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1.
A worldwide laboratory intercomparison was organized by the International Atomic Energy Agency's Analytical Quality Control Services (AQCS) involving the determination of elements in plant materials used for human consumption. The main purpose of this work was to evaluate the performance of our analytical methods including sample preparation and to obtain new reference materials that can be used in our further work. Both materials (spinach and cabbage) were analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA). Six subsamples of each material were subjected to our digestion procedure and the solutions were measured by ICP-AES. The dried samples were analyzed using INAA. Up to 26 elements were determined in plant materials. For easy review of our data a score has been calculated based on the reference value for each measured element. According to our results the ICP-AES technique was useful for determination of the following elements: Ba, Ca, Cr, Fe, K, Mn, Mo, P, S, Sr, Ti. The INAA method was reliable for measurement of Ce, Co, Mn, Na, Rb, Th, and V. 相似文献
2.
J. H. Lee J. S. Kim K. H. Cho J. Ch. Woo M. S. Han Y. S. Chung 《Journal of Radioanalytical and Nuclear Chemistry》1998,234(1-2):77-83
Trace impurity elements in high purity copper metal (4 mine class) put on the market were analyzed by Instrumental Neutron
Activation Analysis (INAA) and the results compared with those from Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS)
and Inductively Coupled Plasma Atomic Emission Spectrophotometry (ICP-AES). The sample irradiation was done at the irradiation
facilities (thermal neutron flux, 5·1012 n·cm−2·s−1) of the TRIGA Mark-III research reactor in the Korea Atomic Energy Research Institute. Four unalloyed copper standards (NIST
SRM # 393, 394, 395 and 398) were used to identify the accuracy and precision of the analytical procedure. The homogeneity
of samples was assessed by means of the elements such as Ag, As, Co, Sb, Se and Zn. The analytical results of INAA, GFAAS
and ICP-AES were in good agreement within expected uncertainties each other and showed the possibility of using them for the
analytical quality control. 相似文献
3.
Vanadium determination in rat tissues and biological reference materials by neutron activation analysis 总被引:2,自引:0,他引:2
J. Kučera M. Šimková J. Lener A. Mravcová L. Kinova I. Penev 《Journal of Radioanalytical and Nuclear Chemistry》1990,141(1):49-59
Vanadium was determined in adrenal gland, brain, ileum, kidney, liver, lung, muscle, myocard, skin, spleen, gonads, thyroid, and tibia of rats fed with normal diet and exposed to high vanadium doses in drinking water. Both radiochemical neutron activation analysis (RNAA) and instrumental neutron activation analysis (INAA) were employed. The RNAA procedure consisted in dry ashing samples prior to irradiation and vanadium separation from the irradiated samples by extraction with N-benzoyl-N-phenylhydroxylamine (BPHA) in toluene from 5 mol·l–1 HCl. Vanadium accumulation as a function of a type of the tissue, exposure time, sex of rats, and administration of V(IV) or V(V) was studied. For quality assurance purposes, the biological (standard) reference materials NBS SRM 1571 Orchard Leaves, NBS SRM 1577a Bovine Liver, IAEA H-4 Animal muscle, and Bowen's Kale were analyzed.Presented at the 2nd Balkan Conference on Activation Analysis and Nuclear-Related Analytical Techniques, Bled, 4–6 October, 1989. 相似文献
4.
NAA characterization of the new Bovine Liver SRM 总被引:2,自引:1,他引:1
R. Zeisler W. D. James E. A. Mackey R. O. Spatz R. R. Greenberg 《Journal of Radioanalytical and Nuclear Chemistry》2008,278(3):783-787
The National Institute of Standards and Technology (NIST) is preparing a freeze-dried powdered bovine liver tissue Standard
Reference Material (SRM) to replace SRM 1577b Bovine Liver as the stock of this material was exhausted during 2006. Like the
original SRM 1577 issued in 1972, this renewal focuses on the key elements for diagnostic, nutritional, and toxicological
measurements that are important to medical, veterinary, and environmental sciences investigations. NIST’s approach for value
assignment included extensive characterization by neutron activation analysis (NAA). Difficulties in the determination of
some elements present at very low levels were overcome by use of radiochemical separations. Twentyone elements were characterized
in SRM 1577c by NAA. The previous materials, SRM 1577 and 1577b, served as quality control. 相似文献
5.
Summary Results for a number of trace elements in a total human diet material (USDIET-1), obtained by the application of both INAA and RNAA are presented. Several dietary reference materials such as NBS SRM 1577A, and BCR CRM Single Cell Protein were also analyzed, and these results are also given. Combining measurements on short and long lived radionuclides, the INAA approach is useful for the determination of about 20 elements. In order to expand the elemental coverage or improve detection limits, RNAA was also explored in two modes: separation of radionuclides using organic ion exchange resins and the use of hydrated manganese dioxide. This combination is applicable to 15 trace elements. For example, using RNAA, the following results were obtained for USDIET-1: Cd=31.8, Mo=280, Cr=71, Ag=4, As=117 and Sb=9.4 g/kg. In the INAA mode, special attention was given to Al, F and Se. The F content of USDIET-1 was found to be 840 mg/kg, a rather high value, resulting from handling USDIET-1 by Teflon tools. By applying INAA and RNAA under two different laboratory conditions, it has been demonstrated that, even for the so-called difficult to determine elements like Cr, As or Mo, consistent results can be obtained. Thus, NAA promises to be a strong tool for human nutritional studies.
Einsatz der Neutronenaktivierung für Nahrungsmittel-Referenzmaterialien相似文献
6.
John W. Bennett Peter Grave Attila Stopic 《Journal of Radioanalytical and Nuclear Chemistry》2012,291(1):13-17
The k
0-method of standardisation for instrumental neutron activation analysis (INAA) has been used at the OPAL research reactor
to determine the elemental composition of three certified reference materials: coal fly ash (SRM 1633b), brick clay (SRM 679)
and Montana soil (SRM 2711). Of the 41 certified elements in the three materials, 88 percent were within five percent of the
certified values and all determinations were within 15 percent of the certified values. The average difference between the
measured and certified values was 0.1 percent, with a standard deviation of 4.1 percent. Since these reference materials are
widely used as standards in the analysis of archaeological ceramics by INAA, it has been concluded that the INAA facility
in Australia is particularly well-suited for nuclear archaeometry. 相似文献
7.
R. Zeisler R. R. Greenberg E. A. Mackey K. E. Murphy R. O. Spatz B. E. Tomlin 《Journal of Radioanalytical and Nuclear Chemistry》2009,281(1):11-15
Analyses for value assignment in the renewal Standard Reference Materials® SRM 1598a Animal Serum and SRM 1577c Bovine Liver included extensive characterization by neutron activation analysis (NAA). Conventional instrumental NAA procedures were complemented by pre-irradiation chemical separations for the determination of Al, V, Mn, and Cu, radiochemical separations for the determination of Ag, As, Cd, Cr, Cu, Mo, Sb, and Se, and the use of (anti-) coincidence gamma-ray spectrometry systems for the instrumental determination of Ag, Cr, and Hg. The previous materials, SRMs 1598, 1577, and 1577b, were analyzed together with the new materials for quality control. 相似文献
8.
A microwave-digestion system with a closed PTFE vessel was used to improve the leaching of inorganic constituents from biological samples with tetramethylammonium hydroxide (TMAH) and ethylenediaminetetraacetic acid (EDTA). The effects of microwave parameter settings and the quantities of TMAH and EDTA used on leaching efficiency were evaluated. This new digestion method has been applied to the standard reference materials NIST SRM 1577 B Bovine Liver 1515 Apple Leaves and NIES CRM No. 1 Pepperbush, No. 3 Chorella, No. 6 Mussel and No. 7 Tea Leaves. The major and minor elements in the digests were analyzed by flame atomic absorption spectrometry or graphite furnace atomic absorption spectrometry. Good agreement of the analytical results with the certified values was obtained. 相似文献
9.
Huang Donghui Sun Hongchao Ni Bangfa Tian Weizhi Zhang Yuanxun Wang Pingsheng Liu CunXiong Zhang Guiying Xiao Caijin Zhang Haiqing Zhao Changjun 《Journal of Radioanalytical and Nuclear Chemistry》2011,288(1):163-169
Sampling behavior of multielements for NIST SRM 2703, a marine sediment, was studied with sample sizes from 1 mg down to ng level by a combination of INAA, PIXE and SRXRF. On 1 mg sample size level, sampling behavior for multielements in NIST SRM 2703 and its parent SRM 2702 were comparatively characterized by using INAA combining with Ingamells model. Results showed that sampling uncertainties for 12 elements of both materials were found to be better than 1%, and those of four other elements in SRM 2703 better than in SRM 2702. At sample sizes not able to be accurately weighed (<1 mg), PIXE and SRXRF were used and the effective sample sizes estimated. Sampling uncertainties for nine elements were found to be better than 1% at sample sizes of tenth mg level, and those for six elements better than 10% on ng levels. 相似文献
10.
Use of neutron activation analysis for the characterization of single-wall carbon nanotube materials
Rolf Zeisler Rabia Oflaz Rick L. Paul Jeffrey A. Fagan 《Journal of Radioanalytical and Nuclear Chemistry》2012,291(2):561-567
Instrumental neutron activation analysis (INAA) and prompt gamma neutron activation analysis (PGAA) were used to characterize
a variety of single-wall carbon nanotube (SWCNT) materials from different principal production processes, as well as a material
containing SWCNTs together with other carbon species, catalyst residues, and trace element contaminants to be issued by the
National Institute of Standards and Technology for characterization and distribution as Standard Reference Material SRM 2483
Carbon Nanotube Soot. INAA proved to be well suited for the direct determination of catalyst and contaminant trace elements
requiring only minimal sample preparation. PGAA complemented the INAA data in particular with determinations of the light
elements. Carbon and hydrogen results provided information on the materials purity and storage properties. Strategies for
the quality assurance of the measurements in these new materials were developed. INAA and PGAA data were provided for the
value assignment of mass fractions of catalyst and trace elements in the candidate SRM and a systematic overview was obtained
of the catalyst and trace element contaminants associated with each of the major production routes. 相似文献
11.
A microwave heated, vapor-phase nitric acid-hydrogen peroxide digestion method for pulverized, biological sample materials was developed. Sample masses up to 200 mg were digested using calibrated quartz inserts inside first generation type, low-pressure, Teflon-PFA microwave vessels. In the first step, samples were digested in the vapor-phase for 80 min using a progressive heating pattern. Three mL of 70% nitric acid and 0.5 mL of 30% hydrogen peroxide were used as digestion reagents. In the second step, the small residue left after first step digestion was dissolved in 1.4% nitric acid or additionally with 0.5% hydrofluoric acid by heating for 15 min. The digestion method was optimized using pike (Esox lucius) muscle as a test material. The method was further optimized using three certified reference materials. Ca, Cu, Fe, Mg and ¶Zn were determined from NIST-SRM 1577a bovine liver by ICP-AES. Cr and Ni were determined from NIST-SRM 8433 corn bran and NRCC DOLT-2 dogfish liver by GFAAS. For all elements the values obtained were close or within certified limits. Spike recoveries were between 96 to 107%. Digestion efficiency ranged from 91 to 99%. 相似文献
12.
Instrumental neutron activation analysis (INAA) was applied to assess element concentrations in eleven samples of mineral supplements/multivitamins acquired in drugstores and pharmacies in São Paulo city, SP, Brazil. Concentrations of Ca, Co, Cr, Cu, Fe, K, Na, Se and Zn were determined. A comparison was made between the results obtained with the labels of the mineral supplents. Certified reference materials, NIST SRM1400 Bone Ash and NIST SRM 1633b Coal Fly Ash were analyzed for quality control of the analytical results. 相似文献
13.
Yang Yan-Zhao Sun Si-Xiu Yang Yong-Hui Li Hong-Bin 《Journal of Radioanalytical and Nuclear Chemistry》2000,246(2):263-266
The biological standard reference materials Orchard Leaves SRM 1571 and Oyster Tissue SRM 1566a was analysed by instrumental neutron activation analysis (INAA) at the International Centre for Environmental and Nuclear Sciences, Jamaica at (ICEN) and at the Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), Brazil. The comparison of the results with those obtained with the more powerful reactor are used to evaluate the possibilities of INAA for the analysis of biological samples at ICENS. The detection limits, the precision and accuracy of the results obtained in both laboratories are compared. The advantages and disadvantages of the different irradiation facilities are discussed. Some results obtained for Jamaican biological samples are also presented. 相似文献
14.
A. M. S. Nyomora R. N. Sah P. H. Brown R. O. Miller 《Analytical and bioanalytical chemistry》1997,357(8):1185-1191
This study compares four sample dissolution methods for Boron determination in two National Institute of Standard and Technology
(NIST) botanical Standard Reference Materials (SRMs) and three Agriculture Canada/NIST RMs, each having a reference (certified
or best estimate) B concentration. The dissolution treatments consisted of: 1) dry ashing at 500° C, 2) wet digestion with
HNO3 + H2O2, 3) extraction with hot HNO3 and 4) closed vessel microwave dissolution. The samples were spiked before and after imposing dissolution treatments to study
B recovery by inductively coupled plasma mass spectrometric (ICP-MS) analysis. Microwave digests of NIST SRM 1515 and some
in-house RMs were also used to compare the B values of ICP-MS and ICP-AES (atomic emission spectrometry). While all three
digestion methods (dry ashing, wet ashing and microwave) dissolved botanical samples, only the microwave method worked well
for animal tissues. In terms of B values in these materials, there was no significant difference among the three digestion
treatments. Near 100% recovery of B spiked before and after the sample dissolution indicates that there may not be a significant
loss of B during the dissolution process used in this study. Extraction with hot HNO3 was as effective as the three digestion treatments, and B values for this method agreed well with reference values. For the
botanical materials studied, the B values determined by ICP-AES were not significantly different from ICP-MS values. This
study shows that a simple, time and labor efficient hot HNO3 extraction is as effective as other digestion/dissolution methods for quantitative B recovery from biological materials.
Received: 13 June 1996 / Revised: 17 September 1996 / Accepted: 19 September 1996 相似文献
15.
Three digestion procedures have been tested on lichen samples for application in the determination of major, minor and trace elements (Al, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, V and Zn) in lichen samples collected in Aegean Region of Turkey by inductively coupled plasma atomic emission spectrometer (ICP-AES). The acid mixture of concentrated HNO3, H2O2 and HF were used. The instrument was optimized using lichen matrix considering RF power, nebulizer pressure, auxiliary flow rate and pump rate. The accuracy of the overall analyses was first estimated by analysis of two certified reference materials. Good agreement between measured and reference values were found for almost all elements. As the second way of determining the accuracy, results obtained from independent analytical techniques (ICP-AES and instrumental neutron activation analysis (INAA)) were compared for all elements by analyzing real samples. Correlation coefficients of two techniques for the elements ranged between 0.70 (Mg) and 0.96 (Fe). Among the three digestion systems, namely microwave, open vessel and acid bomb, microwave digestion system gave the best recovery results. The method detection limit (MDL) was computed using reagent blanks of microwave digestion system since it provides cleaner sample preparation. Detection limit is adequate for all elements to determine the elements in lichen samples. The precision was assessed from the replicate analyses of reagent blanks of microwave digestion system and was found to be less than 1.5% relative standard deviation (R.S.D.). 相似文献
16.
A microwave heated, vapor-phase nitric acid-hydrogen peroxide digestion method for pulverized, biological sample materials was developed. Sample masses up to 200 mg were digested using calibrated quartz inserts inside first generation type, low-pressure, Teflon-PFA microwave vessels. In the first step, samples were digested in the vapor-phase for 80 min using a progressive heating pattern. Three mL of 70% nitric acid and 0.5 mL of 30% hydrogen peroxide were used as digestion reagents. In the second step, the small residue left after first step digestion was dissolved in 1.4% nitric acid or additionally with 0.5% hydrofluoric acid by heating for 15 min. The digestion method was optimized using pike (Esox lucius) muscle as a test material. The method was further optimized using three certified reference materials. Ca, Cu, Fe, Mg and Zn were determined from NIST-SRM 1577a bovine liver by ICP-AES. Cr and Ni were determined from NIST-SRM 8433 corn bran and NRCC DOLT-2 dogfish liver by GFAAS. For all elements the values obtained were close or within certified limits. Spike recoveries were between 96 to 107%. Digestion efficiency ranged from 91 to 99%. 相似文献
17.
A radiochemical neutron activation analysis using a rare earth group separation scheme has been used to measure ultratrace levels of rare earth elements (REE) in IAEA Human Hair (HH-1), IAEA Animal Bone (H-5), NBS Bovine Liver (SRM 1577), and NBS Orchard Leaf (SRM 1571) standards. The REE concentrations in Human Hair and Animal Bone range from 10–8 g/g to 10–11 g/g and their chondritic normalized REE patterns show a negative Eu anomaly and follow as a smooth function of the REE ionic radii. The REE patterns for NBS Bovine Liver and Orchard Leaf are identical except that their concentrations are higher. The similarity among the REE patterns suggest that the REE do not appear to be fractionated during the intake of biological materials by animals or humans. 相似文献
18.
Silver in selected, predominantly biological, reference materials (NIST SRM 1515, 1547, 1549, 1566a, 1571, 1577b, 2704, CTA-OTL-1,
and Bowen’s Kale) was determined using neutron activation analysis (NAA) in two different analytical modes: instrumental NAA
with epithermal neutrons (ENAA), and NAA with radiochemical separation (RNAA). The ENAA mode was based on long-time 5-hour
irradiation of samples in a special Cd lined box with counting after 8-month decay. The RNAA procedure consisted in 20-hour
irradiation of samples, their decomposition/dissolution by alkaline-oxidative fusion, and precipitation of AgCl including
several purification steps. Both methods provided Ag contents in the analyzed reference materials consistent with certified
and/or literature values down to the ng·g−1 level. 相似文献
19.
Michael Raessler Jan Rothe Ines Hilke 《International journal of environmental analytical chemistry》2013,93(9):707-715
AI, Fe, Mn and Zn were determined in two ditTerent species of woodlouse: Porcellio scaber and Porcellio dilalalus. Both species were cultivated under standardized conditions in a climatic chamber. Moreover, skins of the cultivated animals were collected and analyzed separately to examine a possible way of decontamination by moulting. To obtain enough sample material for each species, IS animals of the same age and size were pooled. For skin analysis, 10–12 skins were collected and pooled. The animals and their skins were dried, ground and digested in pure concentrated nitric acid using multiwave-assisted high-pressure digestion and. finally, analyzed by ICP-OES. Special emphasis was given to quality control: the reference materials Dorm-2, Dogfish Muscle (Squalus acanthias) and SRM 1577b Bovine Liver, were used to evaluate the whole analytical process including sample digestion. These reference materials of animal origin were selected to match the matrix of the samples as closely as possible. While concentrations of Fe. Mn and Zn were traced to both reference materials, the concentration of AI was checked by Dorm-2 only. Analyses of the elements in the reference materials were carried out using four ditTerent wavelengths for each element simultaneously. aiming at the determination of the best suited wavelength for each element. Analyses of woodlouse samples and their skins were finally carried out using the wavelengths with the highest sensitivities after absence of spectral interferences had been demonstrated. 相似文献
20.
Ochsenkühn-Petropoulou M Ochsenkühn KM 《Fresenius' Journal of Analytical Chemistry》2001,369(7-8):629-632
The capability of three analytical techniques, inductively coupled plasma-atomic emission spectrometry (ICP-AES), anodic stripping voltammetry (ASV), and instrumental neutron-activation analysis (INAA) have been compared for the determination of Cd, Fe, Pb, and Zn in airborne particulate matter, collected on cellulose filters, from the atmosphere of the large area of Thessaloniki, Greece. Two procedures were tested for quantitative leaching of these elements from the filters before ICP-AES and ASV, digestion with aqua regia in a Teflon autoclave, after dissolution of the organic matter with HClO4 under ambient conditions, and ultrasonic extraction with a mixture of HNO3 and HCl. Validation of the leaching and digestion procedures revealed that digestion in the autoclave is more effective, especially for Fe. The concentrations of these elements over a decade in both industrial and urban areas of the investigated region are compared. 相似文献