Mercury Determination in Certifiable Color Additives Using Thermal Decomposition Amalgamation and Atomic Absorption Spectrometric Analysis

Author(s):  
Kha Phan ◽  
Nicole Richardson ◽  
Nancy M Hepp

Abstract Background Color additives requiring batch certification by the U.S. Food and Drug Administration (FDA) have Code of Federal Regulations (CFR) specification limits for certain elements and are usually analyzed by x-ray fluorescence spectrometry (XRF). However, sensitivity for Hg is too low in some color additives. Objective The thermal decomposition amalgamation-atomic absorption spectrometric (TDA-AAS) technique was investigated for providing quick and accurate determinations of Hg in certifiable color additives. Methods Tests were performed to optimize conditions and test reliability of Hg determinations at and below the CFR specification limit of 1 mg/kg. Results Sensitivity is much improved over XRF with limits of quantitation of 0.03 mg/kg for highly homogeneous color additives. Conclusions The TDA-AAS method can be used for determining Hg concentrations at and below the CFR specification limit. The technique is effective for all color additives, including those that are difficult to analyze by XRF, but less efficient for color additives that quickly deteriorate the catalyst. Regular quality checks using certified reference materials and in-house matrix-matched check standards are essential. Highlights The TDA-AAS method is applicable for use in routine color additive batch certification. Certain matrices (notably those that release nitrogen or sulfur oxides or halogens upon combustion) necessitate more frequent replacement of the catalyst and recalibration, impacting productivity. Color additives containing BaSO4, in color additive lakes, that are difficult to analyze by other techniques are well suited for TDA-AAS analysis.

2010 ◽  
Vol 1 (2) ◽  
pp. 111-119
Author(s):  
Narsito Narsito

In the present work, some fundamental aspects of the formation of gaseous lead hydride from aqueous solutions containing divalent lead ions (Pb2+) and its application in the atomic absorption spectrometric analysis lead has been investigated. By utilizing a peristaltic pump, an acidic solution of Pb2+ was first oxidized with ammonium peroxodisulphate, NH4S2O8, and followed by reduction with sodium tetrahydroborate, NaBH4. After a gas-liquid separation, the gaseous lead hydride produced was directly swept into an electrically heated open ended quartz tube, located at the light path of an atomic absorption spectrometer in order to have possibilities for specific atomic absorption spectroscopic measurements. The absorbance signals caused by lead atomic absorption could be used proportionally to estimate the density of atomic lead vapor produced in the thermal decomposition under investigation. Results showed that on-line pre-oxidation of the analyte is very important and crucial step in the gaseous hydride generation of lead, and no lead hydride was produced without the involvement of this step. Moreover, it was observed that the use of low major gas flows cannot be applied in quantitative atomic absorption spectrometric determination of lead by this technique. This condition may result in possible losses of the analyte atomic vapor due to metallic condensation.


1992 ◽  
Vol 7 (7) ◽  
pp. 1085 ◽  
Author(s):  
V. Carbonell ◽  
A. Morales-Rubio ◽  
A. Salvador ◽  
M. de la Guardia ◽  
J. L. Burguera ◽  
...  

2016 ◽  
Vol 99 (1) ◽  
pp. 273-278 ◽  
Author(s):  
Mustafa Soylak ◽  
Ayse Aydin ◽  
Nebiye Kizil

Abstract A preconcentration/separation system for cadmium(II), nickel(II), copper(II), lead(II), iron(II), cobalt(II), and manganese(II) ions has been established prior to their atomic absorption spectrometric determinations. The procedure is based on the co-precipitation of these ions by the aid of a praseodymium hydroxide (Pr(OH)3) precipitate. The precipitate was dissolved in 0.5 mL of concentrated HNO3, and made up to 10.0 mL with water. The analytes were determined by a flame atomic absorption spectrometer. The effects of analytical parameters including pH, amounts of praseodymium as carrier element, sample volume, etc. on the recoveries of heavy metals were investigated. The effects of matrix ions were also examined. The limits of detection for analyte ions were found in the range between 0.7–5.2 μg/L. The validation of this present procedure was verified by the analysis of certified reference materials, TMDA-54.4 (fortified water) and NIST 1570a (spinach leaves). The proposed co-precipitation procedure was applied for the determination of cadmium(II), nickel(II), copper(II), lead(II), iron(II), cobalt(II), and manganese(II) ions in various environmental water samples.


Sign in / Sign up

Export Citation Format

Share Document