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.     

Microwave digestion-ICP-MS for elemental analysis in ambient airborne fine particulate matter: rare earth elements and validation using a filter borne fine particle certified reference material

NIST standard reference material SRM 2783 was employed to validate a high temperature, high pressure, two-stage microwave assisted acid digestion procedure using HNO₃, HF and H₃BO₃ developed for the analysis of trace elements (including rare earths) in atmospheric fine particulate matter (PM_2.5) prior to inductively coupled plasma mass spectrometry (ICP-MS). This method quantitatively solubilized Na, Mg, Al, K, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sb, Cd, Cs, Ba, Pb, Th, U and several rare earth elements (REEs) (La, Ce, Pr, Nd, Gd, Dy, Er, Sm and Eu) from SRM 1648 and SRM 2783. A small amount of HF in the first stage was required to dissolve silicates necessitating the corresponding addition of H₃BO₃ in second stage to dissolve fluoride precipitates of Mg, La, Ce and Th. The optimized microwave dissolution—ICP-MS method detected Na, Mg, Al, K, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Cd, Mo, Sb, Cs, Ba, La, Ce, Pr, Nd, Sm, Gd, Pb, Th and U at trace to ultra-trace levels in ambient airborne fine particles from three sites in North Carolina. La to light lanthanide signature ratios suggested that soil and motor vehicles are the dominant REE sources in SRM 2783 and PM_2.5 samples collected during this study.     

La0.5R0.5Ba2Cu3O7,Pr0.5R0.5Ba2Cu3O7以及RBa2Cu3o7（R=稀土）的键共价性计

使用复杂晶体化学键理论计算了Ｌａ０．５Ｒ０．５Ｂａ２Ｃｕ３Ｏ７（Ｒ＝Ｐｒ,Ｎｄ,Ｓｍ,Ｅｕ,Ｇｄ,Ｄｙ,Ｙ,Ｈｏ,Ｅｒ,Ｔｍ,Ｙｂ,Ｌｕ）（Ｌａ－Ｒ１２３）,Ｐｒ０．５Ｒ０．５Ｂａ２Ｃｕ３Ｏ７（Ｒ＝Ｌａ,Ｎｄ,Ｓｍ,Ｅｕ,Ｇｄ,Ｄｙ,Ｈｏ,Ｙ,Ｅｒ,Ｔｍ,Ｙｂ,Ｌｕ）（Ｐｒ－Ｒ１２３）以及ＲＢａ２Ｃｕ３Ｏ７（Ｒ＝Ｌａ,Ｐｒ,Ｎｄ,Ｓｍ,Ｅｕ,Ｇｄ,Ｄｙ,Ｈｏ,Ｙ,Ｅｒ,Ｔｍ）（Ｒ１２３）中Ｃｕ－Ｏ键的键共价性,结果表明Ｐｒ－Ｒ１２３,Ｌａ－Ｒ１２３,以及Ｒ１２３都应具有超导性,而实验结果是Ｌａ０．５Ｐｒ０．５Ｂａ２Ｃｕ０７,Ｒ０．５,Ｐｒ０．５Ｂａ２Ｃｕ３Ｏ７（Ｒ＝Ｌａ,Ｎｄ,Ｓｍ,Ｅｕ,Ｇｄ）无超导性,产生这种矛盾的原因尚不明确,需要做进一步的研究。     

Analysis of molybdenum oxide by inductively coupled plasma atomic emission and mass spectrometry

Procedures for the analysis of molybdenum oxide by of inductively coupled plasma atomic emission spectroscopy (ICP-AES) and mass spectrometry (ICP-MS) are proposed on the basis of preliminary extraction separation of molybdenum from impurity elements. To separate 39 impurity elements (Li, Be, Na, Mg, Al, K, Ca, Sc, Ti, Cr, Mn, Fe, Co, Ni, Zn, Ga, Rb, Sr, Y, Cd, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Pb, Bi, Th, and U), the extraction of molybdenum from hydrochloric acid solutions using 5-n-pentylthio-8-hydroxyquinoline was used. The capacities of both methods ICP-AES and ICP-MS in the analysis of molybdenum oxide analysis were examined without the removal of the matrix and after the extraction separation of molybdenum.     

Multielement standards in routine reactor neutron activation analysis

The application of multielement standards (MES) in routine neutron activation analysis brings a whole range of advantages. This paper deals with the experience obtained during many years of application of these MES. Nine of these MES contain a total of 50 elements in suitable combinations and concentrations; thus, the determination of most of the common elements by NAA can be carried out simultaneously. This refers to the following elements: Na, Mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Br, Rb, Sr, Mo, Ag, Cd, In, Sb, Te, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, W, Re, Au, Hg, Th and U. For the determination of the remaining elements such as Zr, Ta, Ir etc., single element standards (SES) are used.     

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.     

Strategy for water analysis using ICP-MS

The developed strategy permits determination in three steps of sixty-seven elements using inductively coupled plasma mass spectrometry (ICP-MS). Sodium, Mg, Si, S, Cl, K, and Ca are determined in a first step; B, Al, P, Cr, Fe, Mn, Ni, Cu, Zn, As, Se, Ag, Cd, Sb, Ba, Hg, and Pb are determined in a second step; and Li, Be, Ti, V, Co, Ga, Ge, Br, Rb, Sr, Y, Zr, Nb, Mo, Sn, Te, I, Cs, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Pt, Au, Tl, Bi, Th, and U are analyzed in a third step. The figures of merit obtained are adequate to carry out water quality monitoring and other hydrochemical studies, such those based in the application of hydrochemical fingerprinting to water management.     

Determination of elements in SRM soil 2709a by neutron activation analysis

A combination of instrumental neutron activation analysis (INAA) and prompt gamma-ray activation analysis (PGAA) was used to value assign 35 elements in SRM soil 2709a (San Joaquin Soil). INAA with counting of short-lived radioisotopes was used for determination of Al, Au, Ca, Dy, K, Mg, Mn, Na, Ti, and V. Elements determined by INAA with counting of intermediate and long-lived radioisotopes included As, Ba, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Lu, Nd, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Yb, Zn, and Zr. Thermal neutron PGAA was used for the determination of H, B, Si, K, Ti, Mn, Fe, Cd and Gd. Expanded uncertainties were determined for all values reported.     

Crystal structure of novel R3Fe(Co,Ni)0.5SnS7 (R = Y,La, Ce,Pr, Nd,Sm, Gd,Tb, Dy and Ho) compounds

Structural Chemistry - The crystal structures of quaternary R3Fe0.5SnS7, R3Co0.5SnS7 and R3Ni0.5SnS7 (R = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy and Ho) compounds of La3Mn0.5SiS7 structure type (space...     

Comparison of digestion methods for ICP-MS determination of trace elements in fish tissues

A comparison is presented of six methods involving nitric acid in conjunction with other reagents to digest three certified marine biological samples (DOLT-3, DORM-3, IAEA-407) and a fish bone homogenate (prepared from Merluccius australis). An inductively coupled plasma-mass spectrometer with an octopole collision cell was used to determine up to 40 elements (Li, B, Na, Mg, Al, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Y, Ag, Cd, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb, Lu, Pb, Th, U) in the digests. These results were assessed in terms of their accuracy and precision, and a flow chart was developed to aid the selection of the optimal digestion method. Although none of the methods was found to give accurate determinations for all elements in the different reference materials, a relatively simple method involving nitric acid and hydrogen peroxide heated in a domestic microwave oven gave the most acceptable results.     

Determination of elemental levels in radiopharmaceuticals by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) was applied to thedetermination of the concentration levels of Na, Mg, Al, Cl, K, Sc, Ti, V,Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Zr, Mo, Ag, Cd, Sb, I, Cs,Ba, La, Ce, Nd, Sm, Eu, Tb, Dy, Yb, Lu, Hf, Ta, Hg, Th and U in three radiopharmaceuticals.The irradiation of the samples was carried out in a 0.5 kW Bariloche RA-6Research Nuclear Reactor and the induced gamma-activity was measured by gamma-spectrometry.INAA proves to be an accurate and precise technique to obtain a quick informationon the concentration levels of several minor and trace components in radiopharmaceuticals.The quantification of heavy toxic elements is required for the registrationof radiopharmaceuticals.     

Determination of lanthanoids and some heavy and toxic elements in plant certified reference materials by inductively coupled plasma mass spectrometry

The possibilities of inductively coupled plasma mass spectrometry (ICP-MS) (choice of isotopes, instrument optimisation) for the determination of lanthanoids, and some heavy and toxic elements in plants are discussed. A variety of plant certified materials (NIST-SRM-1515, NIST-SRM-1547, NIST-SRM-1573a, NIST-SRM-1575, GBW 08504, GBW 08505) are analysed and the elements: As, Be, Bi, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Ga, Gd, Ho, La, Lu, Nd, Ni, Pb, Pr, Rb, Sm, Sr, Th, Te, Th, Tl, U, V, Y, Yb and Zn are determined. The comparison with certified values and literature values indicated that ICP-MS is a very promising method for the instrumental determination of Be, lanthanoids, Th and U and other elements at ng/g level in plants.     

Analysis of apatite crystals and their fluid inclusions by synchrotron radiation X-ray flourescence microprobe

Chemical composition analysis of apatites and their fluid inclusions from Yu'erya granite was carried out by synchrotron radiation X-ray fluorescence (SRXRF) microprobe. The result shows that all these apatite crystals have a similar chemical signature, with Ca, P, Cl, Mn, Fe, K, S, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Er, Yb, Lu, Sr, Y, Zr, U, Th, etc. The rare earth elements chondrite-normalized pattern indicates that these apatites are derived from S-type granite. It is shown by the SRXRF analysis that Zn, Cu and Cl are main components of fluid inclusions in apatites. It is the first time that SRXRF analysis is successfully applied in determination of composition of single fluid inclusions in apatite crystals. This technique was proved to be suitable for crystals with homogenously distributing components and thin covering layer would help to determine the composition of fluid inclusions.     

高能偏振能量色散X射线荧光光谱法分析古陶瓷

以国家地质标准样品制作工作曲线,用粉末压片法制样,高能偏振能量色散X射线荧光光谱法测定古陶瓷中包括15种稀土元素在内的56种元素,通过对6个陶瓷胎标准样品分析,结果表明:钪、钒、锰、铬、锌、镓、锗、铷、锶、钇、锆、铌、镉、锡、铯、钡、镧、铈、镨、钕、钆、钬、铒、铥、镱、镥、钍、铀等28种痕量元素测定值均在参考值的不确定度3～4倍范围,其他痕量元素如镍、铜、钼、锑、钐、铕、铽、铪、铅、铋等10种元素合格率为50%～83%。钠、镁、钾、钙、铁的氧化物和钛等6个项目均在允许误差范围内。氯、硫、磷的合格率均为66.6%。二氧化硅和三氧化二铝测定值和波长色散X射线荧光光谱熔融法测定结果相比,绝对误差分别在0.95%～4.46%和0.60%～1.66%之间。     

Characterization of deep sea sediments by INAA for radioactive waste management purposes

An instrumental neutron activation analysis method, using both reactor flux and epi-cadmium neutrons, has been developed for the determination of major, minor and trace elements in sub-seabed sediments. The method involves two different irradiations followed by three different counting periods using high-resolution Ge(Li) and low-energy photon detectors. The list of elements determined includes Ag, Al, As, Ba, Br, Ca, Ce, Cl, Co, Cr, Cs, Dy, Eu, Fe, Ga, Gd, Hf, Hg, I, In, K, La, Lu, Mg, Mn, Mo, Na, Nd, Ni, Pt, Rb, Re, Rh, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Th, Ti, Tm, U, V. W, Yb, Zn, and Zr. The accuracy of the method has been evaluated by analyzing four different standard reference materials. The method has been applied to core samples collected from the Great Meteor East and the South Nares Abyssal Plain which are being evaluated as potential sites for the possible disposal of vitrified highly active waste.     

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。     

57Fe Mössbauer spectroscopy of banded iron formations from eastern India

Samples of the mosses Hylocomium splendens and Pleurozium schreberi, collected in the summer of 1998, were used to study the atmospheric deposition of heavy metals and other toxic elements in the Chelyabinsk Region situated in the South Urals, one of the most heavily polluted industrial areas of the Russian Federation. Samples of natural soils were collected simultaneously with moss at the same 30 sites in order to investigate surface accumulation of heavy metals and to examine the correlation of elements in moss and soil samples in order to separate contributions from atmospheric deposition and from soil minerals. A total of 38 elements (Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, As, Se, Rb, Sr, Zr, Mo, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Yb, Hf, Ta, W, Au, Th, U) in soil and 33 elements Na, Mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Zn, As, Se, Br, Rb, Ag, Sb, Cs, Ba, La, Ce, Sm, Tb, Yb, Hf, Ta, W, Au, Th, U) were determined by epithermal neutron activation analysis. The elements Cu, Cd and Pb (in moss samples only) were obtained by atomic absorption spectrometry. VARIMAX rotated principal component analysis was used to identify and characterize different pollution sources and to point out the most polluted areas.     

Determination of 34 elements in Chinese geochemical standard reference materials by instrumental neutron activation analysis

Thirty four elements (Al, As, Ba, Br, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Gd, Hf, Ho, K, La, Lu, Mg, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Tb, Th, Ti, U, V, W, Yb) were determined by instrumental neutron activation analysis in the second set of Chinese geochemical standard reference materials (sediments from GSD-9 to GSD-12, soils from GSS-1 to GSS-8, rocks from GSR-1 to GSR-6) using both thermal and epithermal irradiations. Irradiation schemes designed to utilise short, medium and long-lived nuclides were employed in order to analyse major, minor and trace elements with different half-lives. The gamma-ray spectra were measured by Ge(Li) and HP(Ge) detectors. Relevant nuclear data and possible interferences are listed, and analytical results are presented and discussed.     

Microwave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductively coupled plasma-mass spectrometry

A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM_2.5). High temperature (200 °C), high pressure (200 psig), acid digestion (HNO₃, HF and H₃BO₃) with 20 min dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst and PM_2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using ¹¹⁵In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu and Dy in ambient PM_2.5 in an industrial area of Houston, TX.     

Mg(OH)_2共沉淀和直接稀释联用ICP-MS法准确测定海水中的多种常量-微量元素

对海水中多种常量/微量元素分别用Mg(OH)_2共沉淀和直接稀释ICP-MS法进行方法比较研究,分别确定了这些元素适宜的准确分析方法,为海水中常量/微量元素的ICP-MS测定提供了实用的检测手段。结果表明,Mg(OH)_2共沉淀法能够实现对V,Cr,Mn,Co,Cd及稀土元素(La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu)等19种微量元素的分离富集和准确测定;10倍直接稀释法能够同时准确测定海水中B,Sr,Li,Rb,I,V,Cr,As,Cd,U,Mo,Cu,Mn 13种微量元素,但不适合Zn,Ni,Co和Pb,以及稀土元素等在海水中浓度过低元素的测定;两种方法对适宜测定的元素均操作简便快速,具有较高的准确度和精密度。这两种方法联用,就可用约50 mL的海水实现大洋和近海海水中Co,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu(这15个元素采用Mg(OH)_2共沉淀法)及B,Sr,Li,Rb,I,V,Cr,As,Cd,U,Mo,Cu,Mn(这13个元素采用10倍直接稀释法)等28种元素的准确测定。