Lead determination in wine by potentiometric stripping analysis

Summary Computerized potentiometric stripping analysis (PSA) was used for lead determination in wine samples. In this method sample preparation before determination is limited to dilution with an appropriate supporting electrolyte (0.5 mol/l HCl and 40 mg/l Hg²⁺). Due to the very high sensitivity, the time needed for one determination can be reduced to 2 min. The method was tested by lead determination in different wines, different concentration ranges and in one European interlaboratory comparison organized by BCR. Using PSA it is possible to simultaneously determine cadmium, lead and copper in wine. For other elements such as Bi, Tl, Hg, Sn, As, Zn the determination procedures are under development. The PSA equipment is available on the market, small in size, relatively cheap and it does not require any special installation such as gas or cooling water.     

Interlaboratory quality control for lead determination in wine by potentiometric stripping analysis

Summary Computerized potentiometric stripping analysis (PSA) was used for the determination of lead in wine samples. With this analytical method the sample preparation is limited to dilution with an appropriate supporting electrolyte (0.5 mol/l HCl and 40 mg/l Hg²⁺). Due to very high sensitivity the time needed for one determination can be reduced to 2 min. This method for lead determination in wine was compared with results from voltammetry and ETAAS from various laboratories participating in two BCR studies. With PSA it is possible to determine cadmium, lead and copper in wine after a single dilution with an appropriate supporting electrolyte. For other elements such as Bi, Tl, Hg, Sn, As, Zn determination procedures are under development.     

智能石墨消解–ICP–MS法测定空气PM2.5中的Pb和Cd

建立电感耦合等离子体质谱(ICP–MS)测定空气PM2.5中的Pb和Cd元素的分析方法。采用连续β射线–DHS PM2.5大气颗粒物浓度监测仪采集空气中的PM2.5,以智能石墨消解PM2.5滤膜样品,ICP–MS测定其中的Pb和Cd元素含量。在优化的仪器条件下,元素Pb和Cd标准曲线的线性相关系数均为0.999 9,检出限分别为0.018,0.52ng/m3,满足HJ 657–2013的要求。Pb和Cd的加标回收率分别为95.8%~101.4%,99.3%~104.9%,测定结果的相对标准偏差分别为4.20%和2.38%(n=6)。对滤膜标准样品进行了测定,测定结果与标准值一致。该方法测定结果准确、可靠,可用于测定空气PM2.5中的Pb和Cd。     

Determination of cadmium, lead and copper in wine by potentiometric stripping analysis

A procedure for the determination of Cd, Pb and Cu in different wine samples after simple sample preparation on a mercury film electrode (MFE) by potentiometric stripping analysis (PSA) is presented. In 150 German wine samples collected in 1993/94 the following values were found: Cd mean: 0.63 ng/mL (range: 0.003– 0.98 ng/mL); Pb mean: 50 ng/mL (range: 4–254 ng/mL); Cu mean: 250 ng/mL (range: 50–394 ng/mL).     

纳米二氧化钛分离富集石墨炉原子吸收光谱法测定水样中痕量铅

提出了纳米TiO2分离富集,GFAAS测定水样中痕量铅的新方法。详细考察了纳米TiO2对铅的吸附行为,结果表明：在pH4．0时,Pb^2 可被纳米TiO2定量富集,吸附于纳米TiO2上的Pb^2 可用0．1mol／L的硝酸完全解脱。本法对Pb^2 的检出限为52ng／L,相对标准偏差为4．7％(n=10,C=0．02mg／L)。本法已用于实际水样中铅的测定,结果满意。     

微波消解–ICP–OES法测定陶土中铅和镉含量

建立微波消解–ICP–OES法测定陶土中铅和镉含量的方法。采用氢氟酸–硝酸作为消解液,微波消解法处理样品,消解液定容后直接进入耐氢氟酸的进样系统,用ICP–OES法测定陶土中重金属铅和镉的含量。结果表明,Pb和Cd检出限分别为0.027μg/m L和0.011μg/m L,回收率分别为90.5%~98.8%和95.0%~98.4%,测定结果相对标准偏差分别为1.38%和2.17%(n=7)。该方法具有快速、准确、灵敏度高等优点,适用于陶土中铅和镉含量的检测。     

Present potential of electrochemical methods for metal determinations in reference materials

Summary Based on high-pressure ashing, the potential to determine some trace metals (Zn, Cd, Pb, Cu, Ni, Co, Al, Tl, Cr, Fe) by anodic or cathodic stripping voltammetry in the square wave (SWV) and differential pulse modes (DPASV) is described. In comparison to the differential pulse mode, the square wave mode shows advantages for cathodic stripping and for zinc determination.New developments by use of potentiometric stripping analysis (PSA) permit the determination of Pb and Cd in whole blood without sample pretreatment and Pb, Cd, and Cu in milk and milk powder with simple pretreatment.Mercury film microelectrodes prepared by electrodeposition of Hg onto a carbon fiber were used for the rapid multicomponent trace determination of heavy metals in very small (5 l) samples by voltammetry and potentiometry.

---

Gegenwärtiges Potential elektrochemischer Methoden für Metallbestimmungen in Referenzmaterialien

     

流动注射分析光泽精-H2O2-Pb(Ⅱ)化学发光体系测定痕量铅的研究

检测铅离子常用的方法有AAS法和双硫腙比色法,前者直接测定工业废水中的铅,灵敏度不高;后者操作步骤繁琐,须使用剧毒试剂氰化钾,污染环境,用流动注射化学发光法测定铅,仪器简单、操作简便、试样消耗量少、精密度高、分析快速准确、自动化程度高。     

微波消解-ICP-OES法测定汽车涂料中8种重金属

建立微波消解-电感耦合等离子体发射光谱(ICP-OES)测定汽车涂料中Pb,Cr,Se,Ba,Sb,As,Cd,Hg含量的方法。以HNO_3-H_2O_2(体积比为4∶1)混合酸消解样品,各元素分析谱线:Pb 220.353 nm,Cr 267.716 nm,Se196.090 nm,Ba 233.527 nm,Sb 217.581 nm,As 189.042 nm,Cd 228.802 nm,Hg 184.950 nm。8种元素测定结果的相对标准偏差为2.02%~12.94%(n=6);对白色、蓝色、红色汽车漆样品进行加标回收试验,Pb,Cr,Se,Ba,As,Cd,Hg,的加标回收率为81.26%~99.79%,Sb的回收率为62.43%~87.61%。该方法快速、简便,精密度、准确度较高,可用于汽车涂料中重金属含量的监控。     

石墨炉原子吸收光谱法测定中药口服液中的铬铅镉

利用石墨炉原子吸收光谱法测定,采用常温消解和密闭微波消解等方式处理口服液样品,并进行比较。结果表明,采用HNO3 HClO4 H2O2作为消解试剂用常温消解方式进行消解后,可不加基体改进剂直接进行测定,在此基础上研究了石墨炉原子吸收测定的最佳条件。应用这种方法测定了双黄连、清开灵、生脉饮和抗病毒口服液中痕量镉、铬和铅,RSD小于5．0％,回收率在83．4％～113％。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定铜砷滤饼中的Pb、Fe、Bi三种元素

采用硝酸、盐酸、氢氟酸、高氯酸分解样品,氢溴酸-盐酸挥发消除砷基体,优化仪器测定参数,选取最佳工作条件,建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铜砷滤饼中Pb、Fe、Bi元素的分析方法。其测定范围为：ω(Pb):0.12%~2.09%;ω(Fe):0.081%~2.10%;ω(Bi):1.20%~6.14%。各元素检出限为Pb:0.010μg/mL;Bi:0.006μg/mL;Fe:0.003μg/mL。加标回收率为95.5%~101.7%。该方法简便,准确,可靠,适用于铜砷滤饼中Pb、Fe、Bi元素的同时测定。     

Simultaneous determination of lead, nickel, tin and copper in aluminium-base alloys using slurry sampling by electrical discharge and multielement ETAAS

The simultaneous multielement determination of Pb, Sn, Ni and Cu in aluminium alloys by electrothermal atomic absorption spectrometry (ETAAS) was performed by a quick method using slurry sampling. The metallic colloidal slurries were obtained by an electrical discharge operated in liquid medium. In this work, the effects of aluminium were evaluated and the results show that it causes a strong retention of Pb, Ni and Cu at low pyrolysis temperatures which is overcome by employing high pyrolysis temperatures. Aluminium also significantly improves the thermal stabilisation of Pb and Sn, it being possible to reach pyrolysis temperatures of 1100 and 1300 °C, respectively. Such stabilisation indicates that the performance of aluminium as a matrix modifier for Pb is better than that obtained using phosphate and magnesium nitrate without substantial changes of the figures of merit. The effects of aluminium on the atomisation characteristics of the elements and those coming from the simultaneous multielement determination on the figures of merit of the elements are also discussed. In this work, a calibration procedure involving a matrix matching method with aqueous aluminium standards is proposed as a simple and efficient way to solve the inconveniences originated by the aluminium matrix. The proposed method was applied to the simultaneous multielement determination of several aluminium-base alloy standards giving results well within the recommended values.     

Enantiomeric separation of basic drugs with partially filled serum albumin as chiral selector in capillary electrophoresis.

A reliable method is presented for the chiral separation of three basic drugs (mexiletine, chlorpheniramine and propranolol) with serum albumins (human and porcine, HSA and PSA) as chiral selectors by capillary electrophoresis in combination with the partial filling technique. Based on the systematic optimization of operation variables, the chiral separation of mexiletine, chlorpheniramine and propranolol was achieved in the pH 7.4 phosphate buffer by using HSA, PSA and PSA as selectors, respectively. The chiral recognition ability of HSA and PSA was compared. HSA and PSA show a different chiral recognition ability for each of the three drugs. In addition, the association constants between enantiomeric drugs and proteins were determined to be 2.00 and 3.80 x 10(2) M(-1) for mexiletine and HSA, 0.59 and 1.12 x 10(3) M(-1) for chlorpheniramine and PSA, and 0.87 and 1.42 x 10(3) M(-1) for propranolol and PSA. The method for the chiral separation and determination of association constants possesses the advantages of simple performance, effective avoiding of the interference of the UV detection from protein, and lowering of the reagent consumption.     

Lead as own luminescent sensor for determination

In our experiments, it was observed that adding bromide to Pb2+ solution of N,N'-dimethylformamide (DMF), the highly emissive cluster Pb4Br11(3-) can be formed and the fluorescence intensity of the formed cluster is proportional to the concentration of Pb2+, based on which, a novel, simple approach that uses the emission from itself as the sensor for determination of Pb2+ is proposed. Under the optimum conditions, the linear range and detection limit is 1.0 x 10(-7) to 1.0 x 10(-5) mol l(-1) (correlation coefficient r = 0.9997) and 7.6 x 10(-9) mol l(-1), respectively. Foreign substrates effects were also investigated. The proposed method has been successfully applied to the determination of lead in the synthetic samples. The mechanism of the reaction is also studied.     

Determination of iron and lead by flame atomic absorption spectrometry after preconcentration with sepiolite

By using a new adsorbent (sepiolite) an adsorption-elution and atomic absorption spectrometric method has been developed for the preconcentration and determination of Fe and Pb. Recoveries of the analytes were 82 ± 3% for Fe and 91 ± 2% for Pb at 95% confidence level. For Cu it was only 5 ± 1%. The recovery of iron could be increased to about 97 ± 1% by complexing with EDTA, the recovery of copper only to 57 ± 2%. The optimised method was applied to the determination of lead in metal materials (e.g. brass). Received: 20 February 1996 / Revised: 7 May 1996 / Accepted: 11 May 1996     

海水中铜锌铅镉的萃取-反萃取法同时提取-原子吸收光谱法测定

采用萃取-反萃取法同时提取出海水中Cu、Zn、Pb、Cd,Cu、Pb、Cd石墨炉法测定,Zn用火焰法测定.对样品的前处理方法和最佳仪器条件进行了研究,并通过加标实验验证了方法的可靠性.结果表明:萃取-反萃取法能完全满足海水中Cu、Zn、Pb、Cd的前处理要求,可节省一半前处理时间,有溶液稳定、环保、节省试剂等优点.     

Potentiometric stripping analysis (PSA) for monitoring of antimony in samples of vegetation from a mining area

A potentiometric stripping analysis (PSA) method has been developed and checked for the fast and reliable determination of antimony in vegetation samples of Cistus ladanifer from a mining area in Badajoz, Southwest Spain. The method, modified from previous PSA methods for Sb in environmental samples, is based on dry ashing of the homogenized leaves, dissolution in hydrochloric acid, and PSA analysis on a mercury film plated on to a glassy carbon disk electrode. The influence of experimental variables such as the deposition potential, the deposition time, the signal stability and the calibration parameters, has been investigated. The method has been compared with an independent technique (instrumental neutron activation analysis) by analysis of standards and reference materials and comparison of the results. As a result of automation of the PSA equipment, the proposed method enables unattended analysis of 20 digested samples in a total time of 2 h, thus providing a useful tool for Sb monitoring of a large number of samples.     

Turn-on fluorescence probe for selective detection of Hg(Ⅱ)by calixpyrrole hydrazide reduced silver nanoparticle: Application to real water sample

A simple and quick method for the synthesis of water dispersible stable silver nanoparticles has been developed. Calix[4]pyrrole octahydrazide(CPOH), has been successfully used as a reducing as well as stabilizing agent for the synthesis of silver nanoparticles. CPOH-AgNps have been duly characterized by SPR, PSA, TEM and EDX-ray. The ability of CPOH-AgNps as selective and sensitive sensor for various ions(Pb(Ⅱ), Cd(Ⅱ), Mn(Ⅱ), Fe(Ⅲ), Ni(Ⅱ), Zn(Ⅱ), Hg(Ⅱ), Co(Ⅱ), Cu(Ⅱ)) by colorimetry and spectrofluorimetry has been explored. CPOH-AgNps were found to be selective only for Hg(Ⅱ) ions. Nanomolar concentration of Hg(Ⅱ) ions can also be determined by spectrofluorimetry by increase in fluorescence intensity. Linear range of detection of Hg(Ⅱ) ions in water was found to be from 1 nmol/L to 1 μmol/L. The method has been successfully applied for determination of Hg(Ⅱ) ions in ground water and industrial effluent waste water samples.     

Ammonium Acetate Extracts and Their Analysis for the Speciation of Metal Ions in Soils and Sediments

Abstract

The use of ammonium acetate (1 mol/l at pH 7) extraction of soils and sediments for the speciation of metal ions is briefly discussed. Because the sensitivity of flame atomic absorption spectrometry (FAAS) is insufficiently sensitive for the determination of many of the heavy metals in ammonium acetate extracts of unpolluted, and even in some polluted soils, the use of electrothermal atomic absorption spectrometry (ETAAS) was studied. A general procedure, using graphite furnace atomisation and the “universal” matrix modifier, palladium, was developed, that was sufficiently sensitive for the determination of Cd, Cr, Cu, Ni, Pb and Zn even in unpolluted soils. The concentration of zinc, however, will almost always be high enough for determination of FAAS and this method is to be preferred to ETAAS for this element.

While, for Cr, Cu, Ni and Pb, direct calibration with external standard solutions is practicable, it is necessary to use the standard additions calibration method for cadmium, to avoid matrix interference effects. The standard additions technique is recommended, however, because it compensates for real differences in the operating parameters of different instruments set to the same nominal values. This is particularly important for interlaboratory comparisons or for certification analyses in the preparation of reference materials.