Determination of trace levels of boron in graphite powder by inductively coupled plasma-optical emission spectrometry (ICP-OES)

Abstract

A method has been developed for the determination of traces of boron in graphite powder. The graphite powder was made into a paste using Na 2 CO 3 solution (flux). The paste form of graphite powder was fused in a muffle furnace and was mixed in a glycerol solution. The flux was separated from the glycerol solution as a solid residue by heating over a water bath. The boron present in the glycerol solution was measured by ICP-OES. Compared to conventional Na 2 CO 3 fusion, the amount of flux and fusion time were reduced by a factor of 32 and 8, respectively. Due to the extraction of boron from the flux into glycerol solution, the preconcentration was increased by a factor of 200. The separation of flux was >92% with the recovery of analyte in the range of 92-96%. The detection limit was found to be 90 ng g À1 .

Development of Oxidative Pyrolysis Method for the Rapid Determination of Boron in Graphite Powders by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES)

“…For validation purposes, a recently reported sodium carbonate fusion method was adopted without any further modifications (31). Approximately 0.5 g of graphite powder and 2.5 mL of 10% Na 2 CO 3 were added to a nickel crucible.…”

“…Hence, highpurity graphite for nuclear purposes (i.e., nuclear-grade graphite) necessitates a strict control of boron whose specification limit has been set as 5 µg g -1 (10). The Department of Customs and Central Excise, Government of India, mandates that any graphite consignment that is nation of boron in refractory materials including graphite (28)(29)(30)(31). However, due to the large quantities of flux employed in decomposing the sample, blanks are significantly increased, which limits its limits of detection (LODs).…”

“…The resulting high salt content also poses problems, especially when the sample is to be introduced into ICP-based techniques, leading to non-spectroscopic interferences. More recently, Thangavel et al (31) reported an alkali fusion method using Na 2 CO 3 solution, followed by glycerol extraction, for the determination of boron in graphite powders with a detection limit of 0.09 µg g -1 . Although this method is suitable for boron determination in nuclear-grade graphite, a large number of steps and long sample preparation time (~3 h per sample) limit its application for routine analysis.…”

AMS with light nuclei at small accelerators

“…From here comes the forensic attribute of this element and the need of methods to measure low limits of boron in graphite. The best detection limit reached until now is in the range of tens of ng/g [7,8]. Our paper presents how AMS is able to push the detection limit to much lower values than all other methods before.…”

Resonance light scattering detection of uranium based on its reaction with a Schiff base containing tetradentate ligand and phosphate groups to form supramolecular polymer

“…At present, several analytical methods have been used for the detection of uranium, such as atomic emission spectrometry [1], gamma ray absorption [2], neutron activation analysis [3], inductively coupled plasma-mass spectrometry [4], fission track registration technique [5], and surface-enhanced Raman spectroscopy [6]. However, these methods need expensive equipments and high running cost, resulting in the unsuitability for the routine analysis.…”