Quantitative determination of chlorine by glow discharge quadrupole mass spectrometry in Zr–2.5Nb alloys

Abstract

Direct determination of chlorine in Zr-2.5Nb alloys down to parts per billion levels has been carried out by use of a glow discharge quadrupole mass spectrometer (GD-QMS). The 35 Cl isotope was used for quantification. The relative sensitivity factor (RSF) for chlorine in zirconium matrix (with a 35 Cl isotope) was determined using a zirconium matrix standard disc of known concentration of chlorine (155 ¡ 5 mg kg 21 ) determined by turbidimetry. The concentrations of chlorine obtained using GD-QMS and by pyrohydrolysis-ion chromatography showed a good agreement, indicating the validity of the RSF value determined. Under optimised conditions the detection limit for chlorine (for 20 ms integration time and 140 points) was found to be 22 mg kg 21 and the internal precision for the measurements was typically 1% RSD for mg kg 21 levels and 10% RSD for mg kg 21 levels. Determination of chlorine above 3 mg kg 21 can also be done using the 37 Cl isotope. However, below 3 mg kg 21 the interference due to the molecular ion, 36 Ar 1 H 1 , starts dominating on the 37 Cl ion signal.

Determination of boron in Zr–Nb alloys by glow discharge quadrupole mass spectrometry

“…The discharge voltage at 1.2 kV resulted in a maximum ion intensity at constant discharge current of 3.0 mA for both matrices (6 · 10 5 ions s À1 for 90 Zr + ion for Zr matrix and 3 · 10 5 ions s À1 for 56 Fe + ion for Fe matrix samples). Earlier it was also observed that the same discharge parameters resulted in sufficient signal intensity for chlorine present at ultra-trace levels along with high signal intensity for zirconium in Zr-2.5%Nb alloys [9]. Our experiments on other Zr-based samples (metals, Zircaloys) also showed that the same discharge parameters resulted in maximum matrix intensity along with sufficient signal for boron.…”

“…Hence the minimum 40 min of pre-sputter time was required to obtain a stable signal for boron determination using GD-QMS technique. In our earlier work [9] for chlorine in zirconium matrix, minimum 50 min of pre-sputter time was found to be essential. In general, elements of higher concentration require less pre-sputter time (20-30 min) only.…”

“…The parameters such as operating mode, use of detectors and mass calibration of GD-QMS are same as those described in detail in our earlier paper [9]. The dual detector system (Model No.…”

Optimization of a fast INAA method for determination of trace concentrations of chlorine in zirconium based alloy and oxide samples

“…PH-IC has been used for the determination of chlorine in nuclear fuels and various material like aluminum foil, Whatman filter paper, surgical gloves, methanol and tetrachloroethelene that were used during fuel fabrication process [4,5]. Chlorine was determined in nuclear fuel by pyrohydrolysis coupled with spectrophotometry [6], while glow discharge mass spectrometry has been used to measure chlorine in Zr-2.5Nb alloys [7].…”

Determination of trace impurities of chlorine in zirconium-alloy matrices using neutron activation technique

“…# Present address: Physics Department, Faculty of Science, The M.S. University of Baroda, Vadodara -390002, India (DPCSV) [7], glow discharge quadruple mass spectrometry (GD-QMS) [8,9], spark source mass spectrometry (SSMS) [10], low-energy deuteron activation analysis and neutron activation analysis [11,12]. Among these, the turbidimetric method [3] is one of the classical methods and is used for the estimation of chlorine concentration in the range of 20-200 µg/g.…”