Untersuchung von systematischen Fehlern bei der Bestimmung von Hg-Gesamtgehalten im Bereich &lt; 10−5% in anorganischen und organischen Matrices mit zwei unabhängigen Verbundverfahren

Kaiser, G.; Götz, D.; Tölg, G.; Knapp, Günter; Maichin, B.; Spitzy, H.

doi:10.1007/bf00491943

Cited by 55 publications

(9 citation statements)

References 67 publications

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“…When SnC12 is used as a reductant (in FIAS), it was observed that the efficiency of the cold vapour generation strongly depends on the type of acid present in the solution as well as on its concentration. This is in agreement with conclusions of Kaiser et al [6]. Therefore the influence of nitric acid, hydrochloric acid and a mixture of both acids on the absorbance was investigated for model solutions containing 20 gg/1 Hg(II).…”

Section: Cold Vapour Atomic Absorption Spectrometrysupporting

confidence: 77%

“…As a reducing agent for CV AAS typically SnC12 is used [4]. Kaiser et al [6] compared tin(II) chloride and sodium tetrahydroborate(III) for reduction of organic and inorganic mercury in respect to their tolerance for other elements present in the sample solution. In our investigations, mercury was reduced by SnC1 e solution in the FIAS unit, while in FIMS mercury reduction was performed by NaBH 4 solution.…”

Section: Measurement Proceduresmentioning

confidence: 99%

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Atomic absorption spectrometric determination of mercury in soil standard reference material following microwave sample pretreatment

et al. 1995

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Abstract. Several decomposition procedures and their influence on the determination of mercury by electrothermal (ET) and cold vapour (CV) atomic absorption spectrometry (AAS) have been studied. Soil samples were decomposed by microwave digestion in closed and open vessels as well as by digestion under reflux according to German standard. The use of different acids (HNO 3, HC1 or aqua regia) was evaluated and compared in respect to their influence on the determination of mercury by ET AAS and CV AAS. The digestion solutions were analyzed by ET AAS with a palladium modifier and by CV AAS using SnC12 or NaBH 4, as reducing agents. The detection limits obtained with different procedures were also evaluated. For the soil containing 6.25 gg/g of Hg the ET AAS measurements were possible. In the case of lower concentration of mercury the CV AAS determination following the microwave digestion procedure with HC1 or aqua regia is recommended. The accuracy of the proposed procedure was confirmed by the determination of total mercury in SRM 27l 1 Montana Soil.

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Section: Cold Vapour Atomic Absorption Spectrometrysupporting

confidence: 77%

Section: Measurement Proceduresmentioning

confidence: 99%

Atomic absorption spectrometric determination of mercury in soil standard reference material following microwave sample pretreatment

et al. 1995

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“…Among the determination methods microwave-induced plasma optical emission spectrometry (MIP-OES)40 proved to be extremely sensitive and up to a large extend free of interferences. 41 By its high volatility, Hg already can be separated from inorganic or organic matrices during the intitial decomposition stage in a sealed system by means of oxygen excited in a microwave field, cf. Fig.…”

Section: Special Sectionmentioning

confidence: 99%

Power of Detection and Accuracy in Elemental Trace Analysis

Tölg

Tschöpel

1987

ANAL. SCI.

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“…Die Nachweisgrenze der Bestimmung von Quecksilber im Urin kann gesenkt werden, wenn eine größere Menge Urin eingesetzt wird. Es ist jedoch darauf hinzuweisen, daß die Kontrolle der Kontaminationen, wenn kleinere Mengen als l Mg/1 nachgewiesen werden sollen, oft sehr schwierig und aufwendig ist (10 …”

Section: Einführungunclassified

Zur direkten Bestimmung von Quecksilber im Urin nach der Kaltdampf-Atomabsorptionsspektrometrie-Methode

Oster¹

1981

CCLM

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Zusammenfassung: Durch vergleichende Untersuchungen wird belegt, daß sich die Gesamt-Quecksilberkonzentration in Urin (> 2 Mg/1) kostensparend direkt durch Atomabsorptionsspektrometrie nach der Kaltdampf-Technik zuverlässig bestimmen läßt, wenn das aus der Urinprobe nach Behandlung mit KMnO 4 -Lösung und einem HN0 3 -H 2 SO 4 -Gemisch mit NaBH 4 zu Metalldampf reduzierte Quecksilber abgetrennt und bestimmt wird.Als Vergleichsmethoden dienten die Standardadditionsmethode und ein Verfahren, bei dem die Urinproben noch zusätzlich mit HNO 3 in einem PTFE-Druckgefäß mineralisiert wurden. Beide Methoden zeigten, daß die empfohlene Vorschrift das Gesamtquecksilber erfaßt und durch weitere anorganische und organische Harnbestandteile nicht gestört wird. Die Nachweisgrenze der Methode ergab sich zu 2 Mg/1 Quecksilber (Probenmenge: l ml). Die Variationskoeffizienten lagen bei 7,4% bzw. 4% für aufgestockte Hg-Mengen von 10 bzw. 30 g/L Für nicht exponierte Personen (30 Männer, 30 Frauen) wurde ein "Normal-Wert" von < 4 g/l Quecksilber gefunden. The direct determination of mercury in urine by cold vapor atomic absorption spectroscopySummary: A method is described for the determination of mercury in urine by atomic absorption spectroscopy. The organically bound mercury is oxidized by treatment of the urine with KMnO 4 , followed by dilution with a mixture of HNO 3 and H 2 S0 4 . The sample is then treated with NaBH 4 to release the mercury vapor. This procedure measures total mercury (inorganic and organically bound) in the urine. The method was compared with the standard addition method and with the determination after wet digestion with concentrated HNOa. A good correlation was found between the three methods. Other organic and inorganic compounds present in urine do not interfere. Using 1 ml urine samples, the detection limit is 2 Mg/1 Hg. Sensitivity is also 2 g/l Hg. Urinary mercury in a non-exposed population (30 men, 30 women) was found to be less than 4 Mg/1 Hg.

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Untersuchung von systematischen Fehlern bei der Bestimmung von Hg-Gesamtgehalten im Bereich < 10−5% in anorganischen und organischen Matrices mit zwei unabhängigen Verbundverfahren

Cited by 55 publications

References 67 publications

Atomic absorption spectrometric determination of mercury in soil standard reference material following microwave sample pretreatment

Atomic absorption spectrometric determination of mercury in soil standard reference material following microwave sample pretreatment

Power of Detection and Accuracy in Elemental Trace Analysis

Zur direkten Bestimmung von Quecksilber im Urin nach der Kaltdampf-Atomabsorptionsspektrometrie-Methode

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