Determination of silicon in fine gold by solution and solid sample graphite furnace atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry

1994 ◽  
Vol 9 (3) ◽  
pp. 451 ◽  
Author(s):  
Michael W. Hinds ◽  
Valentina V. Kogan
Keyword(s):  
Inductively Coupled Plasma ◽  
Graphite Furnace ◽  
Absorption Spectrometry ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Graphite Furnace Atomic Absorption ◽  
Fine Gold

scholarly journals Determination of Calcium by Inductively Coupled Plasma-Atomic Emission Spectrometry, and Lead by Graphite Furnace Atomic Absorption Spectrometry, in Calcium Supplements after Microwave Dissolution or Dry-Ash Digestion: Method Trial

1998 ◽  
Vol 81 (6) ◽  
pp. 1233-1239 ◽  
Author(s):  
Paul H Siitonen ◽  
Harold C Thompson ◽  
Keyword(s):  
Inductively Coupled Plasma ◽  
Method Development ◽  
Graphite Furnace ◽  
Absorption Spectrometry ◽  
Atomic Emission ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Microwave Dissolution

Abstract A 3-laboratory method trial was conducted to evaluate 2 sample digestion procedures and instrumental determination parameters for analysis of calcium and lead in Ca supplements. Calcium supplements were treated by dry-ash digestion or microwave dissolution prior to spectrometric analysis. In each case, Pb was determined by graphite furnace atomic absorption spectrometry and Ca by inductively coupled plasma-atomic emission spectrometry. Blind duplicates of 6 Ca supplement samples were analyzed after each sample treatment procedure. Matrix pairs contained dissimilar Pb levels to cover the analyte range encountered during method development. Calcium content of the Ca supplement samples also reflected the range seen during method development. Stock solutions of Ca and Pb were supplied to collaborators for preparation of quantitation standards to remove a variable external to the method. National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1486, bone meal, was included to assess method accuracy and recovery at NIST certificate Ca and Pb levels for this material (26.58 ± 0.24% Ca and 1.335 ± 0.014 µg Pb/g). Analyses of the NIST SRM yielded 25.9 ± 1.1 and 27.2 ± 2.3% Ca and 1.53 ± 0.19 and 1.26 ± 0.19 µg Pb/g for dryash and microwave procedures, respectively. Statistical analyses of data indicated acceptable repeatability and reproducibility for determination of Pb and Ca in various Ca supplements. With either sample preparation technique, the method Received August 27, 1997. Accepted by JS July 2,1998. is appropriate for determining Pb or Ca in Ca supplements.

Analysis of Calcium and Lead in Calcium Supplements by Inductively Coupled Plasma-Atomic Emission Spectrometry and Graphite Furnace Atomic Absorption Spectrophotometry

1994 ◽  
Vol 77 (5) ◽  
pp. 1299-1304 ◽  
Author(s):  
Paul H Shtonen ◽  
Harold C Thompson
Keyword(s):  
Inductively Coupled Plasma ◽  
Graphite Furnace ◽  
Atomic Emission ◽  
Atomic Emission Spectrometry ◽  
Emission Spectrometry ◽  
Plasma Atomic Emission ◽  
Plasma Atomic Emission Spectrometry ◽  
Inductively Coupled ◽  
Relative Standard ◽  
Graphite Furnace Atomic Absorption

Abstract A method was developed to analyze various calcium supplements for Ca and Pb content. The analysis involves a dry ash of the supplements followed by wet digestion. The Pb is determined by graphite furnace atomic absorption spectro–photometry (GFAAS). Analysis of Ca is by inductively coupled plasma–atomic emission spectrometry (ICP–AES). Ca supplements fortified with Pb at levels ranging from 0.25 to 10.0 μg/g yielded recoveries ranging from 82.7 ± 4.2 to 105.0 ± 1.7%. To test accuracy, the method was applied to National Institute of Standards and Technology standard reference materials (NIST SRMs) 1572 citrus leaves and 1486 bone meal. GFAAS analysis of SRM 1572 averaged 13.1 ± 0.6 μg Pb per g (certificate value, 13.3 ± 2.4 (μg Pb per g), and analysis of SRM 1486 averaged 1.34 ± 0.11 μg Pb per g (certificate value, 1.335 ± 0.014 μg Pb per g). ICP–AES analysis of SRM 1572 averaged 3.12 ± 0.01% Ca (certificate value, 3.15 ± 0.10% Ca by weight), and analysis of SRM 1486 averaged 27.63 ± 0.27% Ca (certificate value, 26.58 ± 0.24% Ca). The method's limit of quantitation (LOQ), on supplement Ca basis and a 1 g sample, averaged 0.75 μg Pb per 1 g Ca for supplements containing 9 to 35% Ca by weight. At a Pb level of 0.663 μg/g Ca, the reproducibility relative standard deviation (RSDr) averaged 7.3% and the repeatability relative standard deviation (RSDr) averaged 8.0%. It is recommended that the method be studied collaboratively.

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