分光光度法测定豆类中铝含量

用分光光度法测定了豆类中的铝含量。利用Al^3＋在乙酸-乙酸钠缓冲介质中，与铬天青S（CAS）及十六烷基三甲基溴化铵（CTMAB）反应形成蓝色三元络合物，在610nm处测定其吸光度，并对CTMAB质量浓度进行了最佳选择。结果表明，该法提高了测定灵敏度。10种豆类中的铝含量中绿豆的铝含量最高，29．49μg／g；菜豆的铝含量最少，8．24μg／g；10种豆类的平均铝含量为15．33μg／g。可见豆类中的铝含量很低，建议放心多食豆类食品。     

连续浸提-分光光度法测定硼泥中不同形态的硼

采用连续浸提法将硼泥中的硼划分为七种物理形态,即:水溶态、醇溶态、盐溶态、络合态、硫酸盐等结合态、Fe-Mn结合态及残渣态。用分光光度法测定各形态硼的含量。测定结果的相对标准偏差为4.4%(n=4),回收率为91.7%~102.4%。     

流动注射-分光光度法在线监测水中微量铝

建立了流动注射-分光光度法在线测定水中铝离子的方法,经过优化实验条件,方法的线性范围为0.01 ～0.6 mg/L,检出限为0.004 mg/L.本法试剂消耗量少,分析速度快,灵敏度高,抗干扰能力强,适宜于现场的即时检测,回收率在97.7％ ～101.7％之间.     

分光光度法测量铝镓氮外延片中的铝含量

采用熔融的氢氧化钠刻蚀在蓝宝石衬底上生长的铝镓氮外延层,用深紫外光致发光光谱仪测量铝镓氮的荧光光谱来控制铝镓氮层的刻蚀深度,用盐酸将含铝氢氧化钠中和并调节至酸性(pH1~2)后转移至250 mL的容量瓶内定容,用铬天青S络合显色,用分光光度计在546 nm处测定吸光度来确定铝的浓度。该法测量结果的相对标准偏差为1.1%(n=5),加铝标准溶液做回收试验,回收率为96%~103%。该法可用于铝镓氮外延片中铝含量的准确测量。     

双波长分光光度法同时测定灌木饲料中的铁和铝

利用铁、铝与邻苯二酚紫（PCV）形成的络合物的最大吸收波长相差30nm的光谱性质，建立了同时测定铁和铝的双波长分光光度法，并对络合物的形成条件及相互干扰情况进行研究，方法用于灌木饲料样品中铁和铝测定。     

环境中无机铬形态分析研究进展

本文对近年来环境分析化学中的一个重要分支－环境中无机铬的形态分析进展及有关分析方法的现况和发展趋势进行了概述。     

铬天青S胶束增溶分光光度法测定高纯氧化铋中微量铝

高纯氧化铋试样用硝酸溶解后,加入氢溴酸使铋生成易挥发的溴化铋除去,从而消除了铋对测定铝的干扰,在pH6.7的乙酸乙酸铵缓冲溶液中,在辛基酚聚氧乙烯醚存在条件下,铝与铬天青S生成稳定的三元配合物,其最大吸收波长为620nm,表观摩尔吸光系数为2.30×10⁵L/(mol·cm),铝在0～10μg/50mL范围内符合比耳定律,适用于高纯氧化铋中的微量铝的测定.     

化学浸提-分光光度法测定沙棘叶中不同形态铝

利用KCl、NH4Ac、HCl、NaOH四种浸提液将沙棘叶中的铝浸提溶出,得到沙棘叶中铝的不同化学形态,采用分光光度法定量测定,测定结果:沙棘叶中的Al3+为10.7%,Al(OH)2+和Al(OH)+2为2.1%,胶态Al(OH)03为34.3%,有机铝为53.0%.浸提液中铝的回收率为86.9%～101.0%.     

Speciation of Arsenic in Environmental and Biological Samples

A novel arsine generator glass assembly is constructed and reported for the spectrophotometric determination and speciation of arsenic in real samples. In an arsine generator, sodium borohydride is added dropwise to the acidic sample solution and arsine thus formed is reacted with silver diethyldithiocarbamate (Ag‐DDTC) ‐ Tritron‐X (TX‐100) solution in pyridine to form a red coloured complex. The complex showed the absorption maximum at λ_max 540 nm. The molar absorptivity of the method was found to be (1.55) × 10⁴ L mole^?1 cm^?1 at this wavelength. The presence of non‐ionic surfactant, i.e. TX‐100 in the Ag‐DDTC solution, makes the method ≈ 3 times more sensitive than the conventional Ag‐DDTC method. Beer's law is obeyed in the concentration range of 0.05–2.80 mg L^?1 of arsenic. The detection limit of the method was calculated to be 20 μg L^?1 As. Speciation of arsenite from other forms of arsenic in sample solutions was carried out by extraction of arsenite with Pb‐DDTC in chloroform, followed by spectrophotometric determination. After arsenite separation the sample is used for the arsenate determination. Total arsenic was determined by acid decomposition of the same sample. The speciation data were found to be comparable (±2%) with ICP‐MS, with better precision (< 1%). The method has been successfully applied for the speciation of arsenic in drinking water and dust samples of arsenic affecting the Rajnandgaon district of Chhattisgarh, India, and urine and blood samples of patients with arsenical diseases. Concentration of total arsenic in tube‐well water of this area was 3–6 times more than the permissible limit. Dust samples contained less amounts of arsenic than the ground water.     

生物和环境样品中硒元素的形态分析研究

金属组学是继基因组学/蛋白质组学和代谢组学后提出的一种新的组学,其研究重点在于对所研究的金属和类金属元素的各种存在形态进行分析。硒是生物环境中存在的一种重要的类金属元素。形态与浓度不同的硒化合物可能是生物体的必需元素,同时也可能导致中毒。本文对目前存在的硒元素形态分析方法的研究现状进行了总结,并对前景进行了展望。     

铝形态分析的研究进展

介绍了铝形态分析的意义,环境和生物体系中铝存在的形式,综述了铝形态分析时采用的连续静态浸提法、铝-试铁灵逐时络合比色光度法、酸碱电位滴定、电化学分析、色谱分析、核磁共振及计算机拟合等分析方法(1984—2009年间),引用文献65篇。     

土壤中锰的形态分析方法研究

采用Tessler的连续浸取程序，利用La-Zr涂履石墨管，石墨炉原子吸收光谱对土壤中不同形态锰的浸取与测定的条件进行了研究。经过对土样－3各形态的浸取液进行加标试验，其回收率在90%－110%，测定了一组土样，结果满意。     

Speciation Analysis of Chromium by Adsorptive Stripping Voltammetry in Tap and River Water Samples

An adsorptive stripping voltammetric method for speciation analysis of chromium in natural water samples has been developed. Ethylenediaminetetraacetic acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) were used as complexing agents for Cr(III) present in the sample and formed as products of Cr(VI) reduction, respectively. Under optimum experimental conditions linear relations in the range from 1×10^?6 to 3×10^?5 mol L^?1 without accumulation and from 1×10^?9 to 1×10^?7 at 30 s accumulation time were obtained for Cr(III) and Cr(VI), respectively. For samples in which Cr(III) concentration is higher than 1×10^?6 mol L^?1 the Cr(III) and Cr(VI) were determined simultaneously in one voltammetric cell. For samples in which Cr(III) concentration is below 1×10^?6 mol L^?1 only Cr(VI) was selectively determined in the presence of Cr(III), which did not influence the Cr(VI) signal. The determination of Cr(III) and Cr(VI) was successful with the application of the proposed procedure in the presence of common foreign ions. The presented method was applied for the speciation of chromium in spiked tap and river water samples with satisfactory results.     

Optimization of a Sample Preparation Procedure for the Speciation of Organotin Compounds in Sediment Samples Using GC-AED

Abstract

Results of a comprehensive study of all analytical steps involved in the sample preparation procedure for the speciation of butyl- and phenyltin compounds in sediments are presented. The proposed method is based on acid leaching (using aqueous acetic acid) and simultaneous extraction of the ionic species into an organic solvent (n-hexane/ethyl acetate) with the addition of a complexing agent (diethyl dithiocarbamic acid). After evaporation to dryness, the residue is derivatized with sodium tetraethylborate in an aqueous buffer solution (acetate buffer, 0.1 M, pH 5) and extracted into n-hexane. Cleanup is performed over basic alumina and the ethylated organotin species are analyzed with a gas chromatograph coupled to a microwave-induced helium plasma atomic emission detector (GC-AED). The optimized method was validated within an interlaboratory study for the certification of tributyltin, triphenyltin and their degradation products in a freshwater sediment, the BCR candidate reference material 646.     

纳米二氧化锆微柱分离电感耦合等离子-质谱分析水样中铬的形态

以纳米ZrO2为微柱填充材料,采用电感耦合等离子-质谱(ICP-MS)研究了Cr(Ⅵ)/Cr(Ⅲ)在纳米ZrO2微柱上的吸附性能。当pH值为8时,纳米ZrO2能完全吸附Cr(Ⅲ),而对Cr(Ⅵ)基本不吸附。对影响Cr(Ⅵ)和Cr(Ⅲ)分离的主要因素进行了详细研究,据此建立了纳米ZrO2微柱分离ICP-MS分析铬形态的新方法。方法对铬的检出限(3σ)为0.06ng/mL,定量测定下限(10σ)为0.37ng/mL,相对标准偏差为2.2%(n=9,c=100ng/mL)。本法选择性好、简便、快速,已用于不同水样中铬形态的测定,结果满意。     

Speciation and Determination of Trace Amount of Inorganic Arsenic in Water,Environmental and Biological Samples

A new speciation and preconcentration method based on dispersive liquid‐liquid microextraction has been developed for trace amounts of As(III) and As(V) in urine and water samples. At pH 4, As(III) is complexed with ammoniumpyrrolidine dithiocarbamate and extracted into 1‐Hexyl‐3‐methylimidazolium hexafluorophosphate, as an ionic liquid (IL) and As(III) is determined by electrothermal atomic absorption spectrometery (ETAAS). Arsenic(V) in the mixing solution containing As(III) and As(V) was reduced by using KI and ascorbic acid in HCl solution and then the procedure was applied to determination of total arsenic. Arsenic(V) was calculated as the difference between the total arsenic content and As(III) content. The effect of various parameters on the recovery of the arsenic ions has been studied. Under the optimum conditions, the enrichment factor 135 was obtained. The proposed method was successfully applied to the determination of trace amounts of As(III) and As(V) in water and biological samples.     

土壤样品中砷的形态分析方法研究

对生态地球化学土壤样品,在Tessier修正顺序提取方法(即七步法)的基础上对提取方法、提取时间、提取溶液的处理方法进行优化选择,用超声法提取水溶态、离子交换态、碳酸盐结合态、腐殖酸结合态、铁锰氧化物结合态、强有机质结合态和残渣态七种形态的砷元素,用原子荧光光谱法测定各个形态砷的含量。优化后的方法测得As元素各形态的检出限均小于1.0μg/g,相对标准偏差(RSD)小于10%,准确度高,质量参数均满足生态地球化学土壤样品评价形态分析的需要。     

微波消解-液相色谱-原子荧光光谱联用(LC-AFS)法测定稻米样品中砷形态

建立了稻米中4种砷元素形态的液相色谱-原子荧光光谱联用法(LC-AFS),样品用0.15mol/L的硝酸溶液微波提取50min,提取液经离心分离后,采用Hamilton PRP-X100色谱柱,45mmol/L KH2PO4-5mmol/L Na2HPO4缓冲液为流动相,砷形态4个组分能够在7min内达到基线分离,且无需调pH。优化了氢化物发生条件,使用了更低浓度的载流和还原剂。方法学实验结果表明,各组分在2~10ng/mL范围内线性关系良好,相关系数为0.9988~0.9998,各组分的检出限分别为0.29 ng/mL、0.47 ng/mL、0.62 ng/mL和1.16 ng/mL;各组分峰面积的相对标准偏差均低于3.11%;加标回收率为85.3%～112.8%;对稻米标准物质的分析测定结果表明该方法定值准确。最后,与GB 5009.11-2014中使用的提取及测量条件进行对比,表明该方具备法快速、环保、高效的特点。