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。     

微波消解—ICP-MS法测定有机肥料中8种元素

采用电感耦合等离子体质谱法(ICP-MS)测定,来比较不同混合酸体系对有机肥料中As、Pb、Cd、Cr、Hg、Ni、Cu、Zn 8种元素的提取效果,建立了微波消解—ICP-MS测定有机肥料多元素含量的方法。研究结果表明,8种元素在0.10～1600 μg/L质量范围内线性关系良好,线性相关系数为0.99970～0.99995,检出限范围为0.003～0.400 μg/L。三水平加标回收率范围为81.8%～108.0%,相对标准偏差为0.9%～4.9%(n=6)。国家标准物质灌木枝叶GBW07603(GSV-2)除汞元素缺少相应的认定值以外,其余7种元素的测定值均在标准物质证书认定值的范围内,且相对标准偏差为0.5%～5.0%(n=6)。该方法灵敏度、准确度高,可实现有机肥料中多元素的通量检测。     

微波消解法快速测定土壤中有机质的含量

报道了用微波消解取代油浴消解或灼烧法来测定土壤中有机质的含量,详细讨论了微波消解法的有关测定条件.该法和传统的重铬酸钾油浴法相比,具有快速、经济、重复性好等优点,值得在相关行业中推广应用.     

土壤、沉积物和植物样品中多环芳烃（PAHs）不同提取与净化方法比较

系统分析和比较了土壤、沉积物和植物样品中多环芳烃（PAHs）的提取与净化方法,阐述和对比了索氏提取法、超声波提取法、超临界流提取法、固相提取与固相微提取法、固液提取法、微波辅助提取法、快速溶剂提取法等提取方法以及定量浓缩净化法、硅胶柱层析净化法、费罗里土柱层析净化法、氧化铝净化法、固相萃取（SPE）净化法等净化方法。旨在通过比较目前的提取和净化方法,展望将来提取与净化方法发展的新方向。     

农产品中重金属痕量分析样品制备的质量控制

根据农产品中重金属痕量分析的要求,探讨影响分析样品制备质量的一些因素。通过对3种试样制备方法优缺点的比较,指出各自的操作难点,并提出相应的质量控制措施,对实验室环境条件以及分析人员也提出相应要求。     

微波消解-ICAP法测定土壤中总铬含量的研究

采用微波消解仪对土壤样品进行前处理,用ICAP测定土壤中总铬含量。通过硝酸-氢氟酸以及硝酸-盐酸-过氧化氢体系消解液对土壤样品消解,优化试验选择出微波最佳消解条件和ICAP的工作参数。结果表明,发现用硝酸-氢氟酸体系消解液,在谱线283.56 nm、267.72 nm处用ICAP能够准确而稳定地测得土壤中总铬含量。     

微波消解-原子荧光法测定肥料中砷汞含量

建立了微波消解-原子荧光法同时测定肥料中砷和汞,进行消解条件、精密度、回收率等试验。方法显示,砷的检出限为0.014μg/L,汞的检出限为0.001 6μg/L,6次平行相对标准偏差<3%,3个水平的砷加标回收率90%~110%,汞加标回收率77%~83%。     

Comparison of Five Digestion Procedures for Recovery of Nutrients and Trace Elements in Plant Tissue

Comparison of five digestion procedures for recovery of nutrients and trace elements in plant tissue were examined. The objectives of this study were to compare five digestion procedures: AOAC (dry ashing), two nitric acid, (NA1, commonly used and NA2, our modification), and two aqua regia (AR1, commonly used and AR2, our modification) procedures for recovery of 15 plant nutrients and trace elements in corn, swiss chard, thorn apple, and barley flour (certified material). Generally, the recovery of various elements depended on the digestion procedure used and the plant species. In most instances, NA2 recovered more phosphorus (P), potassium (K), sulfur (S), and manganese (Mn) than the AOAC or the two AR procedures. Also, overall NA2 recovered more K and magnesium (Mg) than NA1. Extractants AR1 and AR2 recovered more iron (Fe) than the two NA procedures, and the same as the AOAC. The AR2 recovered very similar concentrations of nutrients as the AOAC; and in corn tissue, AR2 recovered more zinc (Zn), chromium (Cr), nickel (Ni), copper (Cu), and boron (B) than the AOAC. The AOAC recovered less S and B than the other procedures tested. For instance, in barley flour, AOAC recovered eight to nine times less S, while in corn tissue AOAC recovered around three times less S than the NA procedures. Overall, there are three important findings: (1) NA procedures may be used for recovery of most elements in plant tissue; (2) AR2 procedure is comparable to the official AOAC method for recovery of nutrients and trace elements in plant tissue, and (3) the official AOAC method used in Canadian plant testing laboratories may underestimate the concentration of S and B in plant tissue.     

Comparison of Open Digestion Methods for the Determination of Rare Earth Elements in Plant Samples by ICP-MS

An analytical procedure for the reliable determination of rare earth elements (REEs) in plant samples by inductively coupled plasma-mass spectrometry (ICP-MS) was developed. The influence of the main matrix elements was investigated first. It was established that moderate amounts (0.1–1.0%) of dissolved solids decreased the REEs signals significantly. Internal standardization with indium proved to be useful for obtaining correct results. Various digestion procedures were next applied to converting various solid plant samples to aqueous solution, namely dry-ashing, dry-ashing including a hydrofluoric acid (HF) step, and wet digestion using hydrogen peroxide (H₂O₂) and nitric acid (HNO₃). Obtained results showed that the simple dry-ashing procedure was sufficient for plants. A certified reference material (BCR-670, aquatic plant) was used to validate the accuracy of the method. Relative standard deviations varied from 1% (holmium, gadolinium) to 4% (europium). Detection limits between 13 (lanthanum) and 0.02 ng L^?1 (lutetium) were achieved.     

水稻和两种野生植物对酸性硫酸盐土耐性及矿质元素吸收

酸性硫酸盐土是发育于还原性硫化物成土母质的一种恶劣土壤类型,虽然其分布区气候条件十分有利于水稻生长,但由于土壤条件限制,水稻生产潜力难以发挥。为筛选出适应该土壤的水稻品种,在酸性硫酸盐土(pH 3.69)上种植了240个水稻品种,但是所有水稻品种均未获得经济产量,却发现两种野生植物在该土壤中生长茂盛。经形态和分子鉴定,两种野生植物为野荸荠(Eleocharis kuroguwai)和五棱飘拂草(Fimbristylis quinquangularis)。进一步分析了水稻和两种野生植物的根际和非根际土壤性质、根部和地上部矿质元素含量。结果表明,根际土壤pH、交换性铝和有效锰含量不能解释水稻和两种野生植物耐性差异,锰毒和缺氮亦不是酸性硫酸盐土限制植物生长的关键因子,而植物地上部矿质元素含量与植物耐性差异相关。铝毒、铁毒和较低的养分(磷、钾、钙、镁)吸收是酸性硫酸盐土中水稻生长不良的主要因子。相反,两种野生植物对铝毒和铁毒的耐性较强,对养分吸收能力较强,所以生长良好。     

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.     

Rapid,Wet Oxidation Procedure for the Estimation of Silicon in Plant Tissue

Abstract

The quantification of silicon (Si) in plant samples is being requested more frequently, especially in agricultural laboratories associated with the determination of nutritional requirements of sugarcane (Saccharum officinarum L.) and rice (Oryza sativa L.). The analysis of plant material for Si can be protracted, especially if laboratories do not have access to X‐ray flourescence (XRF) instrumentation and large numbers of samples are involved. A simplified procedure using equipment considered standard in most agricultural laboratories is reported. Dry, ground plant material is subjected to nitric acid/peroxide oxidation in a low‐pressure laboratory microwave digestion system. The hydrated silica liberated from the organic matrix is dissolved in a small volume of sodium hydroxide solution also using the microwave digestion system. Silicon is measured by inductively coupled plasma atomic emission spectrometry (ICP‐AES). This method gives results that are linearly correlated with the much slower conventional techniques and avoids using hazardous chemicals (hydrofluoric acid) sometimes employed in other microwave methods.     

水稻土和湿地土壤有机碳测定的CNS元素分析仪法与湿消化容量法之比较

土壤固碳研究中需要精确的(有机)C计量,而常规的湿氧化法与CNS元素分析仪法测定结果的吻合性足C计量中的问题.国外对旱地土壤的研究表明,这两种方法的结果基本可以对比,但是否同样对于湿地土壤也适用还不清楚.采用CNS元素分析仪(仪器法)和重铬酸钾外加热湿氧化法(容量法)对20个水稻土样品,26个淡水湿地土壤样品和20个沿海湿地土壤样品进行了总有机C(TOC)的对比测定.结果表明,无论是土壤的表土样品还是剖面样品,仪器法测定结果约低于容量法10%以下.两种方法对淡水湿地土壤和水稻土的有机C含量的测定可以对比,但是重铬酸钾氧化容量法对于含氯化物较高的沿海湿地土壤有机C的测定可能不精确.CNS元素分析仪测定的精密度和准确度较高,可以用于各种湿地土壤的C计量.     

转基因植物中CaMV35S和tNOS元件的4种定性PCR检测方法的比较

花椰菜花叶病毒35S启动子(promoter of Cauliflower mosaicvirus 35S,CaMV35S)和胭脂碱合成酶基因终止子(terminator of nopaline synthase gene,tNOS)是转基因产品筛选检测中的首选参数,日常检测中发现,个别标准中用于筛选检测这两种元件的引物存在非特异性扩增和灵敏度差的问题。本研究收集了国内外标准中常用的扩增片段分别为195、165、147和123 bp的CaMV35S和扩增片段分别为180、172、165和118 bp的tNOS各4对引物,应用普通PCR和实时荧光(Real-time)PCR方法,对8对引物的特异性、灵敏度及在加工品中的扩增性进行了测试和适用性评价。结果表明,CaMV35S 165和147 bp引物具有很好的特异性,灵敏度高,在不同的加工品中也表现出强的检测能力,筛选检测效果最佳;195bp引物扩增性稍差,且经常出现非特异性扩增;123bp引物较其他引物扩增弱且扩增不稳定。tNOS 172和165bp引物具有很好的特异性,灵敏度高,在不同的加工品中也表现出强的检测能力,筛选检测效果最佳;180bp引物扩增性较差,且易出现非特异扩增;118bp引物较其他引物扩增弱且扩增不稳定。本研究通过普通PCR和实时荧光(Real-time)PCR对不同国标中出现的引物进行适用性评价,为转基因产品的检测监管提供可靠技术依据。     

Microwave Digestion for Colorimetric Determination of Total Si in Plant and Mineral Samples

A new method for determining the soluble silicon (Si) concentrations in nonliquid plant and mineral samples was developed using sodium hydroxide (NaOH)–hydrogen peroxide (H₂O₂) matrix for microwave digestion (MWD-Na) followed by colorimetric Si testing. MWD-Na was compared with autoclave-induced digestion and alkali fusion. The data have shown no significant difference between these three methods. HNO₃–H₂O₂ or HNO₃?–H₂O₂?–HF microwave technique results in Si loss. The reduction of the total Si can be realized via low solubility of Si in the acid solutions or silicon tetrafluoride formation. The Mullen and Riley method for colorimetric testing of Si in a solution that uses ascorbic acid to reduce the silicomolybdate complex formed under acid conditions to an intensely blue complex was modified using iron sulfate. The combination of MWD-Na and modified colorimetric blue method provides cheap and valid data on determining the total Si in both plant and mineral samples.     

Soil and Atmospheric Inputs to PAH Concentrations in Salt Marsh Plants

Polycyclic aromatic hydrocarbons (PAHs) were measured in two wetland plant species grown outdoors in pots of sediment contaminated with up to 730,000 μg/kg total PAHs. After approximately 3 months, the plants were harvested, cleaned, and analyzed for an expanded suite of PAHs which included both the 16 priority PAHs and 22 alkyl PAH homologs. Sediment and air samples were also collected and analyzed. PAH compounds were detected in all of the samples, with the highest concentrations in the contaminated sediment. The root sample concentrations were generally about one order of magnitude lower than that of the sediment, and were strongly correlated with the concentration in the sediment in which they were grown. The concentrations in foliage were much lower and did not correlate with sediment concentration. Concentrations of low molecular weight PAH compounds detected in the foliage were not significantly lower in plants grown in control sediments, suggesting that the sediment is not the primary source of these PAHs. Several high molecular weight PAHs were detected only in plants grown in contaminated sediment. Plants of both species grown in control sediment were larger than plants grown in contaminated sediment.