Substoichiometric determination of phosphorus

Phosphorus in orchard leaves (NBS SRM-1571) and spinach (SRM-1570) was determined by various substoichiometric analytical methods such as the direct method, GRASHCHENKO's method and the method of carrier amount variation. All samples were labelled with³²P radioisotope. The data obtained by the method of carrier amount variation were also treated by the method of least squares instead of De VOE's method. Phosphorus concentration in orchard leaves was 0.206±0.011% by the direct method, 0.219±0.011% by GRASHCHENKO's method, 0.211±0.011% by the method of carrier amount variation and 0.207±0.007% by the method of least squares, respectively. These values agree with the value reported by NBS (0.21±0.01%). Furthermore, these concentrations obtained by various substoichiometric methods were compared with those by radioactivation reported in a prevoius paper.     

Monostandard instrumental neutron activation analysis of Chinese Biological Standard Reference Material using short-lived radionuclides

A routine procedure for monostandard INAA using short-lived radionuclides with half-lives from 2 min to 15 hrs is described. Ten elements (Al, Mg, Ti, V, Mn, Cl, Na, K. Br and Cu) are determined in Chinese Biological Standard Reference Material (peach leaves). The quality of analysis was checked by analyzing the U. S. NBS Standard Reference Materials SRM-1571 and SRM-1648.     

Possibilities of low-level determination of silicon in biological materials by activation analysis

The capabilities of neutron and photon activation analysis (NAA and PAA, respectively) for low-level determination of silicon in biological materials have been examined. Sensitivities of a variety of modes of NAA and PAA with radiochemical separation have been evaluated. Results are presented for silicon in reference materials CSRM 12–2-03 Lucerne, Bowen’s Kale, NIST SRM-1571 Orchard Leaves, and NIST SRM-1515 Apple Leaves. The results were obtained by employing the ²⁹Si(n,p)²⁹Al reaction with fast reactor neutrons and the radiochemical procedure developed for aluminium separation. Possibilities of further improvement of the silicon determination limit down to the μg g^–1 level by employing NAA and PAA with radiochemical separation are outlined.     

Multielement analysis of Chinese Biological Standard Reference Material by monostandard instrumental neutron activation analysis

A procedure for monostandard INAA of 21 elements (Hg, As, Br, Cr, Sb, Se, Ba, Zn, Ca, Ce, Co, Cs, Eu, Fe, Hf, K, La, Rb, Sc, Sr, Ta) in Chinese Biological Standard Reference Material (peach leaves) is described. The accuracy of the procedure was checked by analyzing the U.S. NBS Standard Reference Materials SRM-1571 and SRM-1632a.     

Application of instrumental neutron activation analysis to plant medicines in Ghana: A review

Some essential elements in eleven plant medicines used at the Center for Scientific Research into Plant Medicine (CSRPM), Mampong-Akwapim, Ghana, for the management and cure of various diseases were determined by instrumental neutron activation analysis (INAA), using thermal neutrons at a flux of 5^.10¹¹ n^.s^-1.cm^-2. The plant medicines were: Sirappac powder-E, Tina-A powder, Blighia powder, Aphrodisiac powder, Ninga powder and Lippia tea. The others are Olax powder, Ritchiea powder, Momordica powder, Kenken and Fefe powder. Concentrations of seventeen elements namely Al, Br, Ca, Cl, Co, Cu, Cr, K, Mn, Mg, Na, Rb, Sb, Sc, Ta, V, and Zn have been determined by short, medium and long irradiation times. Of these elements Co, Sb, and Sc are found to be present at the trace level, Br, Cu, Cr, Mn, Rb, Ta, V and Zn at the minor level, while Al, Ca, Cl, K, Mg and Na were generally at major level. The differences in the concentration of the elements are attributed mainly to soil composition and climate in which the plants grow. Standard reference material NIST SRM-1571 (Orchard Leaf) was analyzed simultaneously with the samples. The precision and accuracy of the method were evaluated using real samples and the standard reference material. It was found that the elemental concentrations measured in the NIST SRM-1571 were within ±10% of the reported values. The importance of these elements as related to human health and nutrition has been discussed.     

Natural radioactivity in Brazilian bottled mineral waters and consequent doses

Instrumental neutron activation analysis (INAA) has been applied tomultielement determination of five medicinal plants which are used to curevarious diseases in Ghana. These are: Sirappac powder-E, Tina-A powder, Aphrodisiacpowder, Blighia powder and Olax powder. Concentrations of fifteen elementsAl, Ba, Br, Ca, Cl, Co, K, Mn, Mg, Na, Rb, Sb, Sc, Se, Ta, V and Zn have beendetermined by short, medium, and long irradiation times with a thermal neutronflux of 5 . 10 11 n . cm –2. s –1 . Of these Co, Sb, and Sc arefound to be present at trace level, Br, Mn, Rb, Ta, V and Zn at the minorlevel and Al, Ca, Cl, K, Mg, and Na are generally at the major level. StandardReference Material NIST SRM-1571(Orchard Leaf) was analysed simultaneouslywith the samples. The precision and accuracy of the method was evaluated usingreal samples and the standard reference material. It was found out that theelemental concentrations measured in the NIST SRM-1571 are within ±10%of the reported values.     

Surface treatment of borosilicate glass beakers for prevention of sodium contamination

Pyrex glass beakers are treated with molten Ca(NO₃)₂-KNO₃ (20:80 mol %) mixture at 500°C for 3 h. Treated beakers can be used successfully in wet oxidation of SRM-1571 Orchard Leaves for sodium determination; at least 10 oxidations can be done without sodium contamination. Mass spectrometry is used to investigate the depth profiles of glass components within 60 nm of the glass surfaces and to clarify the mechanism of the sodium contamination.     

Characterization and traceability of two generations of standard reference material for the measurement of vitamin K1(phylloquinone) at endogenous concentrations in human plasma and serum

Vitamin K is an essential micronutrient required for blood coagulation, regulation of vascular calcification and bone mineralization. Plasma and serum measurements of vitamin K₁(phylloquinone, K₁) made using high-performance liquid chromatography with fluorescence detection, or tandem mass spectrometry are used clinically and in population studies to assess vitamin K status. Standard reference materials provide a validation tool for laboratories, helping assure clinical diagnosis and the comparability of data from different populations. We manufactured two K₁ standard reference materials, in 2009 (KEQAS SRM-001) and in 2019 (KEQAS SRM-002). The target concentrations of K₁ were assigned to each SRM using the All Laboratory Trimmed Mean of results reported by selected laboratories enrolled in the Vitamin K External Quality Assurance Scheme (KEQAS). The assigned concentrations of K₁ for KEQAS SRM-001 and SRM-002 were 0.25 and 0.36 μg/L respectively. In 2019 KEQAS SRM-001 was re-analysed simultaneously with KEQAS SRM-002 to provide traceability between the two standards, therefore aiding comparability of analysis performed using these materials. Both standards were stored as aliquots at −80°C in the dark; annual re-analysis of the materials indicated that K₁ is stable for at least 12 years in these conditions.     

Determination of sampling constants for selenium in biological reference materials by neutron activation

Summary A cyclic instrumental neutron activation analysis method has been used to calculate sampling constants and to evaluate homogeneity for Se in five biological reference and certified reference materials, namely NRC lobster hepatopancreas (RM TORT-1), IAEA horse kidney (RM-H8), and NIST bovine liver (SRM-1577a), oyster tissue (SRM-1566) and mixed diet (RM-8431). The between-weight-range heterogeneity has been observed to be no greater than the within-weight-range heterogeneity. The subsampling standard deviation (S _s) has been found to be less than the measurement standard deviation (S _m) for H-8 (>5 mg sample) and TORT-1 (>50 mg). For 1577a, S _s is almost equal to S _m; while S _s is 2–3 times higher than S _m for the other two materials. The sampling constants varied between 0.04 and 3.0 g for four materials while the mixed diet had a value of 31 g.     

Total analysis of plant material and biological tissue by spark source mass spectrometry

Summary Analysis of biological material by spark source mass spectrometry is reported. Preliminary studies mainly based upon the analysis of the NBS standard reference material SRM-1571 (Orchard Leaves) are described. Attention is drawn to the importance of a suitable sample preparation method. The advantages of a wet digestion technique in a Teflon bomb are discussed and its use is justified by the satisfactory overall analysis precision of about 20%.

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Gesamtanalyse von Pflanzenmaterial und biologischem Gewebe mittels Funken-Massenspektrometrie

Zusammenfassung Die Analyse von biologischem Material mit der Funken-Massenspektrometrie wird beschrieben. Erste Untersuchungen basieren auf der Analyse der NBS-Standardprobe Orchard Leaves (NBS SRM-1571). Die Wichtigkeit einer geeigneten Probenvorbereitung wird betont. Die Vorteile der Naßaufschlußtechnik in einer Teflonbombe werden diskutiert und ihr Einsatz durch die gute Gesamtreproduzierbarkeit von etwa 20% gerechtfertigt.

     

Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultra-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B&C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS.     

Possibilities of low-level determination of silicon in biological materials by activation analysis

The capabilities of neutron and photon activation analysis (NAA and PAA, respectively) for low-level determination of silicon in biological materials have been examined. Sensitivities of a variety of modes of NAA and PAA with radiochemical separation have been evaluated. Results are presented for silicon in reference materials CSRM 12-2-03 Lucerne, Bowen's Kale, NIST SRM-1571 Orchard Leaves, and NIST SRM-1515 Apple Leaves. The results were obtained by employing the 29Si(n,p)29Al reaction with fast reactor neutrons and the radiochemical procedure developed for aluminium separation. Possibilities of further improvement of the silicon determination limit down to the microg g(-1) level by employing NAA and PAA with radiochemical separation are outlined.     

Instrumental neutron activation analysis of trace elements in quartz

A scheme for INAA of 32 elements (As, Au, Ba, Br, Ca, Cd, Ce, Co, Cr, Cs, Eu, Fe, Hf, Hg, Ir, K, La, Lu, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Tb, Th, U, W. Yb, Zn) in quartz glass is proposed. The accuracy of the procedure is evaluated by the analysis of two NBS standard reference materials (SRM-1571 and SRM-1632-a). The method is convenient for routine work. The method was used for the determination of impurities in laboratory quartz glass. Dedicated to the 60th birthday of acad. prof. g. bliznakov     

Application of NAA standardization methods using a low power research reactor

Two widely used neutron activation analysis (NAA) standardization methods (relative and k ₀) have been validated at the Ghana Research Reactor-1 (GHARR-1) Centre using environmental and biological standard reference materials (SRMs). The samples were IAEA Soil-7 as an environmental sample, and NIST Orchard Leaves 1571 as a biological sample. The qualitative and quantitative analyses were done using a high resolution Canberra N-type high purity germanium (HPGe) detector. The accuracy and precision were evaluated for the elements analysed. The concentrations of most of the elements were found to be within 10% of the certified values. Precision was calculated from six replicate measurements and was found to be within 15%.     

Elemental analysis of leaves and extracts of Casearia medicinal plants by instrumental neutron activation analysis

Summary Instrumental neutron activation analysis (INAA) was applied to determine the inorganic composition of leaves and extracts from three different species of Casearia genus plant (C. sylvestris, C. decandra and C. obliqua). Statistical analysis of the analytical data of leaf showed that the three Casearia species present similar elemental composition. Extract from C. sylvestris showed significantly different inorganic content in comparison with the two other species. Certified reference material NIST SRM-1515 Apple Leaves was analyzed for quality control.     

Substoichiometric extraction of chromium

Substoichiometric extraction of chromium with tetraphenylarsonium chloride (TPACl), tri-n-octylamine (TNOA), diethylammonium diethyldithiocarbamate (DDDC) and ammonium pyrrolidinedithiocarbamate (APDC) was examined in detail. Chromium can be extracted substoichiometrically in a pH range, which is 1.1–2.6 for the TPACl compound, 0.6–2.3 for the TNOA compound, 5.1–6.4 for the DDCC chelate and 3.9–4.9 for the APDC chelate. Chromium in high-purity calcium carbonate, Orchard Leaves (NBS SRM-1571) and Brewers Yeast (NBS SRM-1569) was determined by neutron activation analysis combined with substoichiometric extraction by DDDC and APDC. The values of 2.0±0.02 ppm and 2.6±0.2 ppm were obtained for Brewers Yeast and Orchard Leaves, respectively. These values were in good agreement with the values reported by NBS. The reaction mechanism and the reaction ratio between hexavalent chromium and dithiocarbamate were also discussed.     

Metal content in mosses from the Metropolitan Area of the Toluca Valley: a comparative study between inductively coupled plasma optical emission spectrometry (ICP-OES) and total reflection X-ray fluorescence spectrometry (TXRF)

The comparison between inductively coupled plasma optical emission spectrometry (ICP-OES) and total reflection X-ray fluorescence spectrometry (TXRF) for simultaneous determination of metal content (Cr, Cu, Fe, Mn, Pb and Zn) in mosses from the Metropolitan Area of the Toluca Valley was performed. Epiphytic mosses (Fabriona ciliaris and Leskea angustata) were collected in two sampling campaigns and were digested with HNO₃, HCl and HF for ICP-OES method and HNO₃ and HCl for TXRF method. The certified reference material (IAEA-336, Lichen) and the Standard Reference Material (SRM-1573, tomato leaves) were used for the quality control and to evaluate trueness and precision. Linearity, detection and quantification limits were also determined. Results show an ICP-OES and TXRF trueness mean of 101 ± 5% and 97 ± 9%, respectively; the relative standard deviation (RSD percent) was less than 17% in both methods. The moss samples exhibit a satisfactory precision (RSD ≤ 20%), because the RSD percent for ICP-OES, from 2% to 15%, and that for TXRF, from 1% to 17%, were obtained. One factor experimental design and simple regression analysis (α = 0.05) were used to compare the ICP-OES and TXRF metal concentrations. The statistical results do not show significantly different values for Cu, Mn, Pb and Zn in both the sample campaigns. In addition, the average results for Cr in the first sample campaign (30.3 ± 11.4 mg/kg for ICP-OES and 18.6 ± 9.8 mg/kg for TXRF) and Fe values in the second sample campaign (10,810 ± 2980 mg/kg for ICP-OES and 8380 ± 2350 mg/kg for TXRF) were significantly different in both methods. These differences are attributed to an incomplete sample digestion in the TXRF sample preparation. The results of the simple regression analyses show p-value less than 0.05, which indicates an equivalent and significant relation between ICP-OES and TXRF.     

Selective preconcentration and determination of iodine species in milk samples using polymer inclusion sorbent

A method to determine low levels of iodine species namely I⁻ and IO₃⁻ in aqueous samples was developed and applied to milk and milk powder samples. It is based on selective preconcentration of I⁻ in polymer inclusion sorbent (PIS) and neutron activation analysis (NAA) of I⁻ sorbed in PIS. The PIS was found to be highly selective for I⁻ in presence of IO₃⁻ and other anions commonly present in the milk samples. In order to preconcentrate total I⁻ + IO₃⁻ content in the PIS, IO₃⁻ was reduced to I⁻ using a mixture of acetic acid and ascorbic acid. It was found that total iodine content in milk could be determined with epithermal neutron activation analysis (ENAA). A scheme was developed to determine I⁻, IO₃⁻ and total iodine. The developed method was applied to milk reference materials (NIST SRM-1549 and IAEA-RM-153 milk powder) and a commercially available milk powder. The scheme for estimation of iodine in different forms was validated by using reference material NIST SRM-1549.     

Alpha spectrometric evaluation of SRM-995 as a potential uranium/thorium double tracer system for age-dating uranium materials

Uranium-233 (t _1/2 ~ 1.59E5 years) is an artificial, fissile isotope of uranium that has significant importance in nuclear forensics. The isotope provides a unique signature in determining the origin and provenance of uranium-bearing materials and is valuable as a mass spectrometric tracer. Alpha spectrometry was employed in the critical evaluation of a ²³³U standard reference material (SRM-995) as a dual tracer system based on the in-growth of ²²⁹Th (t _1/2 ~ 7.34E3 years) for ~35 years following radiochemical purification. Preliminary investigations focused on the isotopic analysis of standards and unmodified fractions of SRM-995; all samples were separated and purified using a multi-column anion-exchange scheme. The ²²⁹Th/²³³U atom ratio for SRM-995 was found to be 1.598E?4 (±4.50 %) using recovery-corrected radiochemical methods. Using the Bateman equations and relevant half-lives, this ratio reflects a material that was purified ~36.8 years prior to this analysis. The calculated age is discussed in contrast with both the date of certification and the recorded date of last purification.