Comparison of methods for measuring heavy metals and total phosphorus in soils contaminated by different sources

The relationships between the concentrations of zinc (Zn), lead (Pb), copper (Cu), nickel (Ni) and chromium (Cr) as measured by X-ray fluorescence analysis (XRF), aqua regia, and HNO₃ pressure digestion were studied in soil samples covering a wide range of heavy metal concentrations. The soils were contaminated by sewage sludge, exhaust depositions, river sediments of mining residues, and dump material. The question was addressed whether the source of heavy metals or other soil properties affect the relationship between these three methods. The aqua regia-digestible fraction of the five heavy metals reached on average 64% of the XRF-detectable content. The pressure accelerated HNO₃-digestible fraction of the five heavy metals was on average 71% of the XRF-detectable content; the respective phosphorus (P) fraction reached a median of 75%. This suggests that HNO₃ pressure digestion can also be used for characterizing the total P content of soils. Aqua regia extraction and HNO₃ pressure digestion gave similar values for Zn, Pb, and Cu, which dominate the heavy metal load of most contamination sources. Significantly higher Cr values were obtained by HNO₃ pressure digestion than by aqua regia extraction. Additionally, the Cr contents were affected by the source, e.g. sewage sludge had relatively high contents of aqua regia and HNO₃ pressure extractable contents in comparison to the XRF values. The element-specific relationships between the three methods were all highly significant. However, the respective multiple linear regression models were in most cases affected by soil organic carbon (C), in some cases by clay or soil pH.     

Phosphorus source effects on alfalfa yield,total nitrogen content,and soil test phosphorus

Abstract

Recent studies showing a lack of response by alfalfa (Medicago sativa L.) to phosphorus (P) fertilization have raised concerns about the efficacy of commonly used P fertilizer materials in the southwestern United States. Studies were conducted between 1982 and 1985 in southeastern New Mexico to evaluate (i) alfalfa yield response to different P sources, (ii) the effect of P fertilizer source on forage total nitrogen (N) content and leafiness, and (iii) the effect of P fertilizer source on soil test P. Nine P sources were applied annually from 1982 through 1984 at a rate of 58 kg P/ha. Alfalfa was grown during 1985 without fertilization to examine the residual effect of P sources. Triple superphosphate (TSP) and monoammonium phosphate (MAP) gave the highest alfalfa forage yields over the 3‐year application period, but no residual fertilizer effects were observed when fertilization was discontinued. Fertilization did not affect forage leafiness. Except for a small N response in forage total N content in 1984, neither P nor concomitant applied N had a significant effect on forage N content over the 3‐year period. Phosphorus fertilization significantly increased average soil test P for the 3‐year period, but there were no significant differences between treatments. Currently used P materials (TSP and MAP) still appear to be the most efficacious for alfalfa production.     

Portable soil test laboratory results compared to standard soil test values

Abstract

Results from a commercially available portable soil test laboratory were compared to standard soil test procedures used by a public soil testing laboratory. Standard soil tests examined were water extracted NO₃‐N, pH, Acid‐P, NaHCO₃‐P, and ammonium acetate extracted K. Approximately 35 to 55 different soils were used to compare methods for each soil test. Linear regression equations between the portable laboratory soil test values and those from the standard procedures were developed. The r² values for NO₃‐N, pH, Acid‐P, NaHCO₃‐P, and K were 0.970, 0.891, 0.734, 0.742, and 0.887, respectively. The coefficient of variability values for NO₃‐N, pH, Acid‐P, NaHCO₃‐P, and K were 10, 1, 13, 15, and 6%, respectively for the portable laboratory, and 9, 2, 8, 9, and 5%, respectively for the public soil testing laboratory. Multiple regression was used to relate soil properties to soil test results. The R2 values for NO3‐N, pH, Acid‐P, NaHCO₃‐P, and K were 0.970, 0.911, 0.860, 0.940, and 0.936, respectively.     

Comparison of phosphorus impregnation and bray 1 soil tests for evaluating plant available phosphorus

Abstract

The relationship between soil test phosphorus and crop response has not been studied for maize (Zea mays L.) in some major benchmark soils of Zambia. The suitable soil test procedure for estimating available P needs to be identified. The objective of this study was to compare two soil test methods, impregnation of phosphorus (Pi) and Bray 1, in predicting P requirement of maize grown in Makeni (fine, mixed Isohyperthermic Udic Paleustalf), Maheba (clayey, kaolinitic, isohyperthermic Haplic Acrustox), and Konkola soil series (fine, oxidic, isohyperthermic oxic, Rhodustalf). The three soil series were treated with 0, 262, 524, and 1,048 mg P per pot as triple superphosphate (TSP). Maize was grown in pots, and after 8 weeks the plants were harvested and analyzed for total P concentration. Phosphorus uptake (P uptake) was calculated as a product of P concentration in the plant and maize dry matter yield. The soil was dried, sieved and analyzed for available P. The available P content estimated by Bray 1, and Pi soil tests was correlated with maize dry matter yield, and P uptake. The P which was extracted from Makeni soil series by Pi soil test correlated highly significantly (r=0.996**) with maize dry matter yield, but the correlation of maize dry matter yield and P extracted by Bray 1 soil test was not significant (r=0.908 ns), Correlation of P uptake with P extracted by Bray 1 soil test was high and more significant (r=0.991 * *), than correlation with P extracted by Pi soil test (r=0.958*). The P extracted from Makeni soil series by Pi soil test correlated highly significantly (r=0.996**) with maize dry matter yield, but the correlation of maize dry matter yield and P extracted by Bray 1 soil test was not significant (r=0.908 ns), Correlation of P uptake with P extracted by Bray 1 soil test was high and significant (r=0.990**), as well as correlation with P extracted by Pi soil test (r=0.958**). The correlation of P extracted from Maheba soil series by Pi soil test and maize dry matter yield followed the same trend as for Makeni series with correlation of r=0.990**. The correlation of P uptake and P extracted by Pi soil test was high but less significant (r=0.955*) than that for Makeni soil series. The correlation of P extracted by Bray 1 soil test with maize dry matter yield was high (r=0.973 *) and significant, but the correlation with P uptake was low and not significant (r=0.879 ns). The available P extracted from Konkola soil series by both Bray 1 and Pi soil tests produced poor and not significant correlation with maize dry matter yield, as well as P uptake. The results show that Bray 1 soil test extracted larger amounts of P from all the three soil series than P impregnation (Pi) soil test. The results further demonstrated that Pi soil test was consistently more closely related to P uptake and dry matter yield of maize grown in Makeni and Maheba soil series. Therefore, Pi soil test was more effective than Bray 1 soil test in evaluating soil solution P that the plant usually takes up.     

Comparison of two rapid test procedures with the standard EC test recovery of fecal coliform bacteria from shellfish-growing waters.

A study was conducted to compare recovery and enumeration capability of two 24-hr multitube fermentation tests with the standard EC test for fecal coliform levels in shellfish-growing waters. The 2 tests were the A-1 test developed by Andrews and Presnell, specifying 24-hr incubation in A-1 medium at 44.5 degree C; and a modification of the A-1 test requiring a 3-hr resuscitation of 35 degree C before incubation at 44.5 degree C for 21 hr. Fifteen State, Federal, and Provincial laboratories examined 10 routine shellfish-growing area samples per month in parallel by the 3 methods for 1 year. IMViC tests (indole, methyl red, Voges-Proskauer, and citrate) were conducted on all gas-positive tubes. The modified A-1 test recovered higher levels of fecal coliforms than the A-1 test. Although there were seasonal and geographic variations in recovery and enumeration by the modified A-1 test, overall there was good correlation of the modified A-1 test with the EC test. Both the A-1 and modified A-1 tests were more specific for Escherichia coli than the EC test. Results of the study indicate that the 24-hr modified A-1 test can be used as an alterantive test for the standard 72-hr EC test as an adjunct to the sanitary survey for the classification and control of shellfish-growing areas waters.     

Crop production impacts on soil phosphorus removal and soil test levels

An 8-year field study documented the impact of tillage, crop rotations, and crop residue management on agronomic and soil parameters at Brookings, South Dakota. The greatest annual proportion of above-ground biomass phosphorus (P) removed was from the grain (78–87% of total) although crop residue removed some P as well. Greater above-ground total biomass P (grain P + crop residue P) was removed from corn than from soybean and spring wheat crops mainly due to the greater corn grain biomass harvested. Cumulative above-ground biomass P removal was greatest for the corn-soybean rotation (214 kg P ha^?1), while it was lowest for the soybean-wheat rotation (157 kg P ha^?1). Tillage treatments within crop rotation or residue management treatments did not influence annual or cumulative P removal rates. Olsen extractable soil orthophosphate-P levels declined consistently through time from a mean of 40 µg g^?1 (2004) to 26 µg g^?1 (2011). Biomass P removal was calculated to be 15.7 ha^?1 yr^?1 to decrease Olsen extractable soil orthophosphate-P levels by 1 µg g^?1 yr^?1 over 8 years of the study.     

Relationships between relative crop yields,soil test phosphorus levels,and fertilizer requirements for phosphorus

Abstract

More uniformity in methods of deriving fertilizer P recommendations from crop response data should improve accuracy and precision of fertilization rates. Experimental data that relate crop yields to soil test levels and describe the effect of fertilizer P on soil test levels provide the basis for determining fertilization rates for specific crop‐soil situations. A modification of the Mitscherlich equation was used in derivation of a new equation for calculating fertilizer P requirements as a function soil test levels of P. The equation was applied to response data for 4 crops.

Response curves and fertilizer requirements as calculated for corn, soybeans, alfalfa, and clover‐grass indicated that soybeans yielded relatively more than the other three crops at low soil test levels of P. Corn and alfalfa required higher soil test levels to reach 95% maximum yield and required higher rates of fertilizer P when initial test levels were low.     

Soil phosphorus testing: 2. Assessment of a rotary blade soil sampler for collecting soil samples to measure soil test phosphorus

Abstract

In Western Australia soil samples to measure soil‐test phosphorus (P) are collected November to March when soils are usually dry. Most of the soils are hard‐setting when dry and it is difficult to penetrate and collect soil samples to 10 cm using the traditional sampler, which is a 2.5 cm diameter tube that is pushed into the soil by foot. Farmers collect too few soil samples at shallow depths to measure soil‐test P. In Part 1 of this paper, it was shown that soil‐test P can vary markedly for individual soil samples collected from uniform areas in paddocks. Consequently, an adequate number of soil samples needs to be collected and bulked from defined areas to measure soil‐test P. Phopshorus accumulates near the top of the soil of (i) pastures since P fertilisers are applied to the surface of pastures, and (ii) crops sown by minimum (conservation) tillage. Crops are increasingly being sown using conservation tillage methods. Collecting too few soil samples to a shallow depth can result in large errors when estimating the current P status of soils and determining optimum fertiliser application levels. A new rotating blade method of collecting soil samples to the standard 10 cm depth for measuring soil‐test P was compared with the traditional sampler. The new sampler successfully penetrated hard‐setting soils to the standard depth and the soil samples it collected produced similar soil‐test P as the traditional sampler. Consequently, the same soil‐test P calibrations determined using the traditional sampler can also be used for the new sampler. The new sampler is, therefore, recommended for collecting soil samples to measure soil‐test P. It should have application wherever hard‐setting soils pose a problem for soil P testing.     

Dairy manure treatment effects on manure phosphorus fractionation and changes in soil test phosphorus

In this research, a sequential fractionation procedure coupled with enzyme hydrolysis was used to categorize the phosphorus (P) forms of 18 manure samples collected from in-barn composted bedded pack (beef manure), anaerobic digestion with liquid–solid separation (dairy manure), and liquid–solid separation systems (dairy manure). This research also determined the effects of those P forms on the increase in soil test P (STP) of five soil series. The soils used had initial Bray-1 P ranging from 16 to 43 mg P kg^?1. Total dry-ash P (P_t) of the manures ranged from 1.4 to 15.0 g P kg^?1; total inorganic P (P_it) accounted for 20 to 81 % of P_t; and enzymatically hydrolysable P (P_et) accounted for 5 to 26 % of P_t. Liquid–solid separation tended to concentrate the manure P in the liquid fractions. In contrast, anaerobic digestion did not affect the manure P distribution compared with the undigested raw manure from the same system. No differences in P distribution were found for the compost bedded pack manure. In the soil incubation study, manure and fertilizer were applied at 40 mg total P kg^?1. Separated liquid manure from two systems tended to increase STP more than the separated solid manures from the same systems. Although anaerobic digestion modified some of the physical and chemical properties of the treated manures, it did not clearly impact how digested manure increased STP compared with the raw manures. Overall, the increase in STP after treated manure application was found to be a function of soil clay content and manure P_it?+?P_et applied.     

Determination of total phosphorus in soil using simple Kjeldahl digestion

Abstract

Following observation of severe chlorosis and dieback of meri‐stem tissue in asparagus seedlings started in the greenhouse in a soilless media, a study was conducted to determine if the growth patterns were associated with one or more of the media components. Asparagus seedling growth using several potting media was compared. Treatments included single component media, washed sand, perlite, peat, Plainfield loamy sand [a local soil (PLS)], plus 1: 1 mixtures of peat/perlite, washed sand/peat, PLS/perlite, washed sand/peat, and PLS/peat. Abnormal growth patterns were observed in several of the media. Chlorosis was associated with high pH which occurred in perlite, washed sand, and their combinations. Chlorotic plants were characterized by low root and fern dry weights and low fern to root ratios. Meristem dieback occurred in several media treatments and did not appear to be pH related. Plants exhibiting dieback had fern to root ratios approaching 1 if they were not also affected by chlorosis. Nutrient availability was suspected to be a cause but this hypothesis was not substantiated by data collected in this experiment. Asparagus growth in a mixture of Plainfield loamy sand and peat was the highest and was similar to that of field grown seedlings.     

流动分析仪快速测定土壤全磷含量

土壤经碱熔法消解,对连续流动分析仪和钼锑抗比色法所测土壤全磷含量进行比较分析,探讨流动分析仪测定碱熔法土壤全磷含量的可行性。结果表明,两种方法测定结果经 t检验,双尾 P(T ≤t)=0.5254,无显著性差异。回归直线方程y(流动分析仪-P)=1.0606x(钼锑抗比色法-P)-0.0191, R=0.9900。流动分析仪测定碱熔法土壤全磷的加标回收率在 98.09%～ 102.89%,3个样品重复测定 5次的相对标准偏差为 1.20%～ 2.07%。流动分析仪精密度与准确性高,试剂用量少,检测效率高,适用于批量土壤全磷的检测分析。     

Spatial distribution of soil nutrient at depth in black soil of Northeast China: a case study of soil available phosphorus and total phosphorus

Purpose

The spatial variability of soil available phosphorus (AP) and total phosphorus (TP) influences crop yield and the environment. The paper aims to identify the spatial heterogeneity of P (AP and TP) and clarify the main driving mechanisms in a Mollisol watershed of Northeast China.

Materials and methods

Both geostatistical and traditional analysis were used to describe the spatial distribution of P at different depths. P in cultivated fields on the upper slopes was compared with secondary forest areas on the lower slopes within the same watershed.

Results and discussion

The horizontal distribution of P was found to be primarily influenced by structural factors (58–95 %). TP was high at both the summit and the bottom of slopes at all depths, being especially high at the watershed outlet due to erosion on the back slope and deposition at the base. AP was higher on south-facing slopes than on north-facing slopes and typically decreased from the summit to the base of south-facing slopes at the 0–40-cm depths, mainly due to solar radiation, soil loss, and water loss. The vertical distribution of TP typically decreased with increasing depths in farmland but did not show systematic variation in the forest profiles. AP was lower in the middle of the 0–60-cm soil profiles in the farmland, reflecting the influence of fertilization, infiltration, and crop absorption. AP in the 30–60-cm and TP in the 20–60-cm layers were lower in farmland than in the secondary forest, and only 2 % of the area showed a risk of P loss through ground flow and infiltration in the 0–20-cm layer.

Conclusions

The horizontal distribution of P in the 0–60-cm layers was mainly influenced by soil and water loss, deposition, and hydrothermal dynamics, while the vertical distribution of P, especially AP, was more affected by fertilization, infiltration, organic matter, and crop absorption. Secondary forestland that had been converted from farmland was found to effectively hold P, especially in deep soil layers, as the loss of P dissolved in water is not a primary process.     

国标土样在土壤有效磷含量检测和质控中的应用

定期使用有证标准物质可验证试验数据准确性,以发现操作者、仪器、材料、方法、环境中出现的超限现象,能有效地监控试验过程,提高检测质量。本试验研究了国标土壤对土壤有效磷测定数据进行控制,保证试验数据可靠性。结果表明,除2010月4月27日结果不稳外,其余测定值在16.4～19.8 mg/kg,相对标准偏差(RSD)为6.20%;质控图有93%试验点在上下辅助线内,未发现连续7个点位于中心线同一侧,质控图可靠;同时期相比2011年上半年测得国标土壤有效磷含量高于2010年,数值多稳定在18.3 mg/kg以上,精确度和准确度均以2011年较好。     

Laboratory study of phosphorus forms and test procedures on soils under aerobic and anaerobic conditions

The inorganic forms of phosphorus in nine samples of surface soils from the Nainital Tarai of India were determined by a series of extractions with different reagents after incubation for 45 days under aerobic or anaerobic conditions. The forms of phosphorus in samples incubated under aerobic conditions and the pH range of 7.2–8.5 indicated that the soils had been subject to slight chemical weathering. Anaerobic incubation to simulate conditions in lowland rice paddies converted part of the inorganic phosphorus into more labile forms, based on changes in amounts of isotopically exchangeable phosphorus. Amounts of the element converted to more labile forms differed among the nine soil samples.A better correlation was found between amounts of phosphorus extracted by 0.5M NaHCO³ (Olsen's method) than by 0.03N NH₄F in 0.25N HCl (Bray's method) and the isotopically exchangeable phosphorus. The better correlation suggests that the bicarbonate extraction would be the better method for estimating “availablelrd phosphorus in soils of lowland rice paddies. Recalibration of the test prior to such use seems desirable to allow for increases in amounts of phosphorus in labile forms after soils have been shifted from aerobic to anaerobic conditions.     

Soil phosphorus testing: 1. studies on spatial variation of colwell soil test phosphorus

Abstract

Spatial variation of soil test phosphorus (P) was studied by measuring soil‐test P for individual soil samples collected from uniform areas in south‐western Australia. The soil samples were collected using standard 10 cm deep by 2.5 cm diameter samplers. The Colwell alkaline bicarbonate soil test, the standard reagent adopted in Western Australia, was used. There were two parts to this study. In Part 1, 36 individual soil samples were collected on 20 m by 20 m grids within a uniform 100 m by 100 m area in paddocks on 16 different lateritic soil types. Superphosphate had been applied each previous year, using normal farmer practices, for either nine years at two sites or >20 years at the other sites. For pastures, fertiliser is usually applied to the surface. For crops, it is drilled with the seed at about 5 cm depth. In Part 2, 10 to 20 individual soil samples were collected at random locations within experimental plots (either 2 or 4.8 m wide by 30 m long) of five long‐term field experiments that were treated once only with different amounts of superphosphate applied from two to eight years previously. The P was applied to the soil surface and either incorporated through the soil with a rotary hoe or when sowing crops at 5 cm depth with tined implements, or the P was placed at 5 cm depth in bands that were 180 mm apart and the soil was not disturbed thereafter. For each site in Part 1, or each plot of each experiment in Part 2, soil‐test P for the individual soil samples varied, often markedly. Coefficient of variation was large. It was up to 56% for Part 1. For Part 2, it was up to 82% when P was incorporated into the topsoil, and up to 210% when P was banded in the soil. Spatial variation of soil‐test P is attributed to natural variation of soil physical, chemical, and mineralogical properties. Some of the variation may also be due to heterogenous mixing through the topsoil of fertiliser P applied in recent years. Soil‐test P is usually larger for recently applied fertiliser P.     

Comparison of soil phosphorus extraction methods regarding their suitability for organic farming systems

Background

Organic farmers frequently report sufficient yield levels despite low or even very low soil phosphorous (P) contents questioning the applicability of widely used laboratory methods for soil P testing for organic farming.

Aims

The aim of this study was to compare the validity of a broad range of different soil extraction methods on soils under organic management from South West Germany and to test the correlation of the measured soil P concentration with plant offtake.

Methods

Twenty-two soil samples of eight different organic farms were extracted with different solutions: (1) water, (2) CAL, (3) Olsen, (4) Mehlich 3, (5) Bray P1, (6) Bray P2, (7) NaOH+Na₂EDTA, and (8) total P. The results were then correlated with above ground plant P.

Results

Spearman's rank correlation coefficient (r_s) of correlations between above ground plant P and extractable soil P (Water-P, CAL-P, and Olsen-P [+active charcoal {+AC}]) determined with ICP-OES were strong (0.94, 0.90, and 0.93, respectively). Among the tested methods, above ground plant P showed a strong correlation with CAL-P as detected by ICP-OES (r_s = 0.90) and colorimetry (r_s = 0.91). The comparison of CAL-P data provided by farmers and CAL-P analyzed during this research showed discrepancies between the results.

Conclusions

The results of this study indicate that the CAL method can be used in organic farming despite a low extraction of organic P (P_org). Furthermore, it is recommended for farmers to take soil samples for analyses regularly and interpret changes in P in the long-term instead of interpreting individual samples.     

河南省土壤全磷质量分数时空变异分析

采用传统统计学、GIS和地统计学的方法分析河南省1982和2009年土壤全磷的时空变异特征。结果表明：1）研究区2个时期土壤全磷半变异函数拟合模型均为球状模型,均存在中等空间相关性;2）土壤全磷平均质量分数由1982年的0.56 g/kg增加为2009年的0.66 g/kg,增幅为17.86%,平均年增长水平为0.66%,其中豫东地区由0.65 g/kg变为0.83 g/kg,增幅27.69%位居全省第1位,豫南地区以6.12%增幅最低;3）主要土类中,全磷质量分数以主要分布在平原区的砂姜黑土、水稻土和潮土的增幅最大,增幅分别为29.55%、29.27%和18.46%,主要受秸秆还田以及施用有机肥等人为活动的影响,此外,黄棕壤中全磷平均质量分数有所下降,下降幅度为6.45%。     

基于可见/近红外光谱技术的土壤总磷分析研究

Overabundance of phosphorus (P) in soils and water is of great concern and has received much attention in Florida, USA. Therefore, it is essential to analyze and predict the distribution of P in soils across large areas. This study was undertaken to model the variation of soil total phosphorus (TP) in Florida. A total of 448 soil samples were collected from different soil types. Soil samples were analyzed by chemical reference method and scanned in the visible/near-infrared (VNIR) region of 350--2 500 nm. Partial least squares regression (PLSR) calibration model was developed between chemical reference values and VNIR values. The coefficient of determination (R²) and the root mean squares error (RMSE) of calibration and validation sets, and the residual prediction deviation (RPD) were used to evaluate the models. The R² in calibration and validation for log-transformed TP (log TP) were 0.69 and 0.65, respectively, indicating that VNIR calibration obtained in this study accounted for at least 65% of the variance in log TP using only VNIR spectra, and the high RPD of 2.82 obtained suggested that the spectral model derived in this study was suitable and robust to predict TP in a wide range of soil types, being representative of Florida soil conditions.     

森林土壤全磷测定中酸溶法的优化

在标准LY/T 1232-2015《森林土壤磷的测定》基础上,通过多个实验对比总结,对土壤全磷测定中酸溶法进行了优化。原方法中,以二硝基酚作为指示剂,2 mol/L氢氧化钠溶液和0.5 mol/L硫酸溶液调色,从黄色到刚呈淡黄色,颜色变化不明显,肉眼判断误差极大。优化后采用硫酸-高氯酸酸溶法消解,以酚酞作指示剂,4 mol/L氢氧化钠溶液和0.5 mol/L硫酸溶液调色,从红色到无色,颜色更为清晰,操作更为简便,结果更为可靠。