Improved Techniques for Isotopic Determination of Boron on Mass Spectrometer

Melton, Charles E.; Gilpatrick, L.O.; Baldock, R.; Healy, Robert M.

doi:10.1021/ac60114a039

Cited by 17 publications

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“…Mass spectrometric techniques based on electron ionization of gaseous boron compounds such as BF3 have been seriously impaired by memory effects resulting from sample material absorption on the surfaces of the inlet system and ion source (8,9). Melton and others (10) reported that BC13 was effective in removing residual BF3 from the glass sample handling system. A number of other gaseous boron-containing materials, including diborane and methyl borate, have been used for the isotopic analysis of boron (11).…”

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“…Tertiary resin bonded amino groups acting as weak anion exchange sites, such as pyridine groups, have been only slightly studied. Silica has been derivatized with /3-(trichlorosilyl)-2-ethylpyridine and the capacity factors of azobenzene dyes and steroids have been investigated (10). Alumina has been used as a support with a bonded phase formed by using 2-(4-pyridyl)-1-(trichlorosilyl)ethane.…”

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Chemical ionization mass spectrometric determination of boron-10 in enriched boron

Cook¹,

Dubiel²,

Hareland³

1985

Anal. Chem.

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A chemical lonlzatlon mass spectrometrlc method for determining ' OB In enrlched boron was developed and Investigated. Boric acld and methanol were reacted to form volatile methyl borate whlch was directly Introduced Into the Ion source of a quadrupole mass spectrometer. Methyl borate was lonlzed by reactlon with methane and methanol Ions. The 'OB content was determlned from the measured lrB/loB ratio by using the (CH30)3BH+ Ion and a mass spectrometer calibration factor based on the Natlonal Bureau of Standards (NBS) SRM 952 boron Isotope standard. The precision of the chemical lonlzatlon mass spectrometrlc method Is comparable to thermionic emlsslon methods. The relatlve standard devlatlon on repilcate samples dld not exceed 0.009% for the 95% enrlched ' OB samples. The analytical results from 96 enriched boron powder samples were compared by using both thermlonlc emisslon and chemlcal ionization mass spectroscopy. The standard error of the dlfference between palred samples was less than 0.097 across the range of 96 samples. The analysls time Is typlcally less than 10 mln per sample.Boron is used extensively in the nuclear power industry as a neutron absorber in nuclear control rods, nuclear shielding, and neutron detecting devices and as a burnable poison in nuclear fuels. The loB isotope with a natural abundance of 19.8 atom % provides this property because of a relatively high thermal neutron capture cross section (3840 b). The isotopic composition of boron can be a critical factor in the design of nuclear shielding, control systems, and neutron detectors. Therefore, it is essential that the ' OB content in boron used in nuclear facilities be known to a high degree of accuracy.Radioanalytical techniques based on both the nuclear transformation of boron nuclei into activated or metastable nuclei and the measurement of the radioactive decay products have been used to determine either loB or "B. Charged particle reactions have been used successfully to distinguish loB and "B in boron by exploiting the reactions 1°B(d, p)llB and "B(p, a)sBe (1, 2). Olivier (3) described a nuclear microprobe method to determine ' OB and "B simultaneously in steel. The coincident measurement of complementary particles in a nuclear transformation, such as the reactions 1°B(d, p)llB and l'B(d, aIQBe, has improved the analytical precision of radioanalytical techniques significantly (4).Neutron absorption and transmission techniques have been applied successfully toward determining loB in boron (5).Indirect techniques provide extremely sensitive methods for the isotopic analysis of boron (6). With these methods, the total boron content must also be known to determine the llB content by difference and, hence, the isotopic composition. A number of other analytical techniques, such as atomic absorption, emission, and nuclear magnetic resonance specPresent address: Sandia National Laboratories, P.O. Box 5800, Albuquerque, NM 87185. troscopy (7), have been applied on a limited basis to the isotopic analysis of boron.Mass spectrometric te...

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Chemical ionization mass spectrometric determination of boron-10 in enriched boron

Cook¹,

Dubiel²,

Hareland³

1985

Anal. Chem.

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“…O sinal de m/z 87 depois do fluxo de 100'-µmolfL NaBF 4 seguido por três procedimentos de limpeza +l~mmol/L manitol, o 0,25 % Triton X~l:-00 em-metanol, À ·metanol.Embora alguns autores relacionem a ação supressora do manitol sobre o boro COll) a formação de um complexo[59,601 No caso do electrospray, a retenção do efeito de memória de ·íon BF 4 não ocorre necessariamente pela formação de um complexo, mas pela deposição de 4ma camada sólida do manitol sobre o resíduo de boro no contra-eletrodo.Capítulo 4-Mecliclas Is0t-ópicas·-para--B-ore-p0r ES~MS 80 Para certificar se que o efeito de memória é provocado por deposição de material sólido sobre o contra-eletrodo, o mesmo experimento foi conduzido usando uma solução de cloreto e sulfato. A Figura 4.6a mostra as intensidades dos íons cloreto (m/z 35) e bissulfato (m/z 97) obtidas durante a injeção de uma solução de 100-µmol/L de cloreto e sulfato em metanol:água (50+50).…”

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Introdução da técnica de espectrometria de massas com ionização por electrospray para determinação da razão isotópica baseada em complexos de carga simples com ligantes monoisotópicos. Uma nova alternativa para Boro e metais de transição

Moraes¹

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Molecular ion beam method of isotopic analysis: Effect of error propagation, a case study with Li₂BO

Datta

Khodade

Parab

et al. 1993

Rapid Comm Mass Spectrometry

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The isotopic analysis of boron has been carried out using dflerent pairs of isotopic Li2BO: ions as monitors. The precision of the mass spectrometric measurements of different molecular abundance ratios is roughly the same. However, the values of the '%/"B abundance ratio calculated from the experimental ratios of different pairs of isotopic molecular ions show large variations. These variations are shown to be a logical consequence of the calculation step which leads to the magnification of measurement errors to different extents for different peak ratios. Similar arguments would apply for the isotopic analysis of any element employing the molecular ion beam technique. The effect of isotopic fractionation on the molecular abundances is also discussed. The important implication of the present investigation is that it sets the guidelines for selecting suitable monitor molecules to avoid such errors.Molecular ion beams are sometimes employed for the isotopic analysis of elements. ' -12 The related analytical procedure is, by and large, comparable to the conventional atomic ion beam method of isotopic analysis. However, the molecular ion beam method involves (barring those cases where all other constituents of the chosen molecule except the element of interest are monoisotopic) calculations of elemental isotopic abundance ratio(s) from the experimentally measured molecular ion ratio(s) using known isotopic abundance values of the other constituent elements. The central theme of this paper is to pay attention to this calculation step. This is because the calculation process may either enhance or even reduce the error in isotopic analysis due to error propagation, as indicated in Ref.12 which dealt with the determination of the 6Li/7Li abundance ratio using the Li2B02 molecule with all constituent isotopes at their natural isotopic abundance. It was demonstrated" that the precision of the measurements of the intensity ratio of the most abundant Li,BO: ions (mlz 56 and 57) is better than 0.1% , while the uncertainty in the value determined for the 6Li/7Li abundance ratio is 0.3%. The present work involves the isotopic analysis of a "B-enriched isotopic reference material of boron, SRM-952. This was chosen with a view to examining whether the selection of the most abundant Li,BO: ions as monitors also ensures accurate isotopic analysis of a constituent element whose isotopic abundance ratios are quite different from the natural ratios. This paper presents the loB/'lB abundance ratios determined using the experimental intensity ratios of different pairs of isotopic molecular ions and discusses the differences in the results so obtained. EXPERIMENTALThe instrument used is a thermal ionization mass spectrometer, model 261 (Finnigan MAT, Bremen, Germany), upgraded for simultaneous collection of separated ion beams.Author to whom correspondence should be addressed.The lithium sample used for this work was Li2C03, a natural isotopic standard of lithium Svec with certified 6Li/7Li abundance ratio of 0.0832 k 0.0002. l3 The ...

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Improved Techniques for Isotopic Determination of Boron on Mass Spectrometer

Cited by 17 publications

References 6 publications

Chemical ionization mass spectrometric determination of boron-10 in enriched boron

Chemical ionization mass spectrometric determination of boron-10 in enriched boron

Introdução da técnica de espectrometria de massas com ionização por electrospray para determinação da razão isotópica baseada em complexos de carga simples com ligantes monoisotópicos. Uma nova alternativa para Boro e metais de transição

Molecular ion beam method of isotopic analysis: Effect of error propagation, a case study with Li₂BO

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Improved Techniques for Isotopic Determination of Boron on Mass Spectrometer

Cited by 17 publications

References 6 publications

Chemical ionization mass spectrometric determination of boron-10 in enriched boron

Chemical ionization mass spectrometric determination of boron-10 in enriched boron

Introdução da técnica de espectrometria de massas com ionização por electrospray para determinação da razão isotópica baseada em complexos de carga simples com ligantes monoisotópicos. Uma nova alternativa para Boro e metais de transição

Molecular ion beam method of isotopic analysis: Effect of error propagation, a case study with Li2BO

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Molecular ion beam method of isotopic analysis: Effect of error propagation, a case study with Li₂BO