Determination of lead and atmospheric particulates by flameless atomic absorption spectrometry

Flameless atomic absorption techniques were used to determine the lead and other atmospheric particulate in the city of Tehran. 640 samples were collected in 20 different stations around the city during four seasons in 1992. The radioactivity of the air samples was also measured by -ray spectrometry using high purity Ge/Li detectors, and a multichannel analyzer. The results were compared with previous measurements in the city of Tehran.     

Determination of cadmium in air particulates by flameless atomic absorption spectrometry with a graphite tube

A sensitive and selective determination of cadmium in aerosols by flameless atomic absorption spectrometry is described. By two successive treatments in 0.1 M suprapure nitric acid, the cadmium is removed from the paper filter on which the particulates have been collected. Routinely 10–50 μl of the 100-ml solution are injected into a graphite oven and the % absorption at 228.8 nm is measured. If half a 24-h filter (400 m³ air) is used, the dilution is made to 50 ml and 50 μl is injected, an unusually low concentration of 0.20 ng m^-3 can be determined quantitatively with a relative standard deviation of 10%. The reproducibility of the complete procedure is 4.8%. An interlaboratory comparison indicated that the accuracy is very good. The same solution can also be used for lead determination mostly without any further dilution. As an application, the cadmium concentrations were measured on two different days at 14 stations of the nationwide sampling network, and the influence of nonferrous industries on the cadmium levels is shown.     

石墨炉原子吸收光谱法测定茶叶中的铅

采用石墨炉原子吸收光谱法测定茶叶中铅,以NH4H2PO4作为基体改进剂,提高了测定的灰化温度,消除了基体干扰.方法简便,快速,准确度高.通过对标准物质的多次测定,结果均在其保证值范围内,相对标准偏差为2.8%.对样品进行加标回收试验,回收率为96%～105%,方法检出限为0.12μg/L.     

Determination of lead in fine particulates by slurry sampling electrothermal atomic absorption spectrometry

A simple method for determining lead in fine particulates (PM2.5) by using electrothermal atomic absorption spectrometry (ETAAS) has been developed. Particulates collected on Nuclepore filter by using a dichotomous sampler were suspended in diluted nitric acid after ultrasonic agitation. The dislodging efficiency is nearly 100% after agitation for 5 min. In order to study the suspension behavior of PM2.5 in solvents, a Brookhaven ZetaPlus Particle Size Analyzer was used to determine the particle size distribution and suspension behavior of air particulates in the solvent. The pre-digestion and modification effect of nitric acid would be discussed. Palladium was added as a chemical modifier and the temperature program of ETAAS was changed in order to improve the recovery. The slurry was introduced directly into a graphite tube for atomization. The metal content in the sample was determined by the standard addition method. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling method. It offers a quick and efficient alternative method for heavy metal characterization in fine particulates.     

Determination of lead in fine particulates by slurry sampling electrothermal atomic absorption spectrometry

A simple method for determining lead in fine particulates (PM_2.5) by using electrothermal atomic absorption spectrometry (ETAAS) has been developed. Particulates collected on Nuclepore filter by using a dichotomous sampler were suspended in diluted nitric acid after ultrasonic agitation. The dislodging efficiency is nearly 100% after agitation for 5 min. In order to study the suspension behavior of PM_2.5 in solvents, a Brookhaven ZetaPlus Particle Size Analyzer was used to determine the particle size distribution and suspension behavior of air particulates in the solvent. The pre-digestion and modification effect of nitric acid would be discussed. Palladium was added as a chemical modifier and the temperature program of ETAAS was changed in order to improve the recovery. The slurry was introduced directly into a graphite tube for atomization. The metal content in the sample was determined by the standard addition method. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling method. It offers a quick and efficient alternative method for heavy metal characterization in fine particulates. Received: 2 August 2000 / Revised: 25 October 2000 / Accepted: 28 October 2000     

Rapid determination of lead in steel by flameless atomic absorption spectrometry

A method for the determination of 1–100 p.p.m. of lead in high- and low-alloy steels by flameless atomic absorption is described. The sample was dissolved in aqua regia. and 2 μl of the diluted solution were pipetted into a Massmann-type furnace. Ashing of the sample at 625°C eliminated influences from hydrochloric acid. Fe, Cr and Ni gave similar negative interferences, which were compensated for by using low-alloy steel with standard additions. An interlaboratory comparison showed that this method gave the same result as extraction with TOPO in MIBK. The procedure could also be applied to commercial instruments. The time for a complete analysis including dissolution was 15 min.     

Determination of boron in river water with flameless atomic absorption spectrometry (graphite furnace technique)

Summary A simple and rapid procedure is described for the determination of boron in water using flameless atomic absorption spectrometry. A Ca/Mg solution is added before measurement. The method is suitable for boron concentrations up to 250 g/l. The mean standard deviation is 6±4 g/l.

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Bestimmung von Bor in Flußwasser mittels flammenloser Atomabsorptions-Spektrometrie (Graphitrohrtechnik)

Zusammenfassung Eine schnelle und einfache Methode zur Bestimmung von Bor im Wasser mittels flammenloser AAS wird beschrieben. Die Messung erfolgt nach Zugabe einer Ca/Mg-Lösung. Die Methode ist geeignet für Borkonzentrationen bis 250 g/l. Die mittlere Standardabweichung beträgt 6±4 g/l.

     

Determination of manganese in natural waters by flameless atomic absorption spectrometry

Manganese can be rapidly determined in natural waters by direct-injection flameless a.a.s. Interference caused by sea salts in waters of salinity 0–35‰ can be eliminated by charring with ammonium nitrate and with a slow temperature rise. The sensitivity of the determination is depressed by the presence of nitric acid, the depression decreasing with graphite tube age. In saline water matrices, the detection limit is better than 0.002 ng and the sensitivity is better than 0.02 ng for 1% absorbance. Precision is better than 10% for manganese concentrations of 10 μg 1^-1 in sea water.     

Non-spectral interferences in flameless atomic absorption spectrometry using graphite mini-tube furnaces

This work concerns non-spectral interferences occurring in flameless atomic absorption spectrometry using a Varian Techtron CRA model 63 instrument. Special attention has been paid to the influence exerted by concomitants on the vaporization and atomization behaviour of the test elements Be, Mn and Zn. Tracer analysis permitted the direct determination of the vaporization patterns of the test elements during the atomization phase. The variation of the transient absorption signals with time was measured using an electronic recording system sufficiently fast to obtain instrumentally undistorted pulses. The concomitants were selected on the basis of literature dealing with thermochemical processes in are emission spectrometry. Results are discussed on the basis of (i) the decrease of the content of the test element in the furnace, (ii) the characteristics of the absorption signal, and (iii) the surface temperature of the furnace. It turned out that the class “atomization efficiency interferences” might constitute one of the most serious sources of systematic error in frameless atomic absorption spectrometry.     

Determination of sub-nanogram quantities of ruthenium by flameless atomic absorption spectrometry

Flameless atomic absorption spectrometry has been applied to the determination of subnanogram quantities of ruthenium in a variety of matrices encountered in the solidification of nuclear waste. Detection limits ranged to below 10^?10 g, depending on the sample matrix. Most matrix effects could be eliminated by proper selection of atomizer temperature program, allowing the use of a single set of standards in 0.1 N HCl. The one exception was the calcined solid matrix, where a fusion and extraction were used to dissolve the ruthenium and separate it from matrix constituents.     

Determination of lead in geological and biological materials by graphite furnace atomic absorption spectrometry

Summary Serious systematic errors inherent in the determination of lead in geological and biological samples by flameless atomic-absorption spectrometry are demonstrated. The reduced absorption of lead is due to partial interaction with alkaline, alkaline-earth and iron chlorides during the atomization stage. Incomplete dissociation of the volatile monochloride of lead in the gaseous phase reduces the absorption signal. An addition of 20% hydrogen to nitrogen (purge gas) diminishes signal suppression by removing the chlorine in form of volatile HCl. The detection limit is about 0.6 ppm in rocks and about 0.3 ppm in plant materials. Depending on the content in the samples the relative standard deviation is between 1 and 12%. The accuracy of the method was tested on 39 international standard reference samples.

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Bestimmung von Blei in geologischen und biologischen Materialien durch AAS mit der Graphitrohrküvette

Zusammenfassung Schwerwiegende systematische Fehler bei der Bestimmung von Blei in geologischen und biologischen Materialien mit der Graphitrohrküvette werden aufgezeigt. Die Reaktion von Blei mit Alkali-, Erdalkali- und Eisenchloriden während der Atomisierungsphase führt zur Bildung von Bleimonochlorid, das nur unvollständig dissoziiert und eine Signalunterdrückung zur Folge hat. Ein Zusatz von 20% Wasserstoff zu Stickstoff als Spülgas vermindert die Signalunterdrückung, indem überschüssiges Chlor als Chlorwasserstoff entfernt wird. Die Nachweisgrenze liegt bei ca. 0,6 ppm für Gesteine und bei ca. 0,3 ppm für Pflanzenmaterialien. Je nach der Konzentration beträgt die relative Standardabweichung 1–12%. Die Genauigkeit der Methode wurde an 39 internationalen Standardreferenzproben überprüft.

     

Determination of tin and lead in sediment slurries by graphite furnace atomic absorption spectrometry

Methods were determined for lead and tin determinations in river, marine and lake sediments by slurry sampling and graphite furnace atomic absorption spectrometry. The optimizations were carried out using River Sediment BCR 320 and Marine Sediment PACS-2 for Pb and Sn, respectively. For Pb determination, the parameters studied included inorganic acid mixture, stabilizing agent, sample mass and sonication time. The influence of diluents and the extraction to the liquid phase for two different matrices was evaluated for Sn. The Pb content in the slurry liquid phase was ca. 56%, and ranged from 75% to 100% for Sn. Representative masses of 34 and 45 mg, and effective masses of 12 and 48 μg for Pb and Sn, respectively, were obtained under optimized conditions. Detection and quantification limits of 0.2 and 0.7 μg g⁻¹ for Pb, and 1.5–2.6 and 4.5–7.6 μg g⁻¹ for Sn were obtained.

     

The determination of germanium by atomic absorption spectrometry with a graphite tube atomizer

A carbon filament atom reservoir and a graphite tube atomizer are compared as methods for the determination of germanium by atomic absorption spectrometry. It is shown that the filament technique is not applicable, probably because of loss of the sample as a volatile oxide species which results in inefficient atomization. The design of a small graphite tube atomizer is described; with this, a limit of detection for germanium of 3·10^-10 g was found. For a 20-μl sample, this corresponds to a concentration of 0.015 p.p.m. The interfering effect of 13 anions and cations is studied.     

Determination of arsenic by arsine generation with reducing tube followed by graphite furnace atomic absorption spectrometry

Summary A sensitive method for hydride generation and graphite tube furnace atomic absorption spectrometric measurements with a reducing tube has been developed for the determination of arsenic in tea and orchard leaves. Arsines were generated in a horizontal glass tube, in which a pellet of NaBH₄ was placed. 1.5–2.0 l/min of argon flow rate and 2,400° C of atomization temperature were the best experimental conditions. The strong supression of the arsenic signal by Ni and Co was effectively eliminated with 1,10-phenanthroline. A detection limit of 0.3 ng was obtained with a precision of 3–4%.Paper read at the Meeting of the Japan Society for Analytical Chemistry, June 1980     

Determination of selenium by hydride generation with reducing tube followed by graphite furnace atomic absorption spectrometry

Summary Selenium was determined in biological samples (tea and bovine liver, NBS, SRM 1577) by a combination of hydride generation with reducing tube, graphite furnace atomization and atomic absorption detection. The selenium was reduced by a pellet of sodium borohydride which was placed in a horizontal glass tube. 1.6–2.0 l/min of argon flow rate and 2400° C of atomization temperature were the best experimental conditions. Copper produces a severe effect on absorbance, even if present in only 2 times the amounts of selenium. Ion-exchange resin (Dowex 50 W-X8) was used for the separation of Cu, Ni and Co. A detection limit of 1 ng was obtained with a precision of 5–6%.

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Selenbestimmung durch Hydriderzeugung im Reduktionsrohr mit nachfolgender Graphitofen-AAS

Zusammenfassung Durch Kombination von Hydriderzeugung und Graphitofen-AAS wurde Selen in biologischen Proben (Tee, Rinderleber, NBS, SRM 1577) bestimmt. Die Reduktion erfolgte durch Natriumborhydrid in einem horizontalen Glasrohr. 1,6–2,0 l/min Argon und 2400° C Atomisierungstemperatur erwiesen sich als optimal. Kupfer übt selbst bei nur doppelter Menge einen störenden Einfluß aus. Zur Abtrennung von Cu, Ni und Co wurde ein Ionenaustauscher (Dowex 50W-X8) verwendet. Die Nachweisgrenze beträgt 1 ng bei einer Reproduzierbarkeit von 5–6%.

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Paper read at the meeting of 9th ICAS/XXII CSI, Tokyo, September 1981     

Determination of beryllium in soils by means of flameless atomic absorption with zirconium-coated graphite tubes

Summary After the enrichment of beryllium by an extraction of digested soils with acetylacetone/benzene in the presence of EDTA and a subsequent reextraction with nitric acid, this element can be determined by means of flameless atomic absorption without interferences, when zirconiumcoated graphite tubes are used as electrothermal atomizers. In this case the coextracted amounts of aluminium and iron do no interfere. Investigations of interferences were also carried out with non-coated and pyrographite coated tubes. It could be shown that even small amounts of coextracted aluminium interfered remarkably with beryllium. Recovery analyses confirmed that the whole analytical procedure was quantitative. The detection limit of beryllium was found to be 1.5 g/l reextract. As an example, three different types of soil were analyzed: Parabrown soil, Ranker and Peat-bog.

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Bestimmung von Beryllium in Böden mit der flammenlosen Atomabsorption in Zirkonium-beschichteten Graphitrohren

Zusammenfassung Es wird ein Verfahren beschrieben, das es gestattet, Beryllium in Bodenaufschlüssen nach einer Anreicherung durch Extraktion mit Acetylaceton/Benzol und anschließender Reextraktion mit Salpetersäure mit Hilfe der flammenlosen Atomabsorptionstechnik zu bestimmen. Die Analyse verläuft störungsfrei, wenn Zirkonium-beschichtete Graphitrohre als Absorptionsvolumina verwendet werden, trotz der Gegenwart von Aluminium und Eisen, die zum Teil beim Anreicherungsverfahren mitextrahiert werden. Störversuche wurden auch mit unbeschichteten und Pyrographit-beschichteten Rohren durchgeführt. Dabei zeigte sich, daß in diesem Fall auch geringe Mengen an Aluminium die Analyse von Beryllium stark beeinflußten. Wiederfindungsversuche bestätigten den quantitativen Verlauf des gesamten analytischen Verfahrens. Als Nachweisgrenze für Beryllium wurde eine Konzentration von 1,5 g/l Reextrakt ermittelt. Als Beispiel wurden drei unterschiedliche Bodenarten mit der oben erwähnten Methode analysiert: Parabraunerde, Ranker und Hochmoortorf.