可溶性滤膜分离富集-电感耦合等离子体原子发射光谱法对水中痕量镉、铜、铅与锌的同时测定

基于金属离子与2-[5-溴-2-吡啶偶氮]-5-二乙氨基酚(5-Br-PADAP)形成的螯合物能被混合纤维素滤膜捕集,建立了可溶性滤膜分离富集ICP-AES法同时测定水中痕量镉(Ⅱ)、铜(Ⅱ)、铅(Ⅱ)和锌(Ⅱ)的新方法.研究了六通道多联装置同时进行过滤富集的可行性,考察了溶液介质酸度、螯合剂用量、共存离子等对分离富集的影响.在优化的实验条件下,100 mL水样中镉、铜、铅和锌的富集倍率分别为18、19、17和19,检出限(3σ,n=11)分别为0.04、0.15、0.44、0.06 μg/L.方法成功用于自来水和市售矿泉水样中镉、铜、铅和锌的测定,加标回收率为86% ～119%.     

浊点萃取-火焰原子吸收光谱法测定菠菜中镁、锌和铜

在pH 8.0缓冲溶液中,以8-羟基喹啉为螯合剂,镁、锌和铜均与8-羟基喹啉生成螯合物,加入Triton X-100表面活性剂用浊点萃取分离富集菠菜样品中镁、锌和铜。分取部分表面活性剂相用乙醇定容至25mL,所得溶液直接用火焰原子吸收光谱法进行测定。对影响浊点萃取的因素和共存离子的干扰等进行了试验并予以优化。镁、锌和铜的检出限(3s/k)依次为0.057,0.064,0.032mg.L-1。应用此法测定了大叶菠菜和小叶菠菜中3种元素的含量,在两种样品中用标准加入法进行方法的回收试验,测得镁的回收率在93.3%～100.5%之间;锌的回收率在91.7%～97.9%之间;铜的回收率在94.0%～107.1%之间。     

微柱高效液相色谱法测定环境样品中的铁、钴、镍、铜、锌、锰

研究了用 2-(2-喹啉偶氮 )-间苯二酚 (QAR)为柱前衍生试剂 ,以WatersXterraTM RP18(1 .0×5 0mm ,2. 5 μm)微柱为固定相 ,60 %的甲醇 (内含 0 . 5 %的醋酸 )为流动相 ,高效液相色谱分离、二极管矩阵检测器测定铁、钴、镍、铜、锌和锰的方法。根据信噪比 (S N =3 )得各金属离子的检测限分别为 :铁3 μg L、钴 4μg L、镍 2 μg L、铜 4μg L、锌 5 μg L、锰 8μg L ,方法用于环境样品中痕量铁、钴、镍、铜、锌、锰的测定 ,相对标准偏差在 1 . 6%～ 3 . 5 %之间 ,标准回收率为 93 %～ 1 0 7%。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中铜、锌、钙、镁、铁

样品经硝酸-高氯酸消化溶解,高氯酸冒烟,盐酸溶解盐类后,在盐酸(5%)介质中,在选定的测定条件下,用电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中微量元素铜、锌、铁、镁、钙。选择Cu 327.3、Zn 206.2、Fe 238.2、Mg 279.5、Ca 315.8nm分别作为铜、锌、铁、镁、钙的分析线与混合标准溶液同时测定;方法加标回收率为98.6%～101%,铜、锌、铁、镁、钙的精密度(RSD,n=8)为0.37%～2%,准确度(RE)为-3.4%～1.15%,检出限分别为0.002 3、0.001 6、0.004 6、0.003 0、0.001 4μg/mL。方法克服了分光光度法和原子吸收光谱法操作繁琐、周期长、成本高、灵敏度低等缺点。用于测定人发样品中的铜、锌、铁、镁、钙元素,测定结果与原子吸收光谱法测定值基本一致。经GBWO7061标准物质和自制标样分析验证,测定值与标准值吻合,结果准确可靠。     

电感耦合等离子体质谱法同时检测红枣中铅、砷、镉、汞、铜、锌和16种稀土元素

为了研究哈密、若羌和和田红枣中铅、砷、镉、汞、铜、锌和16种稀土元素的含量情况,了解红枣重金属及稀土元素摄入的风险,建立同时检测红枣中铅、砷、汞、铜、锌和16种稀土元素的方法。红枣样品用微波消解法进行样品前处理,以电感耦合等离子体质谱法测定红枣中铅、砷、镉、汞、铜、锌和16种稀土元素的含量。各元素校准曲线的相关系数均大于0.999 0,检出限为0.01~0.05μg/L。加标回收率为92.1%~105.2%,测定结果的相对标准偏差为1.2%~3.6%(n=6)。用该方法测定苹果标准物质(GBW 10019),测定值与标准值一致。该方法适用于红枣类样品中多元素污染物快速检测及风险评估,红枣样品分析结果表明铅、砷、镉、汞、铜和稀土元素在3种红枣中的含量较低,风险监测数据表明红枣中存在重金属铅、镉摄入性风险。     

三元硝酸盐预氧化熔融制样-波长色散X射线荧光光谱法测定锌精矿中锌、铜、铅、铁、铝、钙和镁

锌精矿属富锌、高铜、高铅的硫化矿矿物,硫和铜等元素腐蚀铂金坩埚是熔融制样-X射线荧光光谱分析必须解决的问题。在阶梯温度下,以硝酸铵、硝酸钠和硝酸锂的三元硝酸盐混合物为氧化剂,采用半熔法预氧化试料中的硫、铜、锌等元素,以四硼酸锂-偏硼酸锂混合熔剂(m:m=67∶33)为熔剂、过饱和溴化锂溶液为脱模剂,于1 050℃熔铸成XRF分析用试料片,波长色散X射线荧光光谱仪测定试料片中的锌、铜、铅、铁、铝、钙和镁含量。以系列铜、铅、锌的硫化矿及其精矿有证标准物质和工作基准试剂氧化锌作为标准试料建立待测组分的校准曲线,各待测组分的校准曲线的相关系数在0.988 5～0.997 8;方法检出限为0.018%～0.50%。对不少于3个水平的待测组分进行实验室内重复性实验,其相对标准偏差(RSD,n=11)在0.41%～3.9%,除个别分析结果外,测定结果与标准方法的测定结果无显著性差异;经t-检验,锌精矿标准物质中铅和铁测定值与标准值无显著性差异,而锌测定结果与标准值存在显著性差异;除个别水平样品的锌含量、铁含量、钙含量测定值外,测定值与标准方法的测定值无显著性差异。8个实验室对不少于3个水平的待测组分进行5次独立测定,确定了校准曲线测定范围内的方法重复性限和再现性限。     

ICP-AES法测定锌阳极中的铝、镉、铁、铜、铅

通过分析高频功率、雾化压力、辅助气流量和泵速等试验条件，建立了ICP-AES法测定锌阳极中铝、镉、铁、铜、铅的方法。用该方法测定锌阳极中的铝、镉、铁、铜、铅，其RSD分别为0.17%、0.63%、2.7%、5.2%、2.5%，回收率分别为99.3%-101.2%，99.3%-100.3%、97.1%-102.2%、97.8%-102.9%。对锌阳极试样进行测定，该方法的测定结果与GB4951-85方法的测定结果基本一致。     

污泥上培植的黑麦草中微量元素的测定

对污泥增培黑麦草中锌、铜、镍、铬、铅的测定方法进行了研究,样品用HClO4-HNO3(1 4)进行处理,并用火焰原子吸收光谱法对锌、铜、镍、铬、铅进行了测定。结果表明:该法准确、回收率高,平均回收率分别为:锌90.3%、铜92.0%、镍88.4%、铅85.1%、铬82.6%。     

血清铜、锌、硒与恶性淋巴瘤关系的研究

测定６８例恶性淋巴瘤患者血清铜、锌、硒及铜／锌比值水平,采用ｔ检验和非条件Ｌｏｇｉｓｔｉｃ回归因素分析方法对测定结果进行分析。结果表明恶性淋巴瘤患者血清铜、铜／锌比值升高,而血清锌及硒水平降低。血清铜和铜／锌比值升高与肿瘤的负荷状态及病期明显有关,提示血清铜和铜／锌比值的测定对监测恶性淋巴瘤患者的病情变化有一定价值,非条件Ｌｏｇｉｓｔｉｃ多因素分析表明,血清锌、硒可能是恶性淋巴瘤发病的保护因素;而     

极谱法同时测定海水中的铜、镉、铅、锌

建立极谱法同时测定海水中铜、镉、铅、锌的含量。在10.0～35.0℃条件下,试样于–1.15 V恒压下电解,富集在汞电极上生成汞齐,并随电极电位的变化而发生氧化还原反应,产生电流,通过标准加入法进行定性和定量。铜、镉、铅、锌的检出限分别为0.64,0.14,0.17,2.0μg/L,定量限分别为2.5,0.50,0.50,10.0μg/L。样品加标回收率为80.4%～106.0%,测定结果的相对标准偏差为0.43%～6.09%(n=6)。该法具有操作简便、抗干扰性能强、灵敏度高等特点,能够满足海水中铜、镉、铅、锌的监测要求。     

火焰原子吸收法测定竹荪中的微量元素

使用灰化法处理样品,火焰原子吸收光谱法测定了竹荪中的钾、钙、钠、镁、铁、锰、铜、锌的含量。结果显示,竹荪中含有丰富的铁、锰、铜、锌4种人体必需微量元素。加标回收率为93.2%~103.2%,该法测定快速、简单,结果满意。     

Study on Determination of Six Transition Metal Ions in Biological Samples by SPE and RP‐HPLC

This paper reports the utilization of solid phase extraction and the reversed‐phase high‐performance liquid chromatography (RP‐HPLC) for the determination of six transition metal ions (iron, cobalt, nickel, copper, zinc and manganese) in biological samples. The samples were digested by microwave digestion. The iron, cobalt, nickel, copper, zinc and manganese ions in the digested samples can react with 2‐(2‐quinolinylazo)‐5‐diethylaminophenol (QADEAP) to form colored chelates in pH 4.0 acetic acid‐sodium acetic buffer solutions and cetyl trimethylammonium bromide (CTMAB) medium. These chelates were enriched by solid phase extraction with C₁₈ cartridge. Then the chelates were separated on a Waters Nova‐Pak‐C₁₈ column (3.9 × 150 mm, 5 μm) by gradient elution with methanol (containing 0.5% of acetic acid and 0.1% of CTMAB) and 0.05 mol/L pH 4.0 acetic acid‐sodium acetic buffer solution (containing 0.1% of CTMAB) as mobile phase at a flow rate of 0.5 mL/min. The detection limits of iron, cobalt, nickel, copper, zinc and manganese are 3 ng/L, 4 ng/L, 2 ng/L, 4 ng/L, 8 ng/L, 10 ng/L, respectively. This method was applied to the determination of iron, cobalt, nickel, copper, zinc and manganese in biological samples with good results.     

福建长乐市学龄前儿童末梢血矿物质检测结果分析

为了解福建省长乐市学龄前儿童体内矿物质钙、镁、铁、锌、铜的含量与年龄和性别的关系,探讨防治其缺乏的综合措施,利用BH 5100型原子吸收光谱仪对4 231例学龄前儿童末梢血中钙、镁、铁、锌和铜元素进行了检测,采用SPSS 17.0软件进行统计分析。结果表明,该地区学龄前儿童末梢血锌元素含量有3个年龄组低于正常值;其中锌、铁元素缺乏严重,缺乏儿童分别占总样本的61.92%和34.60%;末梢血中矿物质含量在部分年龄组和性别之间比较差异有统计学意义(P<0.05)。提示该地区学龄前儿童铁、锌元素缺乏明显,应定期检测并加强膳食中微量元素铁和锌的补充,保证儿童的健康成长。     

沈阳市学龄前儿童末梢血矿物质检测结果分析

为了解沈阳市学龄前儿童体内矿物质钙、铁、锌、铜、镁的含量与年龄和性别的关系,探讨防治其缺乏的综合措施,利用BH 5100型原子吸收光谱仪对3483例学龄前儿童末梢血中铜、锌、钙、镁和铁元素进行了检测,采用SPSS 17．0软件进行统计分析。结果表明,该地区学龄前4个不同年龄组儿童末梢血锌、钙、铁、铜元素缺乏严重,分别占总样本的66．90％、39．76％、32．5％和26．87％;3～岁组末梢血中钙、铁、锌、镁含量与其它年龄组比较差异有统计学意义（P〈0．05）,各元素在性别问差异无统计学意义（P〉0．05）。该地区学龄前儿童钙、铁、锌、铜失衡明显,应加强营养素的合理搭配及矿物质的补充,保证儿童的健康成长。     

Sequential determination of trace amounts of iron and copper in water samples by flow injection analysis with catalytic spectrophotometric detection.

A simple flow injection analysis (FIA) method is described for the sequential determination of iron and copper. The detection method for iron and copper is based on their catalytic activities in the oxidation reaction of N,N-dimethyl-p-phenylenediamine (DPD) with hydrogen peroxide. The sequential determination of iron and copper can be carried out by injecting two sample plugs into the FIA system, sequentially. One injection does not contain triethylenetetramine (TETA), and is used for the sum of iron and copper concentration; the other which contains TETA is used only for the iron concentration. For iron determination, TETA is used as a masking agent of copper. The difference in peak height can be used for the calculation of copper concentration. Under the optimal conditions, the detection limits (3sigma) of 0.01 and 0.07 microg L(-1) were obtained for iron and copper, respectively. The proposed method can be applied to the determination of iron and copper in tap water and bottled-drinking mineral water samples. Good recoveries of the method, 98-103% for iron and 98-106% for copper, were achieved.     

Determination of transition metal ions in tobacco as their 2-(2-quinolinylazo)-5-dimethylaminophenol derivatives using reversed-phase liquid chromatography with UV-VIS detection

This paper reports the utilization of solid-phase extraction and the reversed-phase high-performance liquid chromatography for the determination of six important transition metal ions: iron, cobalt, nickel, copper, zinc and manganese in tobacco with 2-(2-quinolinylazo)-5-dimethylaminophenol (QADMAP) as chelating reagent. Iron, cobalt, nickel, copper, zinc and manganese ions react with QADMAP to form colored chelates in the medium of acetic acid-sodium acetate buffer solution (pH 4.0). These chelates can be enriched by solid-phase extraction with Waters Sep-Pak-C18 cartridge, and eluted the retained chelates from cartridge with tetrahydrofuran. The chelates were separated on a Waters Nova-Pak-C18 column (150x3.9 mm, 5 microm) by gradient elution with methanol (containing 0.5% of acetic acid) and 0.05 mol/l pH 4.0 acetic acid-sodium acetate buffer solution as mobile phase at a flow-rate of 0.5 ml/min. The detection limits of iron, cobalt, nickel, copper, zinc and manganese are 10, 12, 8, 13, 17 and 22 ng/l, respectively. This method had been applied to the determination of iron, cobalt, nickel, copper, zinc and manganese in tobacco with good results.     

Flow injection and microwave-oven sample decomposition for determination of copper,zinc and iron in whole blood by atomic absorption spectrometry

A simple and rapid method is proposed for the determination of copper, zinc and iron in whole blood. The injected sample is mineralized in the flow system on passage through a microwve oven and the metals are determined by atomic absorption spectrometry. Prior sample destruction or removal of organic material prior to injection is not necessary. The required volumes for each analysis are 90, 60 and 100 μl for copper, zinc and iron, respectively. The relative standard deviations were less than 3% in all cases. There was good agreement between the results obtained with the flow-injection method and those attained by conventional spectrophotometric measurements.     

西安市老年人末梢血铜、锌、铁、镁、钙元素含量分析

为调查60岁以上老年人体内微量元素及钙、镁的含量,采用原子吸收光谱法对西安市60岁以上的老年人末梢血中的铜、锌、铁、镁、钙的含量进行了测定,观察了5元素的缺乏率及随年龄的增长5元素的缺乏情况.结果表明,60岁以上老年人,元素过量的情况鲜见;铜、锌、铁、镁、钙的缺乏率分别为37.87%0,11.76%,21.51%,2....     

花椒中五种微量元素含量的测定

采用原子吸收光谱法,测定了河南太行山区花椒及椒皮、椒籽中锰、铁、铜、锌、铅的含量。结果显示,各元素在实验范围内,线性关系良好,回收率在92%~103%之间。花椒及椒皮、椒籽中均含有微量元素,花椒中锰、铁、铜、锌、铅的含量分别为78.851、90.868、11.571、18.818、0.086μg.g-1,其中锰、铁含量丰富,有害元素铅的含量极低。椒籽中铁、铜、锌的分布量大于椒皮;椒皮中锰的分布量大于椒籽。为探讨花椒的高药用价值提供了有力的证据,椒籽中铜、锌、铁含量高于椒皮,应大力开发利用。     

Metal — organic interactions in sea water: an ecosystem experiment

A model plankton ecosystem was used to study the interactions of trace metals and organic compounds over a 10-day period during a phytoplankton bloom. Six bags of 1200–1 capacity were filled with coastal sea water. Three bags were spiked with copper (78, 157 and 314 nM) and one with copper (4.57 μM) plus nitrilotriacetic acid (10 μM). Samples were analysed for total dissolved copper, zinc, iron, nickel and manganese. The copper complexing capacity, determined by a method based on competition with Chelex-100 resin, was found to be essentially the same (35 nM) in all bags and independent of time. Organically bound complexes of copper (18% of the total), zinc (7%), nickel (4%) and iron (2%) were isolated by adsorption on Sep-Pak cartridges. The metal—organic complexes, were analysed on a liquid chromatograph interfaced to a multichannel atomic fluorescence detector. Organic complexes of zinc, iron and nickel were formed even in the presence of a large excess of copper. The organic and metal—organic compounds isolated by Sep-Pak cartridges became more polar as the bloom progressed.