双波长分光光度法同时测定岩石矿物中的微量金和钯

本文提出以硫代米蚩酮为显色剂，用双波长分光光度法同时测定岩石矿物中的微量金和钯的方法，消除了测定金钯的相互干扰，该方法简便，快速，选择性好，用于矿石样品中金和钯的测定，结果满意。     

5-Br-PADAB分光光度法测定钯

研究了４－（５－溴－２－吡啶偶氮）－１,３－二氨基苯（简称５－Ｂｒ－ＰＡＤＡＢ）分光光度法测定微量钯的反应,在乙酸介质中Ｐｄ（Ⅱ）与５－Ｂｒ－ＰＡＤＡＢ生成紫红色络合物,确定了分光光度法测定钯的新体系。在实验条件下试剂的最大吸收峰位于４３８ｎｍ处,络合物的最大吸收峰位于５６４ｎｍ处,表观摩尔吸光系数ε＝５．２０×１０－４Ｌ／ｍｏｌ．ｃｍ,用等摩尔连续变化法、摩尔比法测得络合比ｎ（Ｐｄ（Ⅱ））∶ｎ（５－Ｂｒ－ＰＡＤＡＢ）＝１∶１,钯离子的量浓度在４．２７×１０－８～１．５４×１０－５ｍｏｌ／Ｌ时,服从Ｂｅｅｒ定律。试验了３０种离子在一定量下不干扰测定。     

人工神经网络紫外分光光度法同时测定去痛片组分含量

用BP人神经网络处理复方制剂去痛片的紫外吸收光谱数据,达到了对其各组分含量进行同时测定的目的。通过对网络结构和参数的优化,提高了预报的准确度。     

人工神经网络-分光光度法同时测定合金钢样中的铈组各个稀土元素

以二溴对甲基偶氮璜（DBM－SA）为显色剂,应用化学计量学中人工神经网络原理,结合分光光度法,对吸收光谱严重重叠的铈组五个元素不经分离可直接进行同时测定。对合金钢试样中铈组五个元素的个别含量及铈组总量的测定,结果令人满意。并进一步讨论了人工神经网络的结构及参数对分析结果的影响。     

2,6-二甲酚分光光度法测定废水中的总氮

废水中的无机态氮和有机态氮被过硫酸钾氧化消解后转变为硝酸盐，在硫酸和磷酸混合酸介质中，硝酸盐与2，6—二甲酚反应生成4—硝基—2，6—二甲酚而显色。废水中的总氮在2～8mg/L范围内与337nm波长处的吸光度成正比，回归方程为A=0．1672X—0．0077，相关系数r=0．9996，回收率为96．5％～105．7％。氯离子浓度高于1．5g/L时有干扰，其它常见的阴、阳离子无干扰。     

人工神经网络算法分光光度法同时测定锰和镍

采用甲醛肟-锰、镍显色体系,应用人工神经网络分光光度法,对吸收光谱严重重叠的两组分锰、镍同时进行测定。应用于工业废水中锰（Ⅱ）和镍（Ⅱ）的同时测定,回收率在95％～102％之间。     

石蜡相分光光度法测定微量钯

以石蜡为固体萃取剂，系统地探讨了钯－丁二酮肟（ＤＭＧ） 显色体系在石蜡相最佳显色条件及光度特性。钯的浓度在０～８０ ｍ ｇ／５０ Ｌ范围内符合比尔定律，相关系数ｒ＝ ０．９９９７。方法检出限为１．７５×１０－ ５ｇ／Ｌ。该法选择性好，大多数常见离子不干扰钯的测定，灵敏度比液相光度法高。应用于分子筛中微量钯的测定，结果良好。     

双波长分光光度法同时测定贵金属钯和锇

本文提出了在对羟基苯基荧光酮和溴化十六烷基三甲烷基甲胺存在下，双波长分光光度法同时测定微量和锇的新方法，在ｐＨ＝７．６～８．０的磷酸盐介质中，钯和锇的对羟基苯基荧光酮－ＣＴＭＡＢ配合物吸收光谱相互重叠，选择测定钯配合物的波长对为５８０．５ｎｍ与５３０．５ｎｍ，测定锇配合物的波长对为５５３．５ｎｍ与６０４．５ｎｍ，钯含量在０～７．０μｇ／１０ｍＬ范围内，锇含量在０～９．０μｇ／ｍＬ范围内，与ΔＡ值呈     

人工神经网络-紫外分光光度法同时测定苯酚、苯胺和苯甲酸

采用人工神经网络方法和紫外分光光度法相结合研究多组分的同时测定,系统地研究了神经网络方法对苯酚、苯甲酸和苯胺混合样品同时测定的可行性.在大量实验数据的基础上采用matlab语言编写两层BP神经网络,并初步探讨了网络参数对网络预测性能的影响.结果表明,BP神经网络能在不改变样品性质的前提下实现了多组分的同时测定,最大限度地保护了样品不被破坏.方法的回收率为96.9%～109.3%,RSD为0.90%～1.28%(n=5).通过时不同隐层神经元数目的研究发现,当隐层神经元数目达到100时,仿真结果和实验数据相似程度达到了90%以上,且随隐层神经元数目增多,训练误差下降速度加快,但训练速度变慢,训练时间延长.     

分光光度法测定痕量钯

在 pH为 7.5 0的条件下 ,Pd2 +与甲基紫、溴化钾反应形成紫色缔合物 ,吸收峰位于 5 80nm ,Pd2 +浓度在 10 0～ 80 0 μg/L范围内与吸光度成正比 ,表观摩尔吸光系数ε580 =2 .4× 10 5L/ (mol·cm) .方法操作简便 ,灵敏度高 ,用于试样中痕量Pd2 +的测定 ,结果令人满意 .     

紫外差示分光光度法同时测定含苯系物废水中苯胺和苯酚

苯胺、苯酚在不同酸度的水溶液中具有不同的结构和紫外吸收光谱。以苯胺水溶液为测定液,以等浓度的苯胺酸溶液为参比液;以苯酚碱溶液为测定液,以等浓度的苯酚水溶液为参比液,分别测定其吸光度。结果表明:在280 nm处,当苯胺质量浓度为1~100 mg/L时;在287 nm处,当苯酚质量浓度为1~30 mg/L时,苯胺、苯酚的吸光度与浓度之间存在良好的线性关系,据此建立了紫外差示分光光度法。用此法不需分离直接测定了含苯系物废水中的苯胺和苯酚,回收率分别大于94.6%和96.7%。     

Simultaneous neutron activation determination of palladium,gold, platinum and iridium in some natural materials

A method for rapid simultaneous neutron activation determination of Pd, Au, Pt and Ir in USGS standard rocks, ores and minerals has been developed based on selective extraction of determined elements. Results of determination of noble metals in standard rocks are discussed.     

Simultaneous determination of mercury and gold in bismuth by neutron activation analysis

After adding mercury as carrier, trace amounts of mercury and gold were simultaneously separated from bismuth by coprecipitating with sulfur produced by the decomposition of bismuth sulfide. The sulfur was filtered on a membrane filter, and the γ-activities were measured with a Ge(Li) detector. The recoveries were quantitative and the measurement of chemical yield was unnecessary. 123 ppm of mercury and 8 ppb of gold in a bismuth sample were determined simultaneously.     

高效液相色谱-串联质谱法同时测定废水中18种酚类污染物

建立了上清液直接进样-高效液相色谱-串联质谱同时测定废水中18种酚类污染物的分析方法。取5.0 mL水样置于具塞离心管中,加氨水调节pH≥12,摇匀,加入1.0 mL二氯甲烷-正己烷(2: 1, v/v)混合溶液并振摇5 min, 4000 r/min离心5 min,用玻璃针筒抽取上清液并经0.22 μ m聚四氟乙烯滤膜过滤,用甲酸调节水样pH至中性;然后采用Thermo Hypersil ODS柱(100 mm×2.1 mm, 5.0 μ m)分离,以甲醇-0.01 mol/L甲酸铵-甲酸水溶液(pH 4.0)为流动相进行梯度洗脱,流速0.2 mL/min,柱温30℃,进样10 μ L,电喷雾负离子电离(ESI^-)模式、多反应监测(MRM)模式进行检测,外标法定量。18种酚类化合物的峰面积与其质量浓度在一定浓度范围内均呈良好的线性关系(r²≥0.9991),方法检出限为0.10~0.88 μ g/L。测定低、中、高加标浓度的样品,18种酚类化合物的相对标准偏差为2.5%~9.9%(n=6);火工药剂废水与石油化工废水样品中的平均加标回收率为68.7%~118%(n=3)。此方法操作简单,灵敏度高,干扰小,分析速度快,可适用于环境废水中18种酚类污染物的同时分析。     

Simultaneous determination of Cs and Sr in the high level waste by ion-chromatography

A method based on ion-chromatography has been developed for determination of Cs and Sr in high level waste (HLW) without matrix separation. The acidity of HLW (3 M HNO₃) was decreased to 0.01 M by addition of NaOH. Chromatographic separation of Cs⁺ and Sr⁺⁺ in presence of bulk Na⁺ has achieved using methane sulphonic acid as mobile phase in isocratic and gradient mode. The calibration plot was linear for the concentration range of 0.5–12 mg/L for Cs and 0.025–6 mg/L for Sr with regression coefficients close to 1. RSD obtained for Cs and Sr was 1 and 5 % respectively. Detection limit calculated as 3(S/N) was found to be 20 μg/L for Cs and 30 μg/L for Sr. The standard addition procedure was used to validate the developed method. The samples received from PREFRE, Tarapur and WIP, BARC were analyzed by the new method and the results are presented.     

Solid-phase extraction in the determination of gold, palladium, and platinum

A simple classification of various sorbents and solid-phase extraction procedures used for preconcentration of trace levels of Au, Pd, and Pt from different sample types is proposed in this review article. The large variety of available sorbents/procedures has been organized according to expected mechanisms of sorption process (complex formation; ion exchange; adsorption; ion-imprinted or molecularly imprinted polymers); according to the kind of monomeric units of the polymer matrix as well as on the basis of the kind of functional group responsible for main performance characteristics (selectivity, capacity) of the sorbent. Advantages of chemically modified sorbents, sulfur-containing sorbent extractants, and ion-imprinted polymers, together with rational pretreatment by means of microwave treatments, scaling down of enrichment, and quantification by means of flow and flow injection approaches are given. Preferred instrumental techniques for quantification of ppb levels of Au, Pd, and Pt in prepared concentrates/column eluates are multielement instrumental techniques: inductively coupled plasma optical emission spectrometry (ICP-OES), and inductively coupled plasma mass spectrometry (ICPMS). Excellent limits of detection at picogram levels of these analytes are provided by electrothermal atomic absorption spectrometry (ETAAS), generally in single-element mode and the neutron activation analysis (NAA), while X-ray fluorescence spectrometry and flame AAS are rarely applied because of lack of sensitivity at sub-ppm levels of Au, Pd, and Pt. Some problems of atomic spectrometric quantification techniques and their representative limits of detection are given. Recent applications to geological, industrial, pharmaceutical, biological, and other materials are tabulated. References have been selected mostly from the period 1995 to 2010.     

Simultaneous determination of pentachlorophenol and carbaryl in water

Summary A rapid method for the simultaneous determination of pentachlorophenol (PCP) and Carbaryl in water is described. A 1 liter water sample is extracted with hexane after acidification with concentrated H₂SO₄. After evaporation to a small volume, the extract is analyzed by gas chromatography-mass spectrometry, operating in the selected ion monitoring mode. Estimated detection limits are 0.08 g L^–1 for PCP and 0.11 g L^–1 for Carbaryl, with recoveries of 96% for PCP and 97% for Carbaryl.