Use of microwave induced plasma spectrometry as detector for the determination of O, N and H traces after carrier gas hot extraction

Abstract

The determination of O, N and H using a microwave induced plasma coupled to carrier gas hot extraction was exploratory investigated. The signal intensities versus time of blanks and calibration materials were recorded. To check for interferences the signal intensities versus wavelength were recorded at the times just before increase and at the maximum of the time dependent analytical signal. O, N and H were investigated at their prominent wavelengths of 777 nm, 174 nm and 486 nm, respectively. Calibration was performed for O, N and H in the ranges of 0-27 mg, 35-1000 mg and 3-43 mg respectively. For concentration values in the middle of the linear part of the investigated calibration interval, a relative precision of 5% at 13 mg, 2% at 74 mg and 0.6% at 23 mg for O, N and H respectively was found. The maximum matrix load to the plasma used was found to be 150 mg min À1 . From the signal to noise ratio and the sensitivity obtained, instrumental limits of detection (3s) of 0.01 mg for O, 1 mg for N and 0.1 mg for H were found. Assuming a typical sample mass of 1 g this corresponds to relative LODs of 0.01 mg g À1 , 1 mg g À1 and 0.1 mg g À1 for O, N and H respectively.

Analysis of gaseous reaction products of wet chemical silicon etching by conventional direct current glow discharge optical emission spectrometry (DC-GD-OES)

“…6 In combination with optical emission or mass spectrometry, most often microwave induced plasmas (MIP) or capacitive coupled microwave plasmas (CMP) are used, if elemental analysis of gases is needed. 7 More recently, MIP spectrometry was used in combination with carrier gas hot extraction for the determination of traces of O, N and H. 8 Even if until now mainly used for fundamental research, microwave boosted glow discharge lamps may have also an application in the analysis of gases in future. 9,10 Electron impact, b-rays, corona discharges, thermospray and chemical ionisation are other possible excitation and ionisation steps.…”

On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis

“…By nature, most non-metallic impurities cannot be measured after dissolution. CGHE, in particular, can be applied here and is constantly being developed further [22,[32][33][34].…”

Atomic Spectroscopy: A Review

“…With the system, determinations in wastewater and in digested biological standard reference materials under the use of a calibration by standard addition were possible (102). MIPs remain interesting sources for the determination of gases in metals after applying carrier gas hot extraction (103). MIP-AES and MS remain appropriate sources for element-specific detection subsequent to gas-chromatographic separations of volatile element compounds, as shown for the speciation of butyl-and phenyltin compounds in human urine by headspace solid-phase microextraction after derivatization with tetraethylborate and separation by capillary gas chromatography (104).…”

“…Channel flow fluctuations were observed by the authors notably after initiation of the fractionation procedure. Their impact on quantification was considered using 103 Rh as internal reference; intensity ratios measured for various elements and Rh were calculated for each data point. These ratios were found to be independent of the metal concentration, and total sample solution flow was introduced into the nebulizer within a range of 0.4-1.2 mL min -1 .…”