The determination of lead in environmental and geological materials by proton activation analysis

Lead is determined in environmental samples and in rocks using the^206,207,208Pb(p,xn)²⁰⁶Bi reaction. Bismuth is separated by anion exchange or by extraction with antimony diethyldithiocarbamate. Sources of errors such as volatilization of the matrix due to heating during the irradiation, variations of the abundance of the lead isotopes and the standardization were studied in detail. For concentrations between 11 mg/g and 3.7 g/g the relative standard deviation ranges from 2.6 to 5.4%. The detection limit is 10 ng/g.     

Sorption-photometric determination of anionic surfactants in water

The adsorption of Crystal Violet, anionic surfactants, and their ion associates on nonionic hydrophobic polymer adsorbent Amberlite XAD-16 was studied. A procedure for the sorption-photometric determination of anionic surfactants in water was developed with a detection limit of 0.001–0.003 mg/L at a sample volume of 50 mL.     

Atomic-absorption determination of lead in geological materials

A method is described for the determination by atomic-absorption spectrophotometry of lead, tip to the milligram level, in samples of geological materials. After attack with perchloric-hydrofluoric acid mixture and the removal of perchlorate ion by precipitation as potassium perchlorate, lead is separated from matrix elements by means of anion-exchange in 2M hydrobromic acid on the strongly basic anion-exchange resin Dowex 1 x 8. Lead is adsorbed on the resin column while practically all other accompanying elements pass into the effluent. For the elution of lead 6(M) hydrochloric acid is used and after evaporation of the eluate lead is determined by atomic-absorption spectrophotometry. The method was tested by analysing numerous samples with contents ranging from a few ppm to milligram amounts of lead. In most cases very good agreement of results was obtained.     

Determination of lead in environmental reference materials (plant materials) by slurry-ETA-AAS

Slurry-ETA-AAS is used to determine lead in plant materials. The stability of the slurry was studied and it was shown that, when NH₄H₂PO₄ modifier is added, the shape of the time resolved absorbance signal for the sample and the standards is similar and the calibration line obtained using aqueous standards is parallel to the standard addition line. Results obtained for several reference materials (lead contents between 6.1 and 64.4 g/g) were in good agreement with the certified value, the relative standard deviation being 3–9%.     

能量色散型X射线荧光光谱法测定聚合物材料中镉和铅含量

提出了能量色散型X射线荧光光谱测定聚合物材料中镉和铅的测试分析方法及制样技巧。按照仪器分析条件测定同时含有镉和铅的6块不同浓度级别的标准物质来建立校准工作曲线,其线性范围分别在250ug·g-1、1100ug·g-1以内。镉和铅的方法检出限依次为4.7ug·g-1、4.1ug·g-1。该方法应用于测定欧洲标准物质ERM-EC680和ERM-EC681k,其镉和铅的实际测定值与标准物质证书的标称值相符,测定实际样品中的镉和铅的回收率介于90~110%。该方法测定标准物质和实际样品中镉和铅的精密度均小于10%。     

Differential pulse polarographic determination of nitrate in environmental materials

Nitrate can be determined with reliable accuracy and sensitivity by differential pulse polarography utilizing the catalytic reaction between nitrate and uranyl ion in the presence of potassium sulphate. The differential pulse polarographic peak-height is proportional to nitrate concentration from 1 to 50 muM. The calculated detection limit for nitrate is 8 x 10(-7)M in pure aqueous solution. The method has been applied to determination of nitrate in fresh snow, and river waters and animal feeds.     

Enzymatic determination of cadmium,zinc, and lead in plant materials

Prospects are outlined for using the following enzymes (native and immobilized on polyurethane foam) in the rapid and highly sensitive determination of cadmium, zinc, and lead ions in plant materials (wild grass, fresh pea, and grape): horseradish peroxidase and alkaline phosphatases isolated from chicken intestine and Greenland seal small intestine. The analytical ranges of the above metals are 1 × 10^–3?25, 7 × 10^?3?250, and 3 × 10^?2?67 mg/kg dry matter, respectively. The enzymatic determination procedures developed are based on the inhibiting effect of metal ions on the catalytic activity of peroxidase in the oxidation of o-dianisidine with hydrogen peroxide and alkaline phosphatases in the hydrolysis of p-nitrophenyl phosphate. The rates of enzymatic reactions were monitored spectrophotometrically or visually. In the analysis of plant extracts, their high acidity was diminished by choosing optimum dilution factors and pH values for test samples and the nature and concentration of a buffer solution. The interference of iron(III) was removed by introducing a 0.1 M tartaric acid solution into the indicator reaction. The accuracy of the results of the enzymatic determination of cadmium, zinc, and lead in plant materials was supported by atomic absorption spectrometry and anodic stripping voltammetry.     

The determination of iodine in biological and environmental standard reference materials

Iodine is an element with excellent intrinsic sensitivity when determined by thermal neutron activation. However, in most real samples, the preponderance of chlorine and bromine, relative to iodine, makes the direct determination of iodine virtually impossible. Over the past 20 years, there probably have been as many publications on the separation of iodine as there have been for any other radionuclide. Upon review, however, the methods are essentially the same. After irradiation, the samples are subjected to a rapid destructive process to free the iodine from the matrix and then the iodine is separated from the other halides either by liquid-liquid extraction or by liquid ion exchange. Both of these procedures are, however, rather complex and do not effect a complete separation of the halides in one pass. In the work presented here, a simple procedure is described for the quantitative separation of iodine from chlorine. The procedure utilizes a gas phase separation on hydrated manganese dioxide with iodine collected on silvered quartz wool. The described procedure has been used for the determination of iodine in numerous new and old SRM's at the NBS.     

The determination of low levels of polonium-210 in environmental materials

A method is presented for the determination of polonium-210 at very low levels in the presence of many different ions. Essentially quantitative recoveries were obtained in 60 min by deposition on to a silver plate in a special holder from 50 ml solution at 85–90° with sodium citrate present.     

Atomic-absorption spectroscopic determination of lead in biological materials by direct solid microsampling

Summary Graphite furnace atomization has been used in the AAS determination of lead in some biological materials (seaweed, vine leaves and edible portion of mussel) with the slurry technique and in solutions of the ashed samples. A hyperbolic calibration graph is adopted, which can be linearized, allowing matrix interferences on the calibration graphs to be assessed by means of the statistical analysis of variance for the linear regression applied to standard additions. The procedure suggested shows that for sampling mussel as a slurry, the analytical sensitivity for lead is about one third of that for the standard solutions. A physical loss of metal before the residue can be decomposed to produce atomic lead is suggested. The occlusion of the analyte in the carbon particles is suggested as a major mechanism. This decrease in sensitivity does not occur with slurries of seaweed or of leaves or with solutions of ashed materials. Both methods show an accuracy comparable to that of macro- and semimicro reference procedures.

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Atomabsorptions-spektroskopische Bestimmung von Blei in biologischem Material unter direkter Verwendung fester Proben

Zusammenfassung Für die Bestimmung des Bleigehalts in biologischer Matrix (Seetang, Weinstockblätter und Miesmuschelfleisch) wurde die flammenlose Atomabsorptionsspektroskopie verwendet. Der Bleigehalt wurde in Aschelösungen und in wässeriger Suspension pulverisierter Proben bestimmt. Eine hyperbole Eichkurve wurde verwendet, die linearisiert werden kann, indem Matrixstörungen der Eichkurve durch statistische Varianzanalyse kontrolliert werden, wenn die Standardadditionsmethode verwendet wird. Die beschriebene Arbeitsweise zeigt, daß die analytische Empfindlichkeit für Blei nur ein Drittel im Vergleich zur Standardlösung ist, wenn die Miesmuschel in Suspension analysiert wird. Ein physikalischer Metallverlust ist zu vermuten, wobei wahrscheinlich eine Okklusion in den verkohlten Partikeln erfolgt. Keine Empfindlichkeitsminderung ist bei der Analyse von Suspensionen des Seetangs und der Blätter oder der Lösungen veraschter Proben bemerkbar. Beide Methoden zeigen eine Treffsicherheit, die mit der anderer Makro- und Semimikromethoden vergleichbar ist.

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Presented at the 8th International Microchemical Symposium, Graz, August 25–30, 1980.     

224Ra correction for determination of 226Ra in environmental materials

The most commonly available 226Ra determination was too time-consuming to be suited to 226Ra monitoring for the accidental release. The formula for determination of 226Ra was derived by 224Ra correction for WHO's equation. A rapid determination of 226Ra in environmental materials was made possible by using this formula. The 226Ra values of the soil and natural water at Ningyoh-Tohge obtained by the present method were in good agreement with those by the conventional WHO method. It was demonstrated that 226Ra of more than about 37 mBq (1 pCi) in the sample could be determined within 4 days by this method.     

Atomic absorption spectrometric determination of copper,zinc, and lead in geological materials

An atomic absorption spectrometric method is described for the determination of copper, zinc, and lead in geological materials. The sample is digested with HF—HCl—H₂O₂; the final solution for analysis is in 10 % (v/v) HCl. Copper and zinc are determined directly by aspirating the solution into an air—acetylene flame. A separate aliquot of the solution is used for determination of lead; lead is extracted into TOPO-MIBK from the acidic solution in the presence of iodide and ascorbic acid. For a 0.50-g sample, the limits of determination are 10–2000 p.p.m. for Cu and Zn, and 5–5000 p.p.m. for Pb. As much as 40 % Fe or Ca. and 10 % Al, Mg, or Mn in the sample do not interfere. The proposed method can be applied to the determination of copper, zinc, and lead in a wide range of geological materials including iron- and manganese-rich, calcareous and carbonate samples.     

New certified reference materials and proficiency test for environmental radioactivity measurements

A reliable determination of natural and anthropogenic radionuclides in environmental samples is necessary to comply with the radiation protection and environmental regulations. This paper presents the results of the characterisation of massic activities of natural and anthropogenic radionuclides in soil and water matrices produced as test items to conduct the proficiency test ERAD-PT-2013. The proficiency test ERAD-PT-2013 was designed to investigate analytical performance in analysing both natural and anthropogenic radionuclides, to assist laboratories to identify analytical problems, and to improve the quality of measurement results. The proficiency test items, their spectral interferences and the activity concentration levels of the analytes were designed in a way to enable identification of potential analytical problems. Methodologies, data evaluation approach and evaluation of proficiency test results for each radionuclide are described and discussed.     

Recent advances in the determination of low level plutonium in environmental and biological materials

The present paper reviews briefly the recent advance in radioanalysis of low level plutonium in environmental and biological samples. Lots of new radiochemical methods for determination of plutonium in aerosols, natural waters, soil, sediments and various biological materials have been developed. The use and prospects of several radiochemical procedures are discussed.     

Possibilities of ion-exchange methods for isolation and determination of transplutonium elements in environmental materials

The methods of TPE isolation and separation from all accompanying and interfering elements, using only one or two ion-exchange columns and mineral acid solutions are proposed. The difficulties of TPE determination in environmental samples and advantages of the methods are discussed.     

Radiochemical proton activation analysis for the determination of cadmium and lead in sediment reference materials

Proton activation analysis was used for the determination of cadmium and lead in three sediment reference materials. The method is based on the^111,112Cd(p, xn)¹¹¹ In and the^206,207,208Pb(p, xn)²⁰⁶Bi reactions.¹¹¹In and²⁰⁶Bi were chemically separated by anion exchange. The results obtained were taken into account for the certification of the materials and are in the excellent agreement with the certified values.     

Particle size determination of some IAEA and NIST environmental and biological reference materials

Particle size distributions in fifteen International Atomic Energy Agency (IAEA) and sixteen National Institute of Standards and Technology (NIST) reference materials (RMs) were measured with the basic aim to investigate the potential of these materials to be used as reference or quality control materials in analyses where a small sample mass is required (< 100 mg). Most of the investigated materials are commercially available environmental or biological natural matrix RMs with certified values for trace elements, radionuclides, or organometallic compounds. The laser diffraction technique was used in all measurements. From the point of particle size distribution, materials IAEA-390 (Algae, a set of three materials), IAEA-396m (Urban Dust, 3x air jet milled), NIST-SRM 1515 (Apple Leaves), NIST-SRM 1547 (Peach Leaves), NIST-SRM 1566a (Oyster Tissue), NIST-SRM 1570a (Spinach), NIST-SRM 1573a (Tomato Leaves), and NIST-SRM 1648 (Urban Particulate) can be considered appropriate for small sample mass analysis. However, additional analytical tests are needed to confirm the appropriate homogeneous distribution of chemical composition, the level of heterogeneity for individual elements, at this sample mass level.     

Spectrophotometric determination of lead in environmental objects with the new highly effective reagent HOCAC

Summary A simple method has been developed for determination of traces of lead with the new organic reagent HOCAC (hexaoxacycloazochrom). The method was used for lead determinations in waters, soils and food after extraction or sorption of the lead followed by direct reagent addition to the acid re-extract or eluate. It is possible to determine Pb down to 2 g in 1 l water after extraction or down to 10 g in 1 l water and down to 500 g in 1 kg potatoes or soil after sorption.