Direct inductively coupled plasma optical emission spectrometry for analysis of waste samarium-cobalt magnets

An analytical procedure for direct determination of Al, Mg, Ti, Cr, Mn, Nb, La, Nd, Eu, Gd, Tb, Dy, Tm, Yb, Lu, Hf, Ni, Cu, Fe, Zr Sm and Co by ICP-OES in waste samarium-cobalt magnets has been developed. The significant influence of the matrix on all determinable components has been shown. The influence of operation parameters (ICP power and nebuliser flow rate) on the matrix effect has been studied using two plasma observation modes (axial and radial). For the first time, the optimal conditions for ICP-OES analysis of waste samarium-cobalt magnets has been substantiated (ICP power 1400 W, nebuliser flow rate 0.5–0.6 L/min). The analytical capabilities of the method have been evaluated using spike recovery test, certified reference materials and comparison with ICP-MS. ICP-OES measurements were performed in the axial mode for trace elements (with concentrations of n·10^?4-n·10^?2 % wt.) and in the radial mode for matrix elements and analytes (with concentrations higher than n·10^?2 % wt.). The limits of quantification (LOQs) were in the range of n·10^?5 wt% for Mn, Zr and Yb and n·10^?4 wt% for Al, Mg, Ti, Cr, Hf, La, Ni, Cu, Tb, Lu, Nb, Fe, Nd, Eu, Gd, Dy and Tm. RSD ranged from 0.2 to 10.6%.     

南极岩石样品中稀土元素的中子活化分析

用仪器中子活化分析技术,测定了南极岩石中8种稀土元素含量,讨论了不同岩石的稀土模式特点。     

Determination of 30 elements in coal and fly ash by thermal and epithermal neutron-activation analysis

Thirty elements are determined in coal and fly ash by instrumental neutron-activation analysis using both thermal and epithermal irradiation. Gamma-ray spectra were recorded 7 and 20 days after the irradiations. The procedure is applicable to the routine analysis of coals and fly ash. Epithermal irradiation was found preferable for the determination of Ni, Zn, As, Se, Br, Rb, Sr, Mo, Sb, Cs, Ba, Sm, Tb, Hf, Ta, W, Th and U, whereas thermal irradiation was best for Sc, Cr, Fe, Co, La, Ce, Nd, Eu, Yb and Lu. Results for SRM 1632 (coal) and SRM 1633 (fly ash) agree with those of other investigators.     

Major,minor and trace element mass fractions determined using ED-XRF,WD-XRF and INAA for five certified clay reference materials: NCS DC 60102–60105; NCS DC 61101 (GBW 03101A, 03102A, 03103, and 03115)

Major, minor and trace element mass fractions were determined using wavelength dispersive and energy dispersive X-ray fluorescence and instrumental neutron activation analysis for five clay certified reference materials (NCS DC 60102–60105, 61101) distributed by the National Research Center for Certified Reference Materials in China. We report mass fractions for 10 major and the following 29 minor and trace elements: As, Ba, Ce, Co, Cr, Cs, Cu, Eu, Hf, La, Lu, Nb, Nd, Ni, Pb, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Th, U, V, Y, Yb, Zn, and Zr.     

Elemental content in ground and soluble/instant coffee

The concentration of thirty-four elements in twelve coffee brands has been measured using instrumental neutron activation analysis. The samples investigated included four brands of commercially available ground coffee and eight brands of soluble/instant coffee. The elements measured were Al, As, Ba, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Gd, Hf, K, La, Lu, Mg, Mn, Na, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, Ti, Tm, U, V, Yb and Zn. Twenty four elements were found to be below the detection limit in one or more samples. These elements were Ce, Cr, Fe, V, As, Eu, Ba, Dy, Gd, Hf, La, Lu, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, Ti, Yb, Tm, and U.     

NAA and ICP analysis of obsidian from Central Europe and the Aegean: Source characterisation and provenance determination

INAA and ICPES are compared for their discriminative power in obsidian source characterisation. Geological samples from the Aegean and Carpathian sources were analysed for Na, Sc, Fe, Co, Rb, Sb, Cs, Ba, La, Ce, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Th, U by INAA and for B, Na, Mg, Al, K, Ca, Sc, Ti, Mn, Fe, Zn, Y, Yr, Cs, Ba, La, Ce, Sm, Eu, Gd, Tb, Yb, Lu, Hf by two ICPES procedures. It is shown that all techniques work successfully, however, INAA is more efficient in the chemical discrimination of neighbouring sources.     

New data on the GSJ reference rocks JB-1a and JG-1a by instrumental neutron activation analysis

Two reference rocks of the Geological Survey of Japan have been analyzed for Na, K, Sc, Cr, Fe, Co, Zn, Rb, Cs, Ba, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu, Hf, Ta, Th and U, using instrumental neutron activation analysis. The results are reported and compared with consensus values proposed in the literature. In general, the agreement is good except for Cs.     

Determination of impurities in titanium and titanium oxide by radiochemical neutron activation analysis

A radiochemical neutron activation analysis has been applied to 2N–4N grade titanium metal and its oxide. Twenty two impurities were separated in a group from scandium by a radiochemical separation method using cation exchange resin with HBr and HCl. The contents of the elements were calculated by a single comparator method using two monitors. The analytical results agree well within 10% deviation with those obtained by instrumental method. Eighteen elements, Na, Fe, Co, As, Se, Sr, Mo, Sb, La, Eu, Tb, Yb, Lu, Hf, Ta, W, Th and U, are determined in titanium oxides and 17 elements, Na, Cr, Fe, Co, Se, As, Zr, Mo, Sb, Cs, Ce, Tb, Yb, Hf, Ta, W and Th, in titanium metals.     

Analysis of a Nd: YAG laser crystal by X-ray fluorescence,scanning electron microscopy and neutron activation analysis

Recently excavated roman amphorae were submitted to instrumental neutron activation analysis for the determination of Ca, Sc, Cr, Fe, Co, Sb, Ba, La, Ce, Eu, Yb, Lu, Hf and Th. Data reduction was carried out by identifying first the elements useful for discrimination purposes and then by submitting the data to cluster analysis. Amphorae are parted in two groups which are related to different provenance areas.     

INAA of Some Fossil Samples from Romanian Sites

Instrumental neutron activation analysis was used to determine elemental contents of Elephas primigenius mammoth mandible bone and Pecten solarium shell fossils discovered in Romania during 1995–1996. In addition, calcareous sedimentary rock surrounding the shell fossil was analyzed. Concentrations of Al, As, Au, Ba, Br, Ca, Co, Cr, Cs, Fe, Hf, K, Mg, Mn, Na, Ni, Rb, Sb, Sc, Se, Sr, Th, U, V, Zn and the rare earth elements Ce, Eu, La, Lu, Nd, Sm, Tb, Yb were determined. The results are discussed and compared to the available data in the literature for similar fossils.     

A Revised Periodic Table: With the Lanthanides Repositioned

The lanthanide elements from lanthanum to lutetium inclusive are incorporated into the body of the periodic table. They are subdivided into three sub-groups according to their important oxidation states: La to Sm, Eu to Tm, Yb and Lu, so that Eu and Yb fall directly below Ba; La, Gd, Lu form a column directly below Y; Ce and Tb fall in a vertical line between Zr and Hf. Pm falls below Tc; both are radioactive, and not naturally occurring. The elements with easily attained 2⁺ and 4⁺ oxidation states are grouped and clearly differentiated. Gadolinium has an important position as the centre of four triads in the block of elements that surround it– La, Gd, Lu; Ba, Gd, Hf; Eu, Gd, Tb; Yb, Gd, Ce. This new arrangement has the advantages of compactness, simplicity and clarity – there are no tie lines; and important oxidation states of these metals are emphasized. The actinides are also accommodated within this system, and element 114 falls naturally below lead in Group 14.     

Multielement analysis of Northwestern Nigerian rocks by instrumental neutron activation analysis

Rock samples from seven different locations in northwestern Nigeria were analyzed by reactor instrumental neutron activation analysis and Ge(Li) gamma-ray spectrometry. Concentration values were obtained for 18 elements (As, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Lu, Sc, Sm, Sr, Ta, Tb, Th, U, Yb). The geochemical implications of the results are discussed.     

Chemical characterization of gas- and oil-bearing shales by instrumental neutron activation analysis

The concentration of As, Ba, Ca, Co, Cr, Cs, Dy, Eu, Fe, Ga, Hf, K, La, Lu, Mn, Mo, Na, Ni, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, U, Yb, and Zn were determined by instrumental neutron activation analysis in block shale samples of the New Albany Group (Devonian-Mississippian) in the in the Illinois Basin. Uranium content of the samples was as high as 75 ppm and interfered in the determination of samarium, molybdenum, barium and cerium. In the determination of selenium a correction was made for interference from tantalum. U, As, Co, Mo, Ni and Sb as well as Cu, V and pyritic sulphur which were determined by other methods, were found to correlate positively with the organic carbon content of the samples.     

Radioanalytical methods for the non-destructive analysis of lunar samples

The elemental compositions of Apollo 11 and Apollo 12 lunar soil samples 10084,141 and 12070,83 and Apollo 12 rock fragment 12063,73 were determined by non-destructive radioanalytical methods. Main mineral fractions and glasses separated from these samples were analyzed as well. Instrumental neutron activation analysis (INAA) was used to determine Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zr, Cs, Ba La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Tm, Yb, Lu, Hf, Ta, W, Ir, Au, Th and U. A method of delayed neutron counting was used for the determination of uranium, and non-dispersive radioisotopic X-ray fluorescence analysis was applied to the determination of Ti, Fe, Sr, Y and Zr.     

Determination of impurities in natural diamonds using neutron activation and high-resolution gamma-spectrometry

Thirty-five natural diamonds from six widely differing localities, weighing from 3.6 mg to 305.3 mg were subjected to instrumental neutron activation analysis using high-resolution semiconductor gamma-spectrometry. By means of short-term and long-term activation in a nuclear reactor, Na, Sc, Cr, Mn, Co, La, Ce, Sm, Eu, Hf, Au, Hg, and Th were determined in all the samples, K, Sr, Ag, Cs, Ba, Yb, Lu and W in some, and qualitative determination was carried out with Ca, Fe, Ni, Ga, As, Zr, Sb, Tb, Dy, Ta, It and U. The study serves as a basis for the study of the relationship between the colour, morphology and luminescence of diamonds and their impurity contents.     

Determination of microelement content in the samples from the cycle of intensive poultry breeding

The results of analysis of 15 samples of meat, eggs, feed and water used in the cycle of intensive poultry breeding are given in the paper. Twenty chemical elements such as: Sm, Lu, Eu, Hf, Ce, Yb, Cr, La, Br, Sb, Cs, Sc, Fe, Co, Na, Ta, Tb, Zr, Rb and Zn have been quantitatively determined in all the samples by nondestructive neutron activation analysis. Qualitative determination of K, Ca, Ru and Au was also performed in some samples.     

Rapid sample digestion by fusion and chemical separation of Hf for isotopic analysis by MC-ICPMS

A new method for rapid sample digestion and efficient chemical separation of Hf and REE from rock samples for precise isotopic analysis is presented. Samples are digested by fusion in the presence of a lithium borate flux at 1100 °C and dissolved whilst molten in dilute nitric or hydrochloric acid. Prior to chemical separation using ion exchange techniques, Li and B from the flux material and Si from the sample are separated from the remaining major elements, REE and high field strength elements (HFSE) in the sample by Fe-hydroxide co-precipitation. The chemical separation of Hf is a two-stage procedure designed to first remove the remaining matrix elements (e.g. Fe, Ba) in the sample using standard cation exchange techniques, followed by separation of Hf from the REE and HFSE on TEVA extraction chromatographic resin. Hf yields are >90% and total procedural blanks are ca. 50 pg. Hf isotope ratios of a synthetic standard solution and replicate digestions of international rock standards BHVO-1 and BCR-1 measured on multi-collector inductively coupled plasma mass spectrometer (MC-ICPMS) reproduce similarly to ≤50 ppm (2 S.D.). The following elemental ratios are routinely obtained for elements, which interfere isobarically or may affect the ionisation and/or fractionation behaviour of Hf during analysis: ¹⁷⁶Yb/¹⁷⁶Hf<0.0001; ¹⁷⁶Lu/¹⁷⁶Hf<0.00001; Ti/Hf<0.05. This technique also provides a means of separating Nd from the REE fraction for isotopic analysis and, potentially, may be adapted for measurement of Lu/Hf ratios by isotope dilution techniques.     

Multitracer study on permeation of rare earth elements through a supported liquid membrane

Separation by means of supported liquid membranes is a useful method for the preparation and preconcentration of radioactive nuclides. The permeation of rare earth elements through a bis(2-ethylhexyl) hydrogen phosphate-decalin membrane supported on a microporous polytetrafluoroethylene sheet was studied using a multitracer containing radioactive nuclides of Sc, Zr, Nb, Hf, Ce, Pm, Gd, Yb, and Lu. Permeation rates of these elements from feed solutions of various acidity to receiving solutions of 0.5 mol·dm⁻³ HCl were determined simultaneously. The feed solution at pH 1.4 gave the highest permeation rate for Ce, Pm, and Gd, amounting to about 95% of permeation for Ce and Pm, 80% for Gd, and 10% for Yb in 21 h. Scandium, Zr, Nb, Hf, and Lu were not transported at all from the feed solution. Permeation rates of Yb and Lu from the feed solution at pH 1.4 to receiving solutions of 0.75, 1.0, 2.3, and 4.0 mol·dm⁻³ HCl increased with the concentration. The results obtained indicate that the light rare earth elements can be separated from the heavy ones by this method.     

The lognormal distribution of trace elements in glacial till

The concentrations of Au, Ce, Cr, Eu, Hf, La, Lu, Sc, Sm, Th, U and Yb were determined by instrumental neutron activation analysis in 1200 samples of glacial till from Quebec by using a SLOWPOKE reactor. All these elements are lognormally distributed in the till which would suggest that their concentrations, while reflecting somewhat the composition of the bedrock, are apparently not regulated about a central value by any geological process.     

The bearing of trace element distribution patterns of deep sea basalts for the interpretation of their genesis

Trace element determinations at 60 samples of Deep Sea Drilling Project Leg 37 from the Mid Atlantic Ridge south of the Azores had been accomplished by instrumental neutron activation analysis. The elements Na, Mn, Fe, Sc, Cr, Co, Rb, Sb, Cs, La, Ce, Nd, Eu, Tb, Dy, Yb, Lu and Hf were determined with satisfying accuracy. The chondritenormalized rare earth distribution patterns showed strong variations within one drill hole. The different REE patterns require a new interpretation for the generation of this part of the oceanic crust. New considerations for the mode of formation of the oceanic basaltic crust are presented.