土壤总砷测定前处理方法探讨

采用加标回收方法比较研究了5种土壤总砷测定的前处理方法(分别为浓HNO3-浓H2SO4-HC1O4法、王水法、浓HNO3-浓H2SO4-V2O5法、浓HNO3-浓H2SO4-V2O5Ⅰ法和浓HNO3-浓H2SO4-V2O5Ⅱ法),结果表明,5种前处理方法的加标回收率在89.9%～102%之间,变异系数在0.56%～5.27%之间。其中,浓HNO3-浓H2SO4-V2O5Ⅰ法处理,土壤所用消解时间40min左右,其回收率较高,在98.5%～99.1%之间,变异系数较小,在0.56%～0.85%之间;该前处理方法具有消解时间最短、加标回收率和精密度高及重现性最好的特点,优于其他4种前处理方法,可作为推荐方法应用。     

一种土壤中缓效钾测定的改进方法

土壤缓效钾是土壤有效钾的一部分,通过对NY/T 889-2004《土壤速效钾和缓效钾含量的测定》测定缓效钾含量的前处理方法进行改进,用标准COD消解器消解替代了油浴（或磷酸浴）,改进后的方法在精密度方面平行测定最大相对相差均≤8%,在准确度方面标准物质测定的单次结果均在标准值范围之内。实际样品测定方面,改进前和改进后的方法相对相差均≤8%。改进后的方法有较好的精密度和正确度,操作更加安全,消解效率高。     

微波消解法测土壤中全磷和全钾

用微波消解法测定土壤标准样品、标准方法测定消解液P和K含量,通过实验确定最佳消解及分析条件;而且比较微波消解法和传统电热板消解法的精密度和准确度,建立微波消解技术测定土壤P和K前处理方法.结果表明:土壤样品用1∶1HNO3∶HF 10ml的混酸体系进行消解,效果最佳;对于土壤标样,微波消解法测定P和K的相对标准偏差分别为1.46%～3.20%和0.38%～0.84%,电热板消解法测定P和K的相对标准偏差分别为3.06%～4.15%和0.40%～2.08%,微波消解法的测出值均高于电热板消解法;微波消解法的准确度和重现性明显优于电热板消解法,与标准值的相对相差比较,微波消解法都低于5%;两种试验方法样品回收率测得为94%～105%,符合分析方法要求.方法快速简便并有较高准确度、精密度,值得推广和应用.     

利用电感耦合等离子体质谱法测定肥料重金属砷、镉、铅、铬含量

选取7个不同的肥料样品,采用硝酸-盐酸（王水）消解,消解液中砷（As）、镉（Cd）、铅（Pb）、铬（Cr）重金属元素含量采用电感耦合等离子体质谱（ICP-MS）法氦碰撞模式测定。结果显示,根据固体称重量为0.2 g,定容体积50 mL,Cr、As、Cd、Pb方法检出限分别为0.018、0.008、0.005、0.021 mg/kg,定量限分别为0.061、0.025、0.016、0.069 mg/kg,根据液体称重量1.0 g,定容体积50 mL,Cr、As、Cd、Pb方法检出限分别为0.004、0.002、0.001、0.004 mg/kg,定量限分别为0.012、0.005、0.003、0.014 mg/kg,待测样品分别进行6组重复测定,结果显示Cr相对标准偏差（RSD）在3.8%～16.8%之间,As的RSD为3.9%～56.5%,Cd的RSD为0.0%～25.7%,Pb的RSD为4.2%～24.5%,样品加标回收率为67.4%～122.0%。4家实验室对不同肥料种类抽取样品进行实验室比对测定,分析显示所有参与实验室测试值之间存在一致性,经柯克伦检验剔除离群值,保留歧离值后,将...     

小麦籽粒中微量铅的快速测定技术(简报)

为建立一种快速测定粮食中微量铅的新方法,以南阳彩色小麦为材料,用微波压力消解技术快速处理样品,对测定条件进行优化,并与国家颁布标准方法(GB/T5009.12-2003)进行比较。结果表明:加标回收率为92.5%～96.8%,相对标准偏差RSD(Relative Standard Deviation)为0.67%～1.7%(n=11),铅的最低检出限为0.0099mg/L,测定的线性范围为0.850～206.0mg/L,相关系数为0.996,电极斜率为24.160。样品用该法与国标方法对照测定并进行显著性检验证明,该方法具有直观、快速、简便、灵敏、准确、适于现场进行测定的显著优点。     

微波消解法测定饲料中的总砷分析

针对国家标准GB/T 13079-2006干灰化、盐酸溶样-原子荧光光谱法测定饲料中总砷时出现回收率偏低、重现性偏差、仪器易污染的缺陷,通过试验和分析,提出了样品前处理优化改进方法;通过测定和银盐法(仲裁法)的对比和加标回收试验,对改良的方法进行验证。从试验结果可得到:本方法检出限为0.01 mg/kg,加标回收率为87.3%~96.4%。微波消解-原子荧光光谱法测定饲料中总砷方法,灵敏度高、检出限低、操作简便、环境污染小,可以满足大批量、多品种日常监测。     

原子吸收法直接测定土壤中的铅

用HNO3-HF -HClO4 消解土壤样品 ,直接用原子吸收分光光度计测定其中的铅 .实验结果表明 ,此方法有较好的准确度 ,精密度和回收率 .测定标准土样 ,结果与推荐值相吻合     

微波消解塞曼火焰原子吸收法测定土壤中重金属元素的方法研究

利用光纤压力自控密闭微波消解系统和采用正交实验等方法,优选了微波消解土壤的酸用量、微波时间及压力强度等项指标。实验结果表明,在供试条件下,以HNO33ml、HClO42ml、HF3ml混合酸作消解液,采用0.5MPa3min、1 5MPa5min二段微波消解方式,可获得满意的检测结果,其准确度和精密度均符合土壤环境样品分析要求,具有操作简便、快速、经济的特点,并可在同一消解液中分别测定土壤Cu、Zn、Pb、Cd、Cr、Ni等重金属元素,是测定土壤重金属元素含量的有效方法。     

不同前处理方法对秸秆金属元素原子吸收光谱分析结果的影响

秸秆中金属元素是关系农作物秸秆科学利用的重要组成部分,目前还没有统一的秸秆中金属元素原子吸收光谱(atomic absorption spectroscopy,AAS)测定方法标准,该研究采用原子吸收光谱测定黄芪(GBW10028)标准物质、玉米秸秆、小麦秸秆和棉花秸秆中金属元素含量,比较了不同前处理方法对样品中K、Cu、Fe、Zn和Mg分析结果的影响。结果表明:微波消解、干法灰化和湿法消解测定黄芪(GBW10028)标准物质中金属元素含量差异性显著(P<0.05),微波消解比干法灰化、湿法消解准确度高。微波消解对玉米秸秆、小麦秸秆和棉花秸秆中各金属元素的影响与黄芪(GBW10028)标准物质趋于一致。微波HNO3与微波HNO3-H2O2测定结果差异性不显著(P>0.05),微波HNO3比微波HNO3-H2O2和微波HNO3-H2SO4测定结果稳定。微波HNO3是进行秸秆样品金属元素含量测定时较准确简便的前处理方法。     

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。     

土壤消解方法研究及对上海浦东环境汞背景值初步调查

利用欧洲标准样作控制,对比研究了土壤总Hg测定的3种消解方法,并对浦东垃圾焚烧发电厂周围土壤总Hg的背景值进行了初步研究,结果发现浦东土壤Hg背景值达到192.68 ng/g,明显高于其它城市,这与上海的工业历史、农业施肥习惯有关,值得注意的是浦东地区土壤中的气态Hg(一个样品除外)含量都很高。     

菜园土壤有效钾提取方法比较研究——以重庆地区为例

研究菜园土壤有效钾的测定方法,为蔬菜合理施用钾肥提供理论依据。以36个莴笋钾肥田间试验的产量及吸钾量为参比标准,采用7种方法 (醋酸铵法、ASI法、Mehlich3法、冷硝酸法、四苯硼钠法1、四苯硼钠法2和沸硝酸法)测定土壤有效钾含量。结果表明,土壤有效钾含量以沸硝酸法四苯硼钠法2四苯硼钠法1冷硝酸法Mehlich3法醋酸铵法ASI法。7种测定方法测得的土壤有效钾含量间呈不同程度正相关,均具有评价土壤钾素有效性的潜力。四苯硼钠法1和四苯硼钠法2测得的土壤有效钾含量与无肥区占施钾区莴笋相对产量(RY_(CK))、缺钾区占施钾区莴笋相对产量(RY_(NP))、无肥区占施钾区莴笋相对吸钾量(RUK_(CK))的相关性均达显著水平,即其测得的土壤钾素的生物有效性均较好。综合而言,在所试验土壤地区,四苯硼钠法1和四苯硼钠法2均是评价菜园土壤当季钾素有效性的较好方法,其中以四苯硼钠法1更好。     

配位体交换在减慢由酸雨造成的可变电荷土壤酸化速度中的意义

For the purpose of evaluating the role of ligand exchange of sulfate ions in retarding the rate of acidification of variable charge soils,the changes in pH after the addition of different amounts of HNO3 or H2SO4 to representative soils of China were measured .A difference between pH changes caused by the two kinds of acids was observed only for variable charge soils and kaolinite,but not for constant charge soils and bentonite,The larger the proportion of H2SO4 in the HNO3-H2SO4 mixture,the lower the calculated H^ ion activities remained in the suspension.The difference in H^ ion activities between H2SO4 systems and HNO3 systems was larger for soils with a low base-saturation(BS) percentage than those with a high BS percentage.The removal of free iron oxides from the soil led to a decrease in the difference,while the coating of Fe2O3 on a bentonite resulted in a remarkable appearance of the difference.The effect of ligand exchange on the acidity status of the soil varied with the soil type.Surface soils with a high organic matter content showed a less pronounced effect of ligand exchange than subsoils did.It was estimated that when acid rain chiefly containing H2SO4 was deposited on variable charge soils the acidification rate might be slower by 20%-40% than that when the acid rain chiefly contained HNO3 for soils with a high organic matter content,and that the rate might be half of that caused by HNO3 for soils with a low organic matter content,especially for latosols.     

Determination of selenium in nuts by cathodic stripping potentiometry (CSP)

The aim of this work was to determine the selenium content in nut samples by cathodic stripping potentiometry. Dry-powdered nuts were digested by HNO(3) and dissolved with concentrated hydrochloric acid. To avoid the interference of natural oxygen, the potentiometric determination of selenium was carried out in an electrolyte solution consisting of 2 M CaCl(2) and 4 M HCl. The analysis was executed applying an electrolysis potential of -150 mV for 60 s and a constant current of -30 microA. Under these conditions, detection limits lower than 1.0 ng g(-)(1) were obtained for selenium analysis in nuts. The relative standard deviation of these measurements (expressed as rsd %) ranged from 0.44 to 0.88% while recoveries ranged from 90.2 to 95.3%. The results obtained with the proposed method were compared with those obtained via hydride vapor generation atomic absorption spectroscopy, a common method for determining selenium. The results of the two methods agreed within 5% for almond, hazelnut, and pistachio samples. The mean concentrations of selenium determined in Sicilian samples of almond, hazelnut, and pistachio were 531 +/- 1, 865 +/- 1, and 893 +/- 4 microg/kg, respectively.     

免耕轮作对旱作区土壤水热动态及速效养分含量的影响

免耕轮作对土壤性质有明显改善作用。在免耕秸秆覆盖基础上进行燕麦、玉米、大豆3种作物轮作2个周期的试验研究。结果表明,免耕秸秆覆盖结合不同作物轮作能调节土壤水热环境,增加土壤速效养分含量。土壤贮水量在不同处理间总体表现为免耕留高茬覆盖(NHS)免耕留低茬覆盖(NLS)免耕留高茬(NH)免耕留低茬(NL)常规翻耕(T),3种轮作方式中均以燕麦-大豆-玉米方式最高。轮作2个周期后NHS、NLS、NH、NL分别较T土壤贮水量在作物苗期增加了16.24%、12.16%、8.75%、5.56%,可见免耕覆盖能明显提高土壤水分蓄储能力。土壤温度在0~5 cm土层受外界环境影响最大;免耕覆盖在低温时起"保温作用",能提高土壤温度1.4~2.4℃;高温时起"降温作用",能降低土壤温度1.8~3.4℃;秸秆覆盖后土壤温度日变化平缓。同时免耕结合轮作处理能不同程度增加土壤有机质及速效养分含量,说明免耕轮作在该地区能较大程度的改善土壤性质,为提高作物产量提供了基础和有效保证。     

不同培肥措施对土壤物理性状及无机氮的影响

通过田间动态监测,在东北中部黑土区比较了不同培肥措施下0~60 cm土壤三相比、容重、含水量及无机氮的变化。结果表明,黑土的土壤容重在深松后随着玉米生育进程逐渐向初始状态(1.36~1.54 g cm-3)恢复;与常规栽培(T1)相比,深松+深追肥(T3)和深松+深追肥+增施有机肥(T4)可有效降低玉米成熟期时的土壤容重,改善土壤结构,使20~40 cm层次的土壤三相比接近理想值,T4处理下在成熟期(R6)20~30 cm和30~40 cm土层土壤三相比分别为53.4∶25.2∶21.4和50.9∶25.1∶24.0;此外,T4处理下20~40 cm土壤容重至成熟期时仍保持在1.16~1.29 g cm-3。深松促进了硝态氮的下移,优化了土壤中氮的分配;在开花后,T4处理下20~40 cm土层中硝态氮含量占总含量的31.1%~37.5%,有效的满足了生育后期根系对养分的需求;T4处理下20~50 cm土壤含水量显著提高,较T1处理下平均提高18.0%。研究表明,深松+深追肥+增施有机肥可以改善土壤物理环境,尤其是在20~40 cm,并能显著提升土壤水养库容能力,从而促进养分吸收,提高玉米产量。     

Optimized gel permeation chromatographic cleanup for soil, sediment, wastes, and oily waste extracts for determination of semivolatile organic pollutants and PCBs

A gel permeation chromatographic (GPC) method, used by the U.S. Environmental Protection Agency (USEPA), was modified for cleanup of soil, sediments, wastes, and oily wastes before determination of semivolatile organic pollutants. The modifications included new calibration procedures and control of the amount of material processed. The modifications were evaluated for soil and sediment matrixes in a 5-laboratory study where each laboratory processed a solution containing a phthalate, substituted phenols and benzenes, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), nitroaniline, and pesticides. With the exception of nitroaniline, analyte recoveries were 87-112%, with relative standard deviations (RSDs) of 6.7-26%. Soil samples containing PCBs and fortified with 6 pesticides at 0.7-4 micrograms/g were also analyzed by the 5 laboratories. The mean recovery of the 6 pesticides was 100% with a mean RSD of 16%. Mean RSD for the determination of total PCBs was 8.9%. An additional modification for the processing of wastes and high concentration waste samples was attempted; this involved GPC processing of sample extracts dissolved in 1 + 1 butyl chloride-methylene chloride. This modification did not improve recoveries of the semivolatile analytes. Finally, the modified GPC protocol was applied to PCB-contaminated reclaimed waste oils samples. Two GPC cleanup steps were used to separate PCBs from the waste oil samples before PCBs were determined by gas chromatography combined with electron-capture detection (GC/ECD).     

伊朗西部地区哈马丹市农业土壤钾地位的多元统计分析

Multivariate statistical technique was used to determine the potassium (K⁺) status and to assess soil fertility and K leaching potential in some calcareous soils. Water-soluble K⁺ (H₂O-K) and ammonium acetate-extractable K⁺ (NH₄OAc-K) ranged from 0.019 to 0.590 (mean value 0.095) and 0.390 to 3.320 (mean value 0.954) cmolc kg^-1, respectively. The nitric acid-extractable K⁺ (HNO₃-K) varied from 1.03 to 13.63 (mean value 5.37) cmol_c kg^-1. The proportion of H₂O-K ranged from 0.34% to 14.8% of HNO₃-K, and 2.2% to 53.2% of NH₄OAc-K. The proportion of NH₄OAc-K ranged from 5.8% to 80% of HNO₃-K (mean value 23% of HNO₃-K). The tendency of the soil to lose K⁺ by leaching was examined by determining K⁺-Ca²⁺ exchange isotherms. The soils mostly had moderate to high values of K⁺ sorption capacity, ranging from 10% to 58% (mean value 28%) of added K⁺. The Gapon coefficient varied widely from 1.1 to 12.0 (L mol^-1)^-1/2. Clay minerals were dominated by illite, smectites and vermiculite with small amounts of kaolinite. Principal component analysis (PCA) showed that the first four components accounted for 27.7%, 21.4%, 13.8%, and 8.9% of total variation, respectively. The non-hierarchical cluster analysis (k-means clustering) grouped 75 sampling sites into six clusters, based on the similarity of soil quality characteristics. The results suggested that such classes could form a basis for variable-rate application to maintain an adequate K⁺ status for crop production and to reduce potential K⁺ loss from soil by leaching.     

Speciation of aluminum in drink samples by 8-hydroxyquinoline loaded silylanization silica gel microcolumn separation with off-line ICP-MS detection

A technique using a flow injection microcolumn separation coupled with ICP-MS detection has been developed for the speciation of Al in drink samples. The retention behaviors of different Al species were studied with 8-hydroxyquinoline (8-HQ) loaded silylanization silica gel as the packing material and inorganic acid (HNO3) as the elution. The results indicated that in a pH range of 5.0 to 8.0, all labile monomeric Al species were retained on the microcolumn while nonlabile monomeric Al species were directly passed through the column. Various Al species after separation were detected by ICP-MS. The detection limit of 0.2 ng mL(-1) and a relative standard deviation (RSD) of 4.2% at 10 ng mL(-1) (n = 11) were achieved, and the recoveries for the spiked samples were 95-108%. The proposed method has been applied to the analysis of Al species in tea infusions, coffee, and tap waters with satisfactory results. The results obtained by this method were compared with that obtained by the cation exchange microcolumn separation and ICP-MS detection system, and some valuable conclusions were drawn.