新镉试剂高灵敏度分光光度法测定酸性土壤中的有效态镉

本文用0.1N硫酸作为土壤中有效态镉的提取剂,在非离子型表面活性剂OP存在下,镉(Ⅱ)与新镉试剂的高灵敏度分光光度法测定酸性土壤中的有效态镉。在Na_2B_4O_7—NaOH介质中,新镉试剂与镉(Ⅱ)生成红色络合物,最大吸收位于520nm处,表现摩尔吸光系数为1.64×10~5L/mol·cm方法灵敏度高且选择性好,准确度和重现性都令人满意。     

氢化物发生原子荧光法在测定土壤中浸出硒、总硒的应用

应用氢化物发生原子荧光光谱法研究了测定基地土壤中的浸出硒、总硒的技术。称取一定量土样置于烧杯中,加蒸馏水间歇手动搅拌2小时后放置过夜,取上清液测有效硒;用HNO3-HF-HClO4分解法全量消解样品,同时做全程空白实验,样品处理后加入10%硫脲-10%抗坏血酸混合改进剂以消除Cu、Ag、Ni、Pd等金属离子的干扰,并以1%硼氢化钠为还原剂,在25%的盐酸介质中测定总硒。其浸出态硒测定的检出限为1.5×10-3mg/kg,总硒测定的检出限为0.032mg/kg。     

不同提取剂提取酸性土壤有效态Cu和Cd的方法研究

选择HCl（1#）、HOAc（2#）、NaNO3（3#）和CaCl2（4#）、NH4OAc（5#）、NaOAc（6#）6种不同的提取剂提取某冶炼厂周边重金属污染水稻田土壤中有效态Cu和Cd。结果表明，对土壤有效态Cu，各提取剂按提取量排序为：1#〉2#〉5#〉4#〉3#〉6#，对土壤有效态Cd，各提取剂按提取量排序为：1#〉5#〉2#≈4#〉6#〉3#，有效态Cu的提取量因提取剂种类不同差异较Cd大；4#、5#两种提取剂对土壤有效态Cu和Cd的提取结果变异范围较集中，实验结果相对较稳定；各提取剂提取土壤有效态Cu和Cd的量与其在土壤中全量都显著相关，仅5撑提取剂的提取量与水稻籽粒中Cu、Cd的质量比显著相关。综合实验结果的稳定性与土壤重金属有效态的实际意义，NH4OAc（5#）为最适合提取该研究土壤中有效态Cu和Cd的提取剂。     

氯化钡浸提法测定土壤可交换酸度

建立了氯化钡浸提测定酸性土壤可交换酸度的方法，优化了水土比、土壤粒度、浸提液质量浓度、浸提次数、震荡时间等试验参数。方法检出限为0．016cmol／kg，经重复性和再现性检验表明精密度良好。该方法可同时用于土壤可交换性氢和可交换性铝的测定。     

测定降水pH的误差及其消除方法

一、接界电位的误差及消除 1.配制低离子强度校准溶液 用市售的高离子强度的0.05MC_6H_4(COO)_2HK(pH=4.00λ=2520μS/cm·25℃),0.025MKH_2PO_4和0.025 MNa_2HPO_4(pH=6.86λ=4000μS/cm·25℃)作校准溶液(A液),测定一组降水样品的pH。然后配制低离子强度的5℃10~(-5)MHNO_3(pH=4.30,λ=16.6μS/cm·25℃),5×10~(-4)MKCl(pH=5.64,λ=64μS/cm 25℃)作校准溶液(B液),测定同一组降水样品的pH,结果见表1。     

异丙醇增感电感耦合等离子体质谱法直接测定土壤和沉积物中硒

提出了沸水浴混合酸法消解,以异丙醇为增感剂,电感耦合等离子体质谱直接测定土壤和沉积物中硒的方法。实验表明2mol/L硝酸-4mol/L盐酸混酸能有效溶出土壤和沉积物中各种形态的硒。相对于1%硝酸基体,4%(V/V)异丙醇基体中硒的ICP-MS响应值提高了12.1倍;而且4%(V/V)异丙醇基体可有效抑制硒的质谱干扰。ICP发射功率和雾化气流速是影响异丙醇在ICP-MS测定过程增敏效应的主要因素。以78硒为测定同位素,方法检出限为0.005mg/kg,实际样品测定精密度均小于5%。用于测定土壤和沉积物国家标准样品并对其消解液进行加标回收实验,结果令人满意。     

荧光法测定生物材料中微量硒

硒是动物和人类必须的微量元素,某些地区水、土壤、植物中硒含量很高而导致家畜发生地方性疾病,硒含量缺乏会使人类诱发心血管疾病和癌症,已引起国内外许多科学家的特别关注。生物样品中痕量硒的荧光法测定,具有灵敏度高,选择性好,操做简便等优点,但样品的消解方法十分关键。 K.Wmiehacl等,比较研究了HNO_3-Mg(NO_3)_2及     

王水消解—原子荧光法测定土壤中的硒

样品经(1+1)王水于沸水浴中加热消解,用氢化物发生-原子荧光法测定土壤中硒的含量。对测定的影响因素:HCl浓度、KBH4浓度及共存离子的干扰等试验条件做了研究并予以优化。荧光强度与硒的质量浓度在30μg.L-1以内呈线性关系,方法的检出限(3s/b)为0.1μg·L-1,方法的相对标准偏差(n=6)小于5%,应用此法对标准物质ESS-3和土壤样品进行分析,测得硒的回收率在90%～110%之间。     

土壤元素背景值在农业应用上的探讨

1.Cu和Zn的生理功能对植物的有效性和应用Cu和Zn是植物需要的营养元素,土壤中Cu和Zn对植物的可给强度、活化率大小受PH、质地、有机质、粘土矿物、水、气等各种因素的综合影响.缺Cu能抑制蛋白质分解,作物缺Cu叶片容易缺绿,禾谷类不能结实.根据吉林省土壤耕层有效态Cu平均含量为1.36ppm,变化范围为0～37.5ppm大于1.00ppm的土壤占50%,可见吉林省土壤有效Cu是比较丰富的,尤其是中部的草甸土、沼泽土、黑土以及东部白浆土、棕壤和暗棕壤有效Cu的含量都比较丰富.土壤活化率7～8%.只     

测定废弃泥浆中的Cr(Ⅵ)的高效浸提方法研究

研究了废弃泥浆中的Cr(VI)提取测定方法并与土壤的浸提方法进行比较。结果表明,用0.1mol/L的KH2PO4为提取剂高速搅拌离心,分离提取液,可简单、快速、准确地测定废弃泥浆中的Cr(VI)。该方法的相对标准偏差为0.6%~2.5%,加标回收率86%~98%。     

氯化亚锡还原光度法测总磷的改进

通过大量试验,对氯化亚锡还原光度法测定总磷过程中如何延长氯化亚锡、磷酸二氢钾试剂的使用保存期、提高显色的稳定度、降低空白值,提出了切实可行的改进方法。     

靛红褪色光度法测定废水中苯酚

基于KH2PO4-Na2HPO4缓冲介质中,痕量苯酚对高碘酸钾氧化靛红反应有催化作用,建立了测定废水中苯酚的催化动力学方法.优化了试验条件,讨论了缓冲溶液酸度、试剂体积、加热时间和反应温度对试验的影响.方法在0.08 mg/L～2.0 mg/L线性关系良好,检出限为5.3×10-3 mg/L,加标回收率为97.6%～103%,实际样品测定结果与4-氨基安替比林法对照,结果令人满意.     

Investigation of arsenic speciation on drinking water treatment media utilizing automated sequential continuous flow extraction with IC-ICP-MS detection

Three treatment media, used for the removal of arsenic from drinking water, were sequentially extracted using 10 mM MgCl2(pH 8), 10 mM NaH2PO4(pH 7) followed by 10 mM (NH4)2C2O4(pH 3). The media were extracted using an on-line automated continuous extraction system which allowed the arsenic in each of the extraction fluids to be speciated on-line using IC-ICP-MS. The 10 mM MgCl2 preferentially extracted As(III) from each of the media. The percentage of the arsenic extracted by the MgCl2, relative to a HNO3/H2O2 digestion of the media, ranged from 0.1-2.3% for the three solids. The next sequential extraction fluid, 10 mM NaH2PO4, extracted some of the residual As(III) remaining on each of the media but the predominant species extracted was As(V). The 10 mM NaH2PO4 extracted 15.3 to 42.8% of the total arsenic relative to a total digested concentration for each of the media. The As(III) and As(V) stability studies conducted in these two extraction fluids indicated that conversion between As(III) and As(V) was not significant for the short extraction fluid sample contact time associated with the on-line continuous flow extraction cell. Finally, the 10 mM (NH4)2C2O4 extraction fluid was utilized in an off-line analysis mode because the Fe and As concentrations extracted from the media were not compatible with direct ICP-MS detection. The (NH4)2C2O4 extracted 2.9-29% As(III) for all three media and caused an oxidation of As(III) to As(V) during the extraction period for one of the three media. The sum of the arsenic from each of the three extraction fluids represented 92%, 44% and 53% of the available total arsenic for the three media, respectively. The speciation results for each media were obtained by adding all the speciation results from all three extraction fluids together and the resulting distribution of As(III)/As(V) compared well with the speciation results obtained via XANES.     

土壤和底泥中砷、铬、锰测定的前处理技术

试验了土壤和底泥中砷的前处理技术，其目的是能对土壤、底泥中砷、铬、锰在一次前处理中制备成试液，比色法分析。试验表明，用Ｈ２ＳＯ４－Ｈ３ＰＯ４－Ｈ２Ｏ２进行前处理是可行的。方法简单、挥发酸雾少，用标准参考物质检验证明，分解完全，数据准确，有粒较好一致性。     

Simultaneous extraction of bromide, chloride, fluoride and sulfate from soils, waste- and building materials

The simultaneous extraction of bromide, chloride, fluoride and sulfate was studied in soils, waste- and building materials. Acid, neutral and alkaline extractants were used; 0.01 mol l(-1) H(3)PO(4), milliQ-water and 0.01 mol l(-1) NaOH, respectively. The extracts were analysed by ion chromatography and ion selective electrode. Extracted concentrations were compared with the amount obtained by an alkaline smelt, as an approximation of the total extractable content. The results indicate that there is a significant difference in extraction behaviour between waste- and building materials and soils. Bromide and chloride were in general completely extracted from the former solid materials, but less than 10% and 50%, respectively, from soils. Fluoride is strongly bound in all investigated samples; less than 10% of the total content was extracted with any of the three extractants. The fraction of extracted sulfate varied between 4 and 87% of the total content, and was in general larger in waste- and building materials than in soils. Differences in extracted concentration between the 3 extractants occurred mainly for fluoride and sulfate. Extracted bromide was similar with all three extractants and extracted chloride showed differences for the various soil samples only. Increasing the NaOH concentration up to 1 mol l(-1) resulted mainly in an increase of extracted amount of fluoride and for soils also in extracted amounts of bromide and sulfate. Although, the results show that the composition of the solid material strongly influences the final pH of the extract and the extracted amount of investigated anions, application of Milli-Q water as an extractant might be a very fruitful option within the development of the Dutch Building Materials Decree.     

Non-target effect of organic insecticides: effect of two plant extracts on soil microbial biomass and enzymatic activities in soil

Efficacious botanical derivatives can provide an alternative to synthetic pesticides for organic farming systems. However, there is lack of information regarding the side effects of organic pesticides on key soil ecological processes. In this study, we investigated the effects of aqueous extracts from Urginea maritima and Euphorbia myrsinites exhibiting translaminar and systemic activity against pests on microbial biomass and enzymatic activities in soil. Two grams of plant material was extracted with 100 ml of water and then diluted 1:100, 2:100, and 4:100 with distilled water. Diluted plant extracts were applied around hypocotyl of tomato by soil drench. The effect of both plant extracts on microbial biomass C, amount of total N and organic C, and enzymatic activity in soil was significant. After the last application, the highest microbial biomass C was determined in the lowest U. maritima concentration (U 1:100). Soils treated with the highest concentration of U. maritima (U 4:100) had always lower SMBC content than control soil. All concentrations of E. myrsinites decreased microbial biomass C by 18% to 27% compared to the control. Total nitrogen and organic carbon decreased in soils without (control) and with treated U. maritima extract from first application to last application. Phosphatase, urease, and β-glucosidase activities were monitored in plant extract-treated soils. Except U. maritima 1:100 treatments of second and fourth applications, the other treatments of plant extracts negatively affected enzymatic activity in soil. U. maritima and E. myrsinites plant extracts exhibited different effects on soil microbial biomass and activity, probably because of their different chemical contents.     

Hydrocarbon Uptake by Roots of Vicia faba (Fabaceae)

Vicia faba was grown in crude oil polluted soil and its roots were extracted for the detection and estimation of hydrocarbons. Saturated and unsaturated Aliphatic Hydrocarbons (AHs) ranging from C₂₂ to C₃₆ were identified in AHs fraction. However, PAHs were not present in the same extract. This could be due to the fact that PAHs being toxic compounds are not accumulated in the plant root extracts of V. faba grown in crude oil polluted soil. Three phytoalexins were identified and estimated by mass spectrometric analysis in the root extracts of V. faba. These three compounds are 2-t-butyl-4-(dimethyl benzyl) phenol, 2, 4-bis (dimethyl benzyl) phenol and 2,4-bis (dimethyl benzyl)-6-butyl phenol. These phenolics in V. faba are being reported for the first time. These compounds are presumably elicited as a direct stress on crude oil hydrocarbons on the roots of this plant.     

Synthesis of HNO3 from Organic Matter and its Influence on Nutrient Replenishment in Forest Soils

Chemical analyses during a decade of bulk precipitation, throughfall, humus water and soil water in forest plots ranging from sand to silt of Pleistocene origin in Flanders (N-Belgium) prove that previous and present weathering is predominantly due to synthesis of HNO3 from soil organic matter. The HNO3 reacts with silicates and possibly PO4(3-) species, releasing Al, Fe, nutrient base cations and H2PO4-, and is transformed into NO3-. In all soils solubilized Al3+ is predominantly associated with NO3- and with some organic bases in the coarse-textured soils with undisturbed or previously plowed spodic B horizon. The amounts of ions leached, especially Al3+ and NO3-, are much higher in the sandy than in the silty soils as a result of a stronger neutralization of acidity in the silty soils. Nutrients, leached from the soil, have to be replenished in some way for a sustained forest growth. N- and S-species must come from the atmosphere. Basic cations and P-species have to be supplied out of the solid phase. The concentrations of NO3- in the soil water show that the liberation of these elements from the solid phase is performed by HNO3. Especially in the coarse-textured soils the need for NO3- is high. Therefore, instead of being a real hazard for the forest ecological system, supplementary addition of HNO3 or NH3 can be beneficial.     

Elemental uptake and distribution of nutrients in avocado mesocarp and the impact of soil quality

The distribution of 14 elements (both essential and non-essential) in the Hass and Fuerte cultivars of avocados grown at six different sites in KwaZulu-Natal, South Africa, was investigated. Soils from the different sites were concurrently analysed for elemental concentration (both total and exchangeable), pH, organic matter and cation exchange capacity. In both varieties of the fruit, concentrations of the elements Cd, Co, Cr, Pb and Se were extremely low with the other elements being in decreasing order of Mg > Ca > Fe > Al > Zn > Mn > Cu > Ni > As. Nutritionally, avocados were found to be a good dietary source of the micronutrients Cu and Mn. In soil, Pb concentrations indicated enrichment (positive geoaccumuluation indices) but this did not influence uptake of the metal by the plant. Statistical analysis was done to evaluate the impact of soil quality parameters on the nutrient composition of the fruits. This analysis indicated the prevalence of complex metal interactions at the soil–plant interface that influenced their uptake by the plant. However, the plant invariably controlled metal uptake according to metabolic needs as evidenced by their accumulation and exclusion.     

Soil solution extraction techniques for microbial ecotoxicity testing: a comparative evaluation

The suitability of two different techniques (centrifugation and Rhizon sampler) for obtaining the interstitial pore water of soil (soil solution), integral to the ecotoxicity assessment of metal contaminated soil, were investigated by combining chemical analyses and a luminescence-based microbial biosensor. Two different techniques, centrifugation and Rhizon sampler, were used to extract the soil solution from Insch (a loamy sand) and Boyndie (a sandy loam) soils, which had been amended with different concentrations of Zn and Cd. The concentrations of dissolved organic carbon (DOC), major anions (F- , CI-, NO3, SO4(2-)) and major cations (K+, Mg2+, Ca2+) in the soil solutions varied depending on the extraction technique used. Overall, the concentrations of Zn and Cd were significantly higher in the soil solution extracted using the centrifugation technique compared with that extracted using the Rhizon sampler technique. Furthermore, the differences observed between the two extraction techniques depended on the type of soil from which the solution was being extracted. The luminescence-based biosensor Escherichia coli HB101 pUCD607 was shown to respond to the free metal concentrations in the soil solutions and showed that different toxicities were associated with each soil, depending on the technique used to extract the soil solution. This study highlights the need to characterise the type of extraction technique used to obtain the soil solution for ecotoxicity testing in order that a representative ecotoxicity assessment can be carried out.