchloric acid block digestion, and analyzed for macro‐and micronutrients. Results of the open‐vessel microwave digested samples were comparable to those digested by conventional block digester and in high agreement with the certified values of reference materials. The open‐vessel microwave can reduce digestion time from about 4 hours to about 30 minutes. Fresh samples up to 10 grams can be completely digested directly by the open‐vessel microwave without sample drying and grinding. Sample representation of bulk manure should be better when sample size increased from 1 to 10 grams. Eliminating drying and grinding before digestion improves lab efficiency.     

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.     

Changes in tissue analysis caused by soil‐borne pathogenic fungl

Abstract

Several different organisms cause corn (Zea mays, L.) root rot. The extent of damage to the root system varies with the aggressiveness of different causal organisms or different strains of the same causal organism. The attack of the roots by disease organisms could cause changes in the tissue analysis that would lead to misdiagnosing the cause of the problem. Studies were conducted to ascertain changes in selected mineral concentrations in the corn tissue and in plant growth resulting from various degrees of root rot caused by root infections of several different soil borne pathogenic fungi. Thermally pasteurized soil was placed in pots and infested with various fungi isolated from root lesions on corn from field studies. Corn was grown in the infested soil for four weeks in the greenhouse. Plants were harvested, roots indexed for disease, above ground visual symptoms noted, dry weight taken, and tissue analyzed for Ca, Mg, P, and K. Results showed that aerial plant parts of infected plants may exhibit typical nutrient deficiency symptoms which are not necessarily reflected in the mineral analysis of the tissue. Elemental uptake and tissue concentration appeared not to be related to changes in mineral analysis regardless of the relative soil mobility of the nutrient. Related fungi did not cause similar changes in mineral tissue concentration for the same or different minerals. Dry matter yields were reduced about 20% for each unit increase in root disease index. The use of the root disease index appears to have potential as a diagnostic tool and should be evaluated for this purpose.     

Use of diffusion for automated nttrogen‐15 analysis of soil extracts

Abstract

Studies to evaluate the use of diffusion for automated ¹⁵N analysis of inorganic N in soil extracts showed that serious error can arise from use of the Devarda's alloy recommended for steam distillations and that the error can be avoided by using a commercial product of higher purity. These studies showed that serious error can also arise when NO₃ ^‐‐N is diffused following NH₄ ⁺‐N and that separate diffusions should be performed for NH₄ ⁺‐N and (NH₄ ⁺ + NO₃‐)‐N. Other work demonstrated that the plastic specimen containers employed for diffusion can be reused if acid‐washed, that diffusions can be performed using either light or heavy MgO without ignition to decompose carbonate, and that labeled NO₂‐is completely removed from soil extracts by treatment with sulfamic acid before diffusion. A comparison of ¹⁵N analyses by steam distillation and diffusion using extracts from two soils revealed better agreement for the soil having a lower content of organic matter. Substantial differences in analyses by the two techniques for the soil having a higher organic‐matter content were attributed to enzymatic conversions of inorganic N during the 6‐d diffusion period.     

Soybean leaf analysis of washed versus unwashed samples from boron‐manganese studies

Abstract

Elemental analyses of soybean leaf tissue from B & Mn field studies Indicate that washing tissue in deiontzed water did not appreciably change the concentration of most elements in the tissue. An exception was N which was decreased 0.54 per cent for one location and 0.33 per cent for the average of 3‐ sites when washed in deionized water prior to analyses. Although the tissue did not Indicate appreciable change tn K content when washed, the water In which the tissue had been washed Increased In K content by 6 ppm. The content of four of the micro elements in the plant tissue was affected by washing as compared to the unwashed samples. Mo and Ni were decreased while Zn and Cu were Increased.     

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.     

Soil macroporosity evaluated by a fast image‐analysis technique in differently managed soils

Abstract

Porosity, pore size distribution and a pore shape factor were measured from resin impregnated soils by means of a fast technique of image analysis. Images are directly captured by a video camera from polished impregnated blocks. Micromorphology was also used to assist in the comprehension of soil porosity changes in three differently managed soils: dry‐farming plus tillage, irrigated plus grass‐covered, steppe natural soil. Under study, alluvial soils from a semi‐arid region in NE Spain.

Even if there are no significative differences in total macro‐porosity between the differently managed soils, pore size distributions are significatively different Both natural and irrigated permanently‐covered soils have a larger amount of pores bigger than 1 mm in diameter, most of them of biological origin, greatly favouring aeration. Tillage contributes significantly to change the relative distribution of pore shape: the amount of rounded pores (vughs) decreases and elongated pores as well as fissures appear.     

Salinity effects on growth analysis and nutrient composition in four grain legumes‐rhizobium symbiosis

The effect of salinity on growth response, nitrogen (N) fixation and tissue mineral content was investigated for four legumes: faba bean (Vicia faba L), pea (Pisum sativum L), soybean (Glycine max L), and common bean (Phaseolus vulgaris L). Plants were grown in a vermiculite culture system supplied with a N‐free nutrient solution with the addition of 0, 50, and 100 mM NaCl. Plants were harvested at the beginning of the flowering period and the dry weights of shoots and roots and acetylene reduction activity (ARA) were evaluated at the same time plant tissues were analysed for N, potassium (K), calcium (Ca), magnesium (Mg), and sodium (Na) contents.

The depressive effect of saline stress on ARA of nodules was directely related to the salt induced decline in dry weight and N content in shoots. Growth inhibition by NaCl treatments was greater for the pea than for other legumes, whereas the soybean was the most salt‐tolerant Saline stress also affected the N content in shoots and roots. In general the N content accumulated in the shoot and Na in the roots of the four legumes tested, while K accumulated both organs. The acquisition of other macronutrients differed according to the legume species. The legumes most sensitive were P. sativum and V. faba which accumulated Ca in shoot and Mg both in the shoot and the roots. On the contrary, in G. max and P. vulgaris, the two most salt tolerant legumes, accumulated Mg in the roots and Ca in both vegetative organs. Our results suggest a relationship between the salt‐tolerant range in legumes and the macronutrient accumulation in vegetative organs.     

Importance of acid‐insoluble residue in plant analysis for total macro and micro elements

Abstract

Insoluble siliceous residues remaining after HNO₃/HClO₄ decomposition of the plant tissues National Bureau of Standards, standard reference materials spinach (Spinacea oleracea), orchard leaves and tomato leaves (Lycopersicon escuientum), contained varying quantities of the macro and micro elements Na, K, Mg, Ca, Mn, Fe, Cu and Zn. For the different samples with total element concentrations ranging from 11 μg/g (Cu in orchard leaves) to 45,000 μg/g (K in tomato leaves), residues contained element concentrations ranging from 0.05 to 88 times the respective concentrations in the samples. Contributions of residues to element concentrations in the plant tissues varied from 0.04 to 42% of the total concentrations. Overall, these constituted negligible (ca 0.1% for Mg and Ca), small (0.5% for Zn, Mn, K and 1% for Cu), and large (6% for Fe, 28% for Na) contributions depending on sample and analyte. Residue contributions to total element concentrations of plant tissues must be considered for reliable estimations of macro and micro elements.     

Cation exchange capacity of two‐component container media predicted from laboratory analysis of components

Abstract

A mathematical equation predicting cation exchange capacity (CEC) of pine bark‐sand container media from CEC of the individual components was formulated. The equation is the weighted sum of milliequivalents contributed by each component and is corrected for shrinkage due to mixing of components. Both measured and predicted CEC increased linearly with increasing percent volumetric bark in pine bark‐sand media. Regression equations describing measured and predicted CEC were not statistically different. The predictive equation was also tested on 6 non‐synthesized 2‐component media prepared from peat moss, perlite, pine bark, vermiculite, and sand. No statistical differences between measured and predicted CEC were obtained.     

A method for preventing the rehydration of heated smectites during X‐ray diffraction analysis

Abstract

Heating samples of clays to various temperatures is a common pretreatment for identification of clay minerals by X‐ray diffraction (XRD). The exchangeable cations in the interlayer region of smectitic clays can rehydrate when the sample is cooled after the heat treatments. Because the basal spacings (d(001)) of smectites are a function of the hydration state of the interlayer cations, they can be easily misinterpreted if the hydration state is not controlled during the XRD analysis. In this report a method for preventing the rehydration of interlayer cations during XRD analysis is described, and its effectiveness is demonstrated on selected samples of clays.     

The rapid determination of nitrate at low concentrations in soil extracts: Comparison of ion‐selective electrode with continuous‐flow analysis

Abstract

The efficiency of extraction of nitrate with saturated CaSCO₄ solution and with IM KCl was compared for a range of field‐moist and air‐dried soils. Saturated CaSO₄ was as effective for moist soils and slightly more effective for dried ones, and removed 95% of the nitrate after shaking for 5 min. Three methods of nitrate analysis using an ion‐selective electrode were compared with continuous‐flow analysis (CFA). All gave good correlations with CFA but only one, a “known addition” method, gave results which agreed quantitatively. This method could be applied at nitrate‐N concentrations at least as low as 0.5 mg kg^‐1.     

The measurement of low concentrations of ammonia in the atmosphere by flow‐injection analysis

Abstract

A flow injection procedure, based on the reaction between ammonia, salicylate, nitroprusside and alkaline dichlorisocyanurate, was developed which enabled changes in the concentration of ammonia in the atmosphere to be monitored at 15 minute intervals. The detection limit was 10 ppb NH₃‐N in solution for a working range of 0 ‐ 1000 ppb, corresponding to a concentration in the air of 4 μg NH₃‐N/m³. Regression analysis revealed a complex inter‐relationship between the concentrations of the reagents. The method was validated by the close correlation obtained between the results with a cross‐check analysis by ion chromatography and its use demonstrated by following the volatilization of ammonia from a soil core treated with urine.     

X‐ray fluorescence analysis of small leaf samples mixed with cellulose or boric acid

Abstract

X‐ray fluorescence (XRF) is an effective and rapid technique for the analysis of many mineral elements in plant tissue. Plant samples sometimes are too small to make good pellets and to provide good XRF analyses. Leaf tissue was mixed with cellulose or boric acid at different ratios to assess whether pellets from these mixtures could be analyzed by XRF and to determine the effects of these inert substances on analysis of Al, Ca, Cl, Cu, Fe, K, Mg, Mn, P, S, Si, and Zn. Concentrations of all elements decreased linearly at all leaf/cellulose ratios. Concentrations of Mn, Fe, Zn, and Cu decreased linearly at all leaf/boric acid ratios, but concentrations of the other elements decreased linearly only when leaf/boric acid ratios were above about 40/60, and decreases in concentration of these other elements were more pronouned at leaf/boric acid ratios below 40/60. Concentrations of P, S, Cl, K, Mg, Ca, Si, and Al were higher in leaf/boric acid than in leaf/cellulose pellets, and similar concentrations were noted for Cu, Mn, Fe, and Zn in both kinds of pellets. Mechanically shaking cellulose with leaf tissue generally resulted in higher mineral element concentrations than if samples were mixed by hand. Cellulose would be the preferred inert substance to mix with plant samples if plant samples are below ～40 mg in size. Small samples of plant tissue can effectively be analyzed by XRF when mixed with cellulose or boric acid.     

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.     

Critical nutrient concentrations and DRIS analysis of leaf and grain from high‐yielding corn

Abstract

A field experiment was conducted to optimize fertilizer inputs for maximizing the yield of irrigated com (Zea mays L.). This report is a summary of the nutrient composition of leaf and grain samples from the highest yielding treatment in the experiment. The experiment had 15 treatments replicated three times in a randomized complete block design. The N rate treatments were 45,100, 200, 300, and 400 kg N/ha with and without 50 kg P/ha, 67 kg K/ha, and 22 kg S/ha. The plant populations were 74,000 plants/ha (30,000 plants/A) and 100,000 plants/ha. The highest corn yield was 15.6 Mg/ha (250 bu/A with 15.5% moisture) which was produced with 300 kg N/ha combined with complete N, P, K, and S fertilization. It is assumed that samples of corn leaf and grain from a plot yielding that high would have nutrient concentrations in the sufficiency range. Many of the nutrient concentrations from these arbitrarily designated sufficiency ranges are close to the critical ranges and concentrations reported in the literature. It can be concluded that established critical concentrations and ranges could be useful for diagnosing high‐yielding corn. Furthermore, the negative DRIS indices for N, P, K, S, and Cu indicate that these nutrients are most likely to be limiting based on the published norms.     

A comparison between the H2SO4‐H2O2‐Li2SO4‐Se oxidation method and alternative digestion procedures for plant nutrient analysis.

Abstract

Ca, Mg, Na, K and P contents of 3 plant tissues obtained by H₂SO₄‐H₂O₂‐Li₂SO₄‐Se peroxidation digestion were compared with those determined by mixed acid (HNO₃‐H₂S0₄‐HC10₄) and dry ashing procedures. Differences between methods were not consistent between elements or tissue types but the mixed acid digestion generally yielded higher Ca, Mg and P values than did dry ashing and peroxidation. Tissue K contents estimated by both wet digestion techniques were not significantly (P ≤0.05) different. Differences in Na values between digestion methods were highly inconsistent between tissue types and the precision of the Ma data was poor. N contents determined by peroxidation digestion and a conventional Kjeldahl method agreed closely.     

Nitric acid digestion and multi‐element analysis of plant material by inductively coupled plasma spectrometry

Abstract

Inductively coupled plasma spectrometry (ICPS) was used for the simultaneous determination of P, K, S, Ca, Mg, Na, Al, Cu, Zn, Mn, Fe, Co, Mo and B in the nitric acid soluble portion of a variety of plant materials. Conditions for pre‐digestion, digestion and the requirement to grind cereal grain were investigated.

Digestion with nitric and perchloric acids caused loss of K (due to the low solubility of potassium perchlorate) and B (due to volatilization). The accuracy of Fe and Na determinations using nitric acid digestion was dependent upon the type of plant material.

The accuracy and precision of the proposed digestion and analytical procedure was confirmed by co‐operation in an interlaboratory quality assurance program using a variety of standard reference plant materials, and the analysis of National Bureau of Standards, Standard Reference Material 1571 (orchard leaves).     

Nitric acid dissolution and multi‐element analysis of soils and sediments by inductively coupled plasma spectrometry

Abstract

A method was developed for the simultaneous analysis of P, K, Cu, Cd, Zn, Fe, Mn and Pb in soils and sediments by inductively coupled plasma spectrometry (ICP) after digestion in nitric acid. The procedure extracted 82 to 94% of the totals of the heavy metals, 78% of total P and 34% of total K. Inter‐element interference correction data are given for the ICP method. The method gave results similar to those obtained by other analytical procedures. The precision of the method was satisfactory but was lowest for Cd which had the lowest concentrations (<2.7 mg/kg) of the elements determined.