Simultaneous determination of zirconium and hafnium in solutions by x-ray fluorescence spectrometry

Journal Article · Mon Sep 01 04:00:00 UTC 1980 · Anal. Chem.; (United States)

DOI:https://doi.org/10.1021/ac50061a040· OSTI ID:5012101

Ricci, E

The importance of Zr and Hf in nuclear reactor research and development is well established. A reliable x-ray fluorescence method (XRF) was developed to determine these two elements simultaneously in (0.5-1.0 M H/sub 2/SO/sub 4/) solutions at levels ranging from 0.5 to 200 ppM. Handling of serial samples is enabled by a 90-sample changer and by the simple chemistry involved. Ferric hydroxide is precipitated with ammonia in a test tube. After washing, the Fe(OH)/sub 3/ slurry containing all the Zr(OH)/sub 4/ and Hf(OH)/sub 4/ is transferred to a 6.4 ..mu..m thick Mylar mount where it is quickly dried on a steam bath. These mounts are inexpensive, hold well during drying, and provide a < 1 mg/cm/sup 2/ thick sample for low-scattering measurements. Fluorescence Zr K..cap alpha.. and Hf L..beta../sub 1/ x-rays are excited by a Ag-anode tube (40 kV-14 mA). The method is based on comparison of multileast-squares results from sample and standard spectra. It is reliable and fast and has an accuracy of 5 to 10%, with detection limits of 0.4 ppM for Zr and 1.2 ppM for Hf.

• Research Organization: Oak Ridge National Lab., TN
• DOE Contract Number: W-7405-ENG-26
• OSTI ID: 5012101
• Journal Information: Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 52:11; ISSN ANCHA
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400103* -- Radiometric &amp; Radiochemical Procedures-- (-1987)
ACCURACY
AMMONIA
CHEMICAL ANALYSIS
ELEMENTS
HAFNIUM
HYDRIDES
HYDROGEN COMPOUNDS
HYDROXIDES
INORGANIC ACIDS
IRON COMPOUNDS
IRON HYDROXIDES
METALS
NITROGEN COMPOUNDS
NITROGEN HYDRIDES
NONDESTRUCTIVE ANALYSIS
OXYGEN COMPOUNDS
QUANTITATIVE CHEMICAL ANALYSIS
REFRACTORY METALS
SENSITIVITY
SULFURIC ACID
TRANSITION ELEMENT COMPOUNDS
TRANSITION ELEMENTS
X-RAY EMISSION ANALYSIS
X-RAY FLUORESCENCE ANALYSIS
ZIRCONIUM