Evaluation of Inductively Coupled Plasma Mass Spectrometry for Determining Ca, Cu, Fe, Mg, Mn, Se and Zn in Bovine Semen Samples using a Simple Sample Dilution Method

A simple and fast method for the determination of Ca, Cu, Fe, Mg, Mn, Se and Zn in bovine semen by quadrupole inductively coupled plasma spectrometry (q-ICP-MS) is described. Prior to analysis, samples (200 mu L) were diluted 1:50 in a solution containing 0.01% v/v Triton (R) X-100 and 0.5% v/v nitric acid and directly analyzed by ICP-MS. The limits of detection of the method are 0.3, 0.03, 0.2, 0.04, 0.04, 0.03 and 0.03 mu g L-1 for Ca-44, Cu-63, Fe-57, Mg-24, Zn-64, Se-82 and Mn-55, respectively. For purposes of comparison and method validation, four ordinary bovine semen samples were directly analyzed by ICP-MS and by flame atomic absorption spectrometry (FAAS) or graphite furnace atomic absorption spectrometry (GF AAS), with no statistical difference between the techniques at the 95% level when applying the t-test. Then, the proposed method was applied in the determinations of Ca, Cu, Fe, Mg, Mn, Se and Zn in collected samples of bovine semen from different breeds, which are used in reproduction programs and artificial insemination.

Evaluation of inductively coupled plasma mass spectrometry for determining Ca, Cu, Fe, Mg, Mn, Se and Zn in bovine semen samples using a simple sample dilution method

A simple and fast method for the determination of Ca, Cu, Fe, Mg, Mn, Se and Zn in bovine semen by quadrupole inductively coupled plasma spectrometry (q-ICP-MS) is described. Prior to analysis, samples (200 µL) were diluted 1:50 in a solution containing 0.01% v/v Triton® X-100 and 0.5% v/v nitric acid and directly analyzed by ICP-MS. The limits of detection of the method are 0.3, 0.03, 0.2, 0.04, 0.04, 0.03 and 0.03 µg L-1 for 44Ca, 63Cu, 57Fe, 24Mg, 64Zn, 82Se and 55Mn, respectively. For purposes of comparison and method validation, four ordinary bovine semen samples were directly analyzed by ICP-MS and by flame atomic absorption spectrometry (FAAS) or graphite furnace atomic absorption spectrometry (GF AAS), with no statistical difference between the techniques at the 95% level when applying the t-test. Then, the proposed method was applied in the determinations of Ca, Cu, Fe, Mg, Mn, Se and Zn in collected samples of bovine semen from different breeds, which are used in reproduction programs and artificial insemination.

Fluorcalciomicrolite, (Ca,Na,□)2Ta2O6F, a new microlite-group mineral from Volta Grande pegmatite, Nazareno, Minas Gerais, Brazil

Fluorcalciomicrolite, (Ca,Na,□)2Ta2O6F, is a new microlite-group, pyrochlore supergroup mineral approved by the CNMNC (IMA 2012-036). It occurs as an accessory mineral in the Volta Grande pegmatite, Nazareno, Minas Gerais, Brazil. Associated minerals include: microcline, albite, quartz, muscovite, spodumene, "lepidolite", cassiterite, tantalite-(Mn), monazite-(Ce), fluorite, "apatite", beryl, "garnet", epidote, magnetite, gahnite, zircon, "tourmaline", bityite, hydrokenomicrolite, and other microlite-group minerals under study. Fluorcalciomicrolite occurs as euhedral, untwinned, octahedral crystals 0.1-1.5 mm in size, occasionally modified by rhombododecahedral faces. The crystals are colourless and translucent; the streak is white, and the lustre is adamantine to resinous. It does not fluoresce under ultraviolet light. Mohs' hardness is 4½- 5, tenacity is brittle. Cleavage is not observed; fracture is conchoidal. The calculated density is 6.160 g/cm3. The mineral is isotropic, ncalc. = 1.992. The Raman spectrum is dominated by bands of B-X octahedral bond stretching and X-B-X bending modes.The chemical composition (n = 6) is (by wavelength dispersive spectroscopy, H2O calculated to obtain charge balance, wt.%): Na2O 4.68, CaO 11.24, MnO 0.01, SrO 0.04, BaO 0.02, SnO2 0.63, UO2 0.02, Nb2O5 3.47, Ta2O5 76.02, F 2.80, H2O 0.48, O=F -1.18, total 98.23. The empirical formula, based on 2 cations at the B site, is (Ca1.07Na0.81□0.12)∑2.00(Ta1.84Nb0.14Sn0.02)∑2.00 [O5.93(OH)0.07]6.00[F0.79(OH)0.21]. The strongest eight X-ray powder-diffraction lines [d in Å(I)(hkl)] are: 5.997(59)(111), 3.138(83)(311), 3.005(100)(222), 2.602(29)(400), 2.004(23)(511), 1.841(23)(440), 1.589(25)(533), and 1.504(24)(444). The crystal structure refinement (R1 = 0.0132) gave the following data: cubic, Fd3m, a = 10.4191(6) Å, V = 1131.07(11) Å3, Z = 8.