抗坏血酸溶液配制方法的改进

磷钼蓝法测定水中总磷，所用的抗坏血酸溶液很不稳定，只能保存数周。为延长抗坏血酸溶液的有效使用时间，节约试剂、提高工作效率，提出改进抗坏血酸溶液的配制方法，即在配制抗坏血酸溶液时，加入适量的EDTA和冰乙酸。经实验，该溶液贮于棕色玻璃瓶，放在冰箱中可稳定3个月，使用效果符合测定要求。     

显色酸度对钼锑抗分光光度法测定土壤中总磷的影响

采用碱熔-钼锑抗分光光度法测定土壤中总磷时,显色溶液的酸度影响磷钼络合物的形成和稳定,p H指示剂2,4-二硝基苯酚在环境温度低时配制困难、辨色不明显。分析了显色酸度对吸光值的影响,并对2,4-二硝基苯酚的配制方法进行了改进,方法操作简单,提高了分析结果的准确性。     

孔雀绿显色光度法测定地面水中痕量磷

研究表明,将碱性染料与杂多酸结合成离子缔合物用于光度法测磷,其灵敏度是简单杂多酸体系所无法比拟的。Altmann H.J,,等人报道了磷钼酸盐与孔雀绿的显色反应机理,并指出利用此反应测定地面水中痕量磷的可能性。Shoji M.等人利用钼酸盐与孔雀绿的显色反应,提出了河水中10~(-9)级总无机态磷的光度测定法。本文在前人工作的基础上,以     

水中总磷和溶解性磷酸盐的快速分光光度法

在H_2SO_4溶液介质中,磷钼钒三元杂多酸与孔雀绿反应形成有色络合物,在波长620nm处表观摩尔吸光系数为1.73×10~5L/mol·cm,线性范围是0～0.4(mg/L).检测下限为0.016mg/L,方法准确、稳定,操作简便、快速.能够用于水中总磷和溶解性磷酸盐的测定.     

用钼兰法定量微量磷

1.前言 有磷酸离子存在的溶液呈酸性,如果在溶液中加入钼酸铵,就生成钼磷酸,若将其还原为兰色物质,就生成钼兰。这是一个古老的反应,因可用来定量微量磷酸离子,故对其反应机制和反应条件已进行过众多研究。例如,下式所示为钼磷酸生成反应: XH_3PO_4+YM_o(Ⅵ)=MoP+ZH~+ 钼磷酸的生成速度与H_3PO_4浓度的X倍,     

铋磷钼蓝分光光度法测定土壤中磷含量

土壤中磷含量的分析是土壤环境监测的主要项目之一.建立了铋磷钼蓝分光光度法测定土壤中磷含量的新方法,与现有的《土壤全磷测定方法》(GB 9837-88)和土壤总磷快速检测仪方法进行了比较讨论.方法的检出限为5.0 mg/kg,对磷含量为475 mg/kg和292 mg/kg的标准土壤样品进行测定,结果与标准值吻合,其相对...     

无水乙醇中元素磷的稳定性

元素磷通常指黄磷,不溶于水,属剧毒物,是我国污水综合排放标准中控制排放的污染物之一[1].在用气相色谱法测定水和废水中元素磷时,为使测定条件保持一致、减少测定误差,标准系列常需与水样同时萃取,为此需用无水乙醇来配制元素磷溶液,使元素磷能与水相互溶[2].在实验中发现,室温下,在无水乙醇溶液中元素磷的稳定时间较短,当无水乙醇用抗坏血酸处理后,所配元素磷溶液可大大延长其稳定性.     

河流底泥中甲基汞、乙基汞的测定

介绍了用气相色谱法(ECD)测定河流沉积物中甲、乙基汞的分析方法.前处理采用湿泥样品直接用盐酸溶液浸提,在酸性条件下用苯萃取,然后在中性条件下用盐酸-L-巯基丙氨酸-醋酸钠溶液提取,最后在酸性条件下用苯反萃取,萃取液直接进样分析.     

AB-DTPA浸提ICP-MS法分析土壤中有效钼的研究

采用AB-DTPA浸提剂和电感耦合等离子体质谱法分析,建立了1种土壤中有效钼的分析方法。将土壤用AB-DTPA在(25±2)℃,(180±10) r/min的振荡频率下浸提8 h,电感耦合等离子体质谱法分析,实验结果表明,检出限为0.000 3 mg/kg,测定下限为0.001 mg/kg。通过对标准物质的测定,土壤有效钼与真值的相对误差在-17.4%～-7.5%,数据测试的准确度较好,加标回收率在90.0%～95.7%,能够满足土壤实际样品的分析测试,同时适用于各种类型土壤的批量检测。     

水中单质磷测定方法的改进

探讨了《水质单质磷的测定磷钼蓝分光光度法(暂行)》(HJ593-2010)中存在的问题,并对方法进行了改进.确定测定目标组分为单质磷中的黄磷；改用酸性高锰酸钾氧化体系,去除了有机磷农药的干扰；改用抗坏血酸为还原剂,采用710 nm比色波长,提高了分析灵敏度；用10 mL甲苯一次萃取,对水中黄磷的检出限为0.002 mg/L.     

The contribution of roadside soil to phosphorus loading in the eutrophic Lagos Lagoon, Nigeria

Roadside soils were sampled from the Lagos Lagoon catchment during the wet and dry seasons over the period 2005-2009. Lagoon sediment samples were also collected within the same period. All samples were digested with aqua regia to determine total phosphorus and extracted with 0.5 M sodium bicarbonate to determine the bioavailable fraction (Olsen-P). A segmented flow analyser method was used for analysis and good accuracy was demonstrated for two reference soils (SO-2 from CCMET and SRM 2711 from NIST). The Lagos Lagoon is a hypereutrophic water body (1270 ± 1170 μg P L(-1)), with significant areas of anoxia and water hyacinth growth. The total phosphorus concentrations in roadside soils (16 sites; mean ± 2 S.D.) were 285 ± 279 mg kg(-1) in the wet season and 424 ± 629 mg kg(-1) in the dry season, indicating that rainwater leaching is a major source of phosphorus in the lagoon. The bioavailable fractions were 5.17 ± 3.47 mg kg(-1) (2.1 ± 1.5% of the total) in the wet season and 13.0 ± 8.7 mg kg(-1) (4.3 ± 4.5% of the total) in the dry season.     

Metal immobilization and phosphorus leaching after stabilization of pyrite ash contaminated soil by phosphate amendments

In this study we would like to show the importance of a holistic approach to evaluation of chemical stabilization using phosphate amendments. An extensive evaluation of metal stabilization in contaminated soil and an evaluation of the leaching of phosphorus induced after treatment were performed. The soil was highly contaminated with Cu (2894 mg kg(-1)), Zn (3884 mg kg(-1)), As (247 mg kg(-1)), Cd (12.6 mg kg(-1)) and Pb (3154 mg kg(-1)). To immobilize the metals, mixtures of soil with phosphate (from H(3)PO(4) and hydroxyapatite (HA) with varying ratios) were prepared with a constant Pb : P molar ratio of 1: 10. The acetic acid extractable concentration of Pb in the mixture with the highest amount of added phosphoric acid (n(H(3)PO(4)) : n(HA) = 3 : 1) was reduced to 1.9% (0.62 mg L(-1)) of the extractable Pb concentration in the untreated soil, but the content of water extractable phosphorus in the samples increased from 0.04 mg L(-1) in the untreated soil sample up to 14.3 mg L(-1) in the same n(H(3)PO(4)) : n(HA) = 3 : 1 mixture. The high increase in arsenic mobility was also observed after phosphate addition. The PBET test showed phosphate induced reduction in Pb bioavailability. In attempting to stabilize Pb in the soil with the minimum treatment-induced leaching of phosphorus, it was found that a mixture of soil with phosphate addition in the molar ratio of H(3)PO(4) : HA of 0.75 : 1 showed the most promising results, with an acetic acid extractable Pb concentration of 1.35 mg L(-1) and a water extractable phosphorus concentration of 1.76 mg L(-1). The time-dependent leaching characteristics of metals and phosphorus for this mixture were evaluated by a column experiment, where irrigation of the soil mixture with the average annual amount of precipitation in Slovenia (1000 mm) was simulated. The phosphorus concentration in the leachates decreased from 2.60 mg L(-1) at the beginning of irrigation to 1.00 mg L(-1) at the end.     

硝酸体系微波消解-偏钼酸铵分光光度法测定固废中总磷方法的研究

固体废物经硝酸体系微波消解,其中难溶盐和含磷有机物分解形成正磷酸盐进入溶液,在酸性条件下,正磷酸盐与偏钒酸铵和钼酸铵反应,生成黄色的三元杂多酸,于波长420nm处进行比色测定.样品量为0.5g,定容体积50ml,使用3cm比色皿,方法检出限为1.1mg/kg,测定下限为4.4mg/kg,满足固废总磷的监测要求.     

Effect of application of phosphate and organic manure-based fertilizers on arsenic transformation in soil columns

The mobility of arsenic in Cambisol under the influence of added barnyard manure and application of a phosphate solution to the soil was described on the basis of column experiments. A soil sample containing 126 mg/kg total As and 3.72 mg/kg specifically-sorbed As was extracted using demineralized water (DIW) or a 28 μmol/l phosphate solution in a column containing untreated soil and in a column with added barnyard fertilizer. The pH, Eh, alkalinity, main components, including DOC, and selected trace elements (Al, Mn, Pb, Cu, Zn, Cd, Cr, Co, Ni, Ba and As) were determined in the extracts. Hydrodynamic tests of the flow and transport of the substances in the columns were carried out. The addition of barnyard manure was manifested in elevated concentrations of the main inorganic components, DOC and Al and a decrease in the Eh value and Mn concentration. Application of a phosphate solution was manifested in a decrease in the NO₃ and SO₄ concentrations, probably as a result of the effect of increased biological fixation. The As concentration in extracts varied from 8.8 to 15.5 μg/l and was not dependent on the composition of the extracting solution or the addition of barnyard fertilizer.     

水杨酸法检测水质氨氮的改进方法

该氨氮检测方法是对水杨酸分光光度法的改进,通过将50 g/L的水杨酸改为150 g/L的水杨酸钠,将有效氯为3. 5 g/L的次氯酸钠溶液改为5 g/L的二氯异氰尿酸钠溶液,增加了检测试剂的稳定性和贮存时间,同时将氨氮测定上限从1 mg/L提高至2. 5 mg/L,并将显色时间从60 min优化为30 min,使得此方法更为便捷。该方法的氨氮标准曲线线性关系良好,相关系数为0. 999 6,准确性和精密度高,加标回收率良好,适用于不同类型水质中氨氮的检测。     

ASE萃取-GPC净化-HPLC法测定土壤中阿特拉津

以二氯甲烷-丙酮（体积比1∶1）为混合溶剂，用加速溶剂萃取仪萃取土壤样品中的阿特拉津，提取液通过凝胶渗透色谱净化，用高效液相色谱仪在220 nm波长下测定，试验表明，在0．05 mg/L～5．00 mg/L范围内线性良好。方法检出限为0．22μg/kg，对空白土壤进行加标回收，平行测定6次，平均回收率为88．2％～102％，RSD为4．5％～7．6％，符合农药残留分析的要求。     

石墨炉原子吸收光谱法测定土壤中银

建立了土壤样品中痕量银的石墨炉原子吸收光谱测定方法,优化了试验条件,标准曲线线性关系良好,当取样质量为0.25 g,定容体积为25 mL时,方法检出限为0.01 mg/kg.经标准样品验证,方法准确度符合土壤样品分析要求.     

淮南潘北矿塌陷湿地土壤退化评价

采煤带来的地面塌陷是极为重要的新生环境地质问题。以淮南潘北矿塌陷湿地为研究区域,其总氮(TN)含量平均水平为1.04g/kg,总磷(TP)含量平均水平为425mg/kg,在空间分布上均有从非季节性积水区向季节性积水区递减的趋势。土壤理化性质指标间总氮与有机质(SOM)含量呈极显著正向相关,与pH呈负向相关,与有效磷(AP)呈正向相关;总磷与有效磷表现为极显著相关;AP与有效钾(AK)、SOM都有很好的相关关系。通过应用相关分析和模糊数学的原理,以TN、TP、AP、AK和SOM等5个土壤肥力指标为基础,对该区域季节性积水区和非积水区土壤肥力进行数值化综合评价。季节性积水区IFI为0.463,非积水区IFI为 0.601,表明塌陷湿地形成后会加剧水域周边土壤的退化。     

Spatial variability of soil total and DTPA-extractable cadmium caused by long-term application of phosphate fertilizers, crop rotation, and soil characteristics

Increasing cadmium (Cd) accumulation in agricultural soils is undesirable due to its hazardous influences on human health. Thus, having more information on spatial variability of Cd and factors effective to increase its content on the cultivated soils is very important. Phosphate fertilizers are main contamination source of cadmium (Cd) in cultivated soils. Also, crop rotation is a critical management practice which can alter soil Cd content. This study was conducted to evaluate the effects of long-term consumption of the phosphate fertilizers, crop rotations, and soil characteristics on spatial variability of two soil Cd species (i.e., total and diethylene triamine pentaacetic acid (DTPA) extractable) in agricultural soils. The study was conducted in wheat farms of Khuzestan Province, Iran. Long-term (27-year period (1980 to 2006)) data including the rate and the type of phosphate fertilizers application, the respective area, and the rotation type of different regions were used. Afterwards, soil Cd content (total or DTPA extractable) and its spatial variability in study area (400,000 ha) were determined by sampling from soils of 255 fields. The results showed that the consumption rate of di-ammonium phosphate fertilizer have been varied enormously in the period study. The application rate of phosphorus fertilizers was very high in some subregions with have extensive agricultural activities (more than 95 kg/ha). The average and maximum contents of total Cd in the study region were obtained as 1.47 and 2.19 mg/kg and DTPA-extractable Cd as 0.084 and 0.35 mg/kg, respectively. The spatial variability of Cd indicated that total and DTPA-extractable Cd contents were over 0.8 and 0.1 mg/kg in 95 and 25 % of samples, respectively. The spherical model enjoys the best fitting and lowest error rate to appraise the Cd content. Comparing the phosphate fertilizer consumption rate with spatial variability of the soil cadmium (both total and DTPA extractable) revealed the high correlation between the consumption rate of P fertilizers and soil Cd content. Rotation type was likely the main effective factor on variations of the soil DTPA-extractable Cd contents in some parts (eastern part of study region) and could explain some Cd variation. Total Cd concentrations had significant correlation with the total neutralizing value (p?<?0.01), available P (p?<?0.01), cation exchange capacity (p?<?0.05), and organic carbon (p?<?0.05) variables. The DTPA-extractable Cd had significant correlation with OC (p?<?0.01), pH, and clay content (p?<?0.05). Therefore, consumption rate of the phosphate fertilizers and crop rotation are important factors on solubility and hence spatial variability of Cd content in agricultural soils.