甲亚胺测定土壤有效硼的前处理方法研究

土壤有效硼测定通常采用甲亚胺-H比色法,该方法前处理(煮沸)过程分析效率低、操作步骤不易掌控,极易给测定结果带来较大误差。为此,以山西省标准土样TCB-2为检测样品,对甲亚胺-H比色法的煮沸提取步骤进行了改进,分别试验了水浴提取、微波提取时间对土壤有效硼测定的影响,确定水浴法最佳提取时间为50 min,微波提取时间为90 s。对国家土壤标准物质GBW07412a检测结果表明,水浴提取和微波提取测定结果与标准参照值符合,相对标准偏差分别为3.43%和8.91%。     

Experimental Evaluation of Procedures to Quantify Carbohydrate Carbon in Some Calcareous Soils

Carbohydrates are an important component of soil organic matter, and a method is needed to quantify them, which would be efficient in terms of time and cost. Different extractants and methods were examined in this work for their efficiency to extract carbohydrate C from four calcareous soils. Four extractants (distilled water, 0.5 M potassium sulfate (K₂SO₄), and 0.25 and 0.5 M sulfuric acid (H₂SO₄)) and three incubation methods (shaking for 16 h, heating in an oven (85 °C) for 16 h, and heating in a water bath (85 °C) for 2.5 h) were compared. The results show that significantly more carbohydrate C was extracted from all four soils with oven and water bath heating of the soil–extractant suspensions than with shaking them at room temperature. The efficiency of the extractants decreased in this order: 0.5 M H₂SO₄ > 0.25 M H₂SO₄ > 0.5 M K₂SO₄. The combination of the heated–water bath incubation method with 0.5 M H₂SO₄ as extractant was the most efficient method.     

运用四苯硼钠法准确测定土壤有效钾素变化的初步探讨

通过室内实验探讨了四苯硼钠法用来测定土壤有效K素变化的效果及其提取条件。结果表明,四苯硼钠法提取的土壤K量因四苯硼钠浓度、提取时间以及提取温度而有显著的变化。选择较高的四苯硼钠浓度、较长的提取时间或较高的提取温度均会显著促进四苯硼钠对土壤中非交换性K的提取。研究初步提出的一种土壤有效K素变化的测定方法,从12种土壤中提取的K量分别为各土壤常规缓效K值的2.3～7.4倍。当土壤添加100～2500mg/kg的外源K后,12种土壤中用该法测定的K素变化的回收率绝大多数在90%～110%之间,平均为101.9%±8.2%,说明改进后的四苯硼钠法将可以用来测定土壤中的有效K素变化。     

Extraction of boron from soil by microwave heating for ICP‐AES determination

Abstract

Extraction with hot water is the most widely used procedure to determine boron (B) in soils for the diagnosis of the nutrient availability for plants. However, this procedure is tedious for routine conditions and requires some special precautions. An alternative extraction procedure was developed, consisting in the extraction of B with a 1.25 g/L solution of barium chloride (BaCl₂) or with water heated in a domestic microwave oven. Boron was determined either by inductively coupled argon plasma emission spectrometry (ICP‐AES) and by spectrophotometry with azomethine‐H. Good correlations were found between the extraction by boiling water under reflux and the extraction by the microwave heating for 13 Brazilian soils, and the contents of B obtained by spectrophotometry did not differ significantly from those obtained by ICP‐AES. Considering the calculated standard deviations, it can be concluded that microwave heating followed by ICP‐AES determination is an adequate procedure for the determination of hot water extractable B in soils.     

Degradation of ginsenosides in American ginseng (Panax quinquefolium) extracts during microwave and conventional heating

The degradation of ginsenosides in American ginseng (Panax quinquefolium) extracts during microwave and water (oil) bath heating (conventional heating) was investigated. Both the 50% ethanol-water extracts and the aqueous extracts were boiled in a modified laboratory microwave oven and in a water (or oil) bath, respectively. The neutral ginsenosides (Rb(1), Rc, Rd, and Re) and malonyl ginsenosides (m-Rb(1), m-Rc, and m-Rd) were determined by reverse-phase high-performance liquid chromatography. The results showed that the degradation of ginsenosides in 50% ethanol-water extracts was a first-order reaction. The malonyl ginsenosides were much less stable than the corresponding neutral ginsenosides, with the rate constant value of the malonyl ginsenosides being 3-60 times that of the neutral ginsenosides. At the same temperature, the effect of microwave heating on the degradation of ginsenosides was the same as that of conventional heating.     

Evaluation of a rapid microwave digestion method for determination of total organic carbon in soil

Precise measurement of soil organic carbon (SOC) is essential for constructing regional inventories, developing best agricultural management practices, and modeling purposes. Currently, the automated dry combustion method is considered standard, but the method is both costly and time-consuming. There is a need for a simple, easy to use and cost-effective method of organic C determination in soil. A simple method of total organic carbon (TOC) determination in soil that involved wet digestion of K₂Cr₂O₇-H₂SO₄-soil mixture in a commercial microwave oven followed by spectrophotomteric measurement of Cr (III) was evaluated. The method was compared with automated dry combustion and two other wet digestion methods. The method showed close agreement with dry combustion method (R² = 0.90; root mean square error = 0.70) and the TOC measured with the two methods did not differ for a range of soils drawn from lowland and upland land-uses and varying in pH (6.2–9.3), TOC (2.8–14 g kg^?1), and calcium carbonate content (0–6.7%). The recovery of the added organic C by the microwave method was 98.6 ± 4.2%. The results suggested that microwave-spectrophotometric method could be easily adopted in routine soil analysis as it is not only precise, rapid, and cost-effective but also produced small volume of reagent waste.     

Elemental analysis of solid samples by low temperature plasma ashing and microwave acid digestion

Sixteen elements (Mn, Zn, Cu, Fe, B, Sr, Ba, Cr, Pb, As, Cd, Ni, Co, Se, Sb, Hg) were determined in oils, sediments, plants and marine organisms by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) or by Graphite Furnace Atomic Absorption Spectroscopy (GF-AAS) after plasma ashing followed by microwave acid digestion with HNO₃/HCl/H₂O₂. Soil and sediment samples were treated directly in the microwave oven without ashing, but the complete procedure must be applied in case of high organic content. The method was tested on a variety of standard reference materials. Good recoveries were obtained for most of the considered trace elements with less time and reagents consumption than conventional open vessels acid digestion procedures. Hg was determined with good recovery in soil samples by the same method and in organic materials by a modified procedure involving digestion of fresh material with nitric acid in a reflux quartz system.     

石灰性土壤供氮能力几种化学测定方法的评价研究

以采自于黄土高原差异较大的25个农田耕层石灰性土壤为供试土样,以淋洗和未淋洗土壤起始NO3--N小麦和玉米两季盆栽试验作物累积吸氮量为参比,对8种反映旱地土壤供氮能力的化学方法进行比较研究。结果表明,在一定程度上,可用有密切关系的土壤全氮或有机质,反映有机氮或全氮存在较大差异的土壤供氮能力,但其灵敏性较差。石灰性土壤矿质氮,特别是NO3--N与未淋洗土壤起始NO3--N作物吸氮量之间有较高相关性(r=0.884,P0.01),而与淋洗土壤起始NO3--N作物吸氮量间相关系数仅为0.472(P0.05),说明矿质氮可反映土壤当前供氮水平,而不能反映土壤潜在供氮能力;石灰性土壤起始NO3--N对各化学方法与作物吸氮量之间相关性影响较大。酸性高锰酸钾法既可反映土壤潜在供氮能力,也可反映土壤总供氮能力;酸性高锰酸钾法的修订方法,即硫酸高锰酸钾法提取出的NH4+-N值接近于KCl水浴法提取出的NH4+-N值,该方法在反映土壤总供氮能力方面与酸性高锰酸钾法相当,但在反映土壤潜在供氮能力方面不及酸性高锰酸钾法优越。KCl水浴法在评价石灰性土壤供氮能力方面,与酸性高锰酸钾法的效果基本相同;沸水浸取法和NaHCO3-UV法在评价石灰性土壤供氮能力方面效果较差。总结以上发现,在以盐类溶液提取法中,酸性高锰酸钾法、硫酸高锰酸钾法和KCl水浴法可作为反映石灰性土壤供氮能力的化学方法,其中以酸性高锰酸钾法最优,其次为KCl水浴法和硫酸高锰酸钾法。这3种方法在不包括起始NO3--N时,可反映石灰性土壤潜在供氮能力;包括起始NO3--N后,可反映土壤总供氮能力(当前供氮能力+潜在供氮能力)。     

不同加热方式对南美白对虾品质变化的影响

为探讨不同加热方式对南美白对虾营养品质的影响,以南美白对虾为原料,采用微波、蒸汽、沸水3种加热方式对其进行处理,并对其质构、色泽及蛋白成分的变化进行分析。结果表明,南美白对虾的最适加热时间为90 s,此条件下微波加热组对虾失水率分别是蒸汽加热组、沸水加热组的1.55倍和1.48倍;微波加热组和蒸汽加热组对虾的硬度相近且均显著高于沸水加热组(P<0.05);微波加热组对虾的弹性和咀嚼性均显著高于其他2种加热方式;微波加热组和沸水加热组对虾的呈色特征值均显著高于蒸汽加热组(P <0.05),但3种加热处理组对虾的内聚性无显著差异。微波加热组对虾的盐溶性蛋白损失较其他2种加热方式小,但水溶性蛋白含量低于其他加热组;微波加热组对虾的碱溶性蛋白含量最高,其次为沸水加热组。本研究结果为南美白对虾热加工方式提供了一定的技术指导。     

土壤中有机酸比色法测定的研究

对Montgomery(1962)比色法测定有机酸总量的方法作了若干改进。根据化学反应的平衡关系,将欲测试的土壤提取液水浴蒸干脱水,大大提高了有机酸的酯化程度,也就提高了测定的准确度。由于提取液浓缩至干,故测定一般可不受吸取的提取液体积和其中有机酸浓度高低的影响。结合温度、时间、pH等条件试验得到了测定的最佳条件。乙酸和丁酸的回收率分别可达99%和102%。几种有机肥料淹水培育10天用气相色谱测定的乙酸含量为本文提出的比色法测定总量的86%。采用这一方法测定土壤有机酸的量,可以在一定程度上反映有机物在土壤中腐解时产生有机酸的实际情况。     

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).     

An application of a modified microwave total dissolution technique for soils

Abstract

Application of a microwave dissolution technique to soil materials aided by acid digestion procedures has many advantages, but the incomplete dissolution of sandy soils has been noted. The objectives of this study were to modify a microwave oven digestion technique to facilitate the determination of the total elemental content of soils and geologic materials containing greater than 45% sand and apply these data to determine natural separations in parent materials. A microwave dissolution technique using aqua regia (HNO₃ and HCl) and hydrofluoric acid (HF) was modified such that the HF is added to the solid 16 hours prior to aqua‐regia addition and subsequent microwave heating. Elemental recoveries were validated using a NBS coal fly ash standard. This procedure was applied to soil core samples representing a wide range of geological and pedological weathering sequences and soil textural classes. Separations in the parent material were determined by observing natural breaks in the elemental concentrations and comparing them to soil morphology data.     

Mercury intrusion porosimetry of some New Zealand soils in relation to clay mineralogy and texture

Pore size distributions in the 10/10⁴ nm e.c.d. range in aggregates from three New Zealand soils with largely monomineralic clay fractions, were determined by mercury porosimetry after oven drying and also after critical point drying following methanol and then CO² exchange from a range of water contents. A soil containing halloysite showed considerable porosity in the fine pores (10–30 nm) regardless of the method of drying. A smectitic soil showed virtually no porosity in the 10²–10⁴ nm range when oven dry. A soil containing allophane was dominated by large pores (> 10³ nm). The change from a fine (clayey) to a coarser (clay loam) texture within the profile of one soil was reflected in an increase in large pores.     

Determination of organic carbon in soils and fertilizers

Abstract

Many methods have been proposed to determine the total amount of organic carbon in soil; some of them determine only a percentage of the actual carbon content and therefore the results need the application of a correction factor. Methods for the determination of organic carbon in soil have been rarely extended to organic fertilizers and amendments.

We propose a rapid method based on a modification of the original Springer and Klee¹⁰procedure. Samples are oxidized for exactly 10 minutes with a mixture of 20 ml 2N K₂Cr₂O₇and 26 ml conc. H₂SO₄at 160±2°C; the excess dichromate is titrated either potentiometrically or manually with FeSO₄.

The method is fast, accurate, and more reliable than other commonly used procedures. The procedure can be easily adopted for serial determination of carbon in both soils and organic fertilizers or amendments     

Kinetics of the hot water soluble boron soil test

Abstract

A first order reversible reaction rate equation was modified to fit the conditions of the hot water soluble boron soil test. This equation was fitted to a boiling time study on one soil fertilized to three different boron levels. The common S‐minute boiling time did not remove enough boron to reach the plateau region of the fitted curve for any sample. It was also found that boiling for too short a time causes more error than excessive boiling. For these samples a boiling time could be more than a minute too short before a 10% error was introduced in the amount of boron extracted. A 10‐minute boiling time would reduce the timing error for these samples by removing enough boron to reach the plateau region of the extraction curve.     

Mineral balance in milk heated using microwave energy

Milk heated to 75 and 85 degrees C in a water bath or in a microwave oven was assayed for changes in salt partitioning after cooling to room temperature. To properly to assess differences and draw valid comparisons, the two heating methods used in the experiment were applied to samples for identical exposure times, and the samples were heated to attain the same final temperatures. Although the soluble Ca and P(i) contents were lower in the heated milk samples, no significant differences in salt partitioning were found between microwave and conventional heating. Ionic calcium levels in the milk samples pasteurized using microwave energy were very close to the levels in the samples heated in a conventional water bath (approximately 90% of the level in the untreated milk samples). The microwave heating-induced changes were completely reversed after storage at 20 degrees C for 24 h. The coagulation properties of the heated milk samples were also examined, and the coagulation time was longer and the curd formation rate slower in the microwave-heated milk than in the raw milk. Still, the experimental results demonstrated that microwave heating was no more detrimental to the milk than conventional heating and could thus be used for pasteurization purposes.     

土壤混掺生物炭对微咸水蒸发特性的影响

为探究不同生物炭混掺量对微咸水蒸发特性的影响,采用离心机试验和室内土柱模拟试验,设置3个生物炭质量添加比例(B₀、B₂、B₄)和4个微咸水矿化度(W₀、W₁、W₃、W₅),分析不同处理对微咸水蒸发下的土壤水分特征曲线、孔隙分布、累积蒸发量、盐分运移、土壤温度日变幅的影响,并应用蒸发模型进行拟合分析。结果表明:生物炭和微咸水联合应用下能提高土壤持水能力,增加土壤中的较大孔隙和较小孔隙的比例;土壤累积蒸发量随着生物炭混掺量的增加先减少后增加,生物炭混掺量为2%时可以更好地抑制微咸水蒸发;Rose蒸发模型可以较好地拟合微咸水蒸发;土壤中混掺生物炭可以降低盐分表聚,使其在土壤中均匀分布;混掺生物炭可以有效降低土壤温度日变幅;相同生物炭施用量下,矿化度为3 g/L的微咸水,可以降低0—10 cm土层土壤平均温度,提高10—50 cm土层土壤平均温度。综合考虑各项指标,处理B₂W₃的生物炭和微咸水更适宜农田施用,为西北干旱地区更好地利用微咸水灌溉提供理论依据。     

石灰性土壤起始NO3——N对土壤供氮能力测定方法的影响

在陕西省的澄城、永寿、杨陵 3地区选取有机质、全N、硝态N含量差异较大的 17个石灰性土壤 ,分别在淋洗与未淋洗土壤起始NO3--N后 ,利用盆栽试验探讨土壤NO3--N淋洗前、后 ,不同方法测定的已矿化N和可矿化N与小麦吸N量之间的相关性。结果表明 ,未淋洗土壤起始NO3--N ,用KCl直接浸取、KCl煮沸法所浸取以及通气培养前CaCl2 所淋洗的起始NO3--N均与小麦吸N量密切相关 ,相关系数 (r)分别为 0.934 ,0.856和 0.862 ,均达1%显著水准。与此相反 ,通气培养、淹水培养、沸水煮沸、碱性高锰酸钾、酸性高锰酸钾及碱解扩散等方法所提取的可矿化N与小麦吸N量间无显著相关。淋洗土壤起始NO3--N后 ,用KCl直接浸取、KCl煮沸法浸取以及通气培养前CaCl2 所淋洗的起始NO3--N与小麦吸N量之间的相关系数明显降低 ,达不到 5%的显著水准。而通气培养、淹水培养、沸水煮沸、碱性高锰酸钾、酸性高锰酸钾及碱解扩散等方法所提取的可矿化N与小麦吸N量之间相关系数却明显提高 ,都达到 5%或 1%的显著水平。其中变化最明显的是淹水培养 1周矿化出的NH4+-N、通气正式培养 2周矿化出的NO3--N及碱解扩散出的NH4+-N ,其与小麦地上部吸N量之间的相关系数 (r)分别由淋洗前的0.443,0.119,0.259增加到淋洗后的 0.866 ,0.767,0.763。说明可矿化N反映土壤供N能力不佳是因为受起始NO3--N的干扰和影响，在土壤NO3--N含量较高的情况下，要正确评价可矿化N测定方法必须考虑NO3--N的作用。     

Determination of total sulfur in soils and plant materials by ion chromatography

Abstract

An accurate and precise ion Chromatographie (IC) method is described for determination of total S in soils and plant materials. It involves ignition of a mixture of soil and NaHCO₃or plant material and NaHCO₃containing Ag₂O at 550°C for 3 h. The residue is dissolved in 1MHOAc, diluted with deionized water, filtered, and analyzed for S0^2‐ ₄by a Dionex model 2002i ion Chromatograph. Results by the IC method of seven Iowa soils, three Chilean soils, and 10 plant materials agreed closely with those obtained by the methylene blue method after alkaline oxidation with NaOBr. In general, the IC method was more precise than the methylene blue method. The method is simple and requires a minimum of analytical skill. A single operator can analyze 30–40 soil or plant samples in a normal working day.     

酸性土壤水溶性氟浸提方法的研究

本文比较研究了振荡、超声、沸水浴和烘箱4种浸提酸性土壤水溶性氟的方法,然后采用离子色谱法对浸提液进行测定,并通过对测定数据进行统计与方差分析来确定最佳浸提方式。结果显示,水土比5:1,浸提时间20 min、温度60℃是振荡法与超声法浸提酸性土壤水溶性氟含量的最佳条件。在此条件下,振荡法与超声法浸提的土壤水溶性氟含量无显著差异,标准偏差均小于0.3%。超声法浸提的酸性土壤水溶性氟含量显著高于各自最佳处理条件下的沸水浴法与烘箱法浸提的水溶性氟含量。在离子色谱测定水溶性氟过程中,质量控制样品均在1倍标准偏差范围内。因此,采用离子色谱法测定超声法或振荡法浸提的酸性土壤水溶性氟是一种可行的、准确的试验方法,特别对于批量土壤样品的测定具有重要意义。