Determination of trace elements in food by neutron activation analysis

Neutron activation analysis (NAA) methods have been developed for the determination of major, minor and trace elements in duplicate diets and individual food items. These include a cyclic instrumental NAA (CINAA) method for measuring Se content through its short-lived nuclide^77mSe; epithermal INAA (EINAA) for I and As; conventional INAA for Br, Ca, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Rb, Sb, Sc, Sn and Zn; combination of EINAA and INAA for Al; radiochemical NAA (RNAA) for As, Au, Co, Cu, Fe, Hg, Mo, Sb, Se and Zn; and preconcentration NAA (PNAA) for U and Th. Accuracy of measurements have been evaluated by analyzing a number of biological and diet reference materials. Multielement concentrations of diets and foods have been measured by these methods.     

Elemental analysis of phosphate rocks: For sustainable agriculture in Pakistan

The concentration of 32 elements was determined in phosphate rock samples from the Hazara phosphate deposits of Pakistan using instrumental neutron activation analysis (INAA) technique employing different irradiation protocols. These included 23 major, minor and trace elements (Al, As, Ba, Br, Co, Cr, Cs, Fe, Ga, Hf, K, Mn, Na, Rb, Sb, Sc, Sn, Ta, Th, U, V, Zn and Zr) and 9 rare earth elements (REEs) namely Ce, Eu, Ho, La, Lu, Nd, Sm, Tb and Yb. The results have been compared with the global values of these elements. The concentrations for most of the elements studied are lower than the concentrations reported in the literature whereas the concentrations of As, Co, Fe, K, Mn, Na and Sb are comparable. Two samples namely HR-4 and HR-5 have the highest concentrations for majority of the REFs with high enrichment factors. The quality assurance of data was performed through the concurrent use of Lake Sediment (SL-1) and GSJ-JR-1 (Rhyolite) reference materials. The acquired data will serve as a reference for the follow-up studies to assess the agronomic effectiveness of the Hazara phosphate rocks.     

Instrumental NAA of carbonate rocks and its application for the analysis of secondary sedimentary environments in shallow sea

Aiming at distinguishing between the sedimentary environments in shallow sea using elemental geochemical markers, the determinations of trace elements in carbonate rocks by thermal neutron, epithermal neutron and short-irradiation activation analysis have been studied, and more than 30 major and trace elements determined. Al, Cl, Sc, Ti, V, Cr, Fe, Co, As, Br, Rb, Sb, Cs, Lu, Hf, Ta, Th and U were found to be the effective distinguishing markers for the secondary environments in shallow sea.     

Investigations on the direct introduction of cigarette smoke for trace elements analysis by inductively coupled plasma mass spectrometry

Direct introduction of mainstream cigarette smoke into an inductively coupled plasma mass spectrometry (ICP-MS) has been investigated with respect to its feasibility for on-line analysis of trace elements. An automated apparatus was designed and built interfacing a smoking machine with an ICP-MS for smoke generation, collection, injection and analysis. Major and minor elements present in the particulate phase and the gas phase of mainstream cigarette smoke of 2R4F reference cigarettes have been qualitatively identified by examination of their full mass spectra. This method provides a rapid-screening analysis of the transfer of trace elements into mainstream smoke during cigarette combustion. A full suite of elements present in the whole cigarette smoke has been identified, including As, B, Ba, Br, Cd, Cl, Cs, Cu, Hg, I, K, Li, Mn, Na, Pb, Rb, Sb, Sn, Tl and Zn. Of these elements, the major portions of B, Ba, Cs, Cu, K, Li, Mn, Na, Pb, Rb, Sn, Tl and Zn are present in the particulate phase, whereas the major portion of Hg is present in the gas phase. As, Br, Cd, Cl, I and Sb exist in a distribution between the gas phase and the particulate phase. Depending on the element, the precision of measurement ranges from 5 to 25% in terms of relative standard deviation of peak height and peak area, based on the fourth puff of 2R4F mainstream cigarette smoke analyzed in five smoking replicates.     

Calcium supplements as additional source of trace elements in health and disease Part 1: adequacy and safety of chelated calcium supplements

Eleven chelated calcium supplements intended for human consumption and produced by national and multinational companies have been studied for their mineral contents. Instrumental neutron activation analysis technique was used to quantify 12 elements (As, Br, Ce, Co, Cr, Fe, K, Na, Sb, Sn, Sr and Zn) while atomic absorption spectrometry technique quantified Cd, Cu and Ni. Three different irradiation protocols were adopted using a 27 kW tank-in-pool type miniature neutron source reactor. Most of the elements were present as minor or trace constituents except for Na that was quantified as major element in CaS-1 (3.73 %), CaS-2 (1.45 %), CaS-4 (1.56 %), CaS-5 (2.31 %), CaS-6 (1.84 %), CaS-7 (1.22), CaS-8 (1.73), CaS-9 (1.94), CaS-10 (2.07) and CaS-11 (2.48). However supplement CaS-3 with Ca source of calcium acetate contained only 53 μg/g of Na and the highest amount of Fe while As, Br, Cd and Sb were not detected in this sample. Percentage daily intakes with respect to their recommended dietary reference intake s and provisional tolerable daily intakes of essential and toxic elements showed that these elements contribute to a very low percentage of the recommended/tolerable levels for most of the supplements studied. Nevertheless the findings depict that it is very important for pharmaceutical and neutraceutical firms to completely identify these elements in the supplements and include their potency on the labels before being released to the consumers.     

马家塔矿煤层中有害痕量元素的质量分数特性

应用仪器中子活化（INAA）、电感耦合等离子体原子发射光谱（ICP AES）和原子吸收光谱（AAS）对神华集团马家塔露天矿2-2#煤层中Hg、As、Se、Pb、Be、Cr、Cd、Ni、Th、U、Mn、Mo、Co、Sb和Br共15种有害痕量元素的质量分数进行测定。结果表明，绝大部分痕量元素的质量分数都明显低于中国煤中元素质量分数的平均值，只有Hg和Mn的质量分数偏高，其中Hg的质量分数异常高；通过分析痕量元素在煤层垂向剖面上的质量分数变化特性，揭示出痕量元素在煤层中分布的非均一性,分析了影响痕量元素分布与富集的因素；通过痕量元素之间以及与黄铁矿硫、Fe、Al、Ca、P的聚类分析，研究了痕量元素之间以及与煤中不同矿物组分之间的亲和特性。     

Characterization of Indian cigarette tobacco and its smoke aerosol by nuclear and allied techniques

Forty brands of tobacco used in Indian cigarettes, 20 brands of bidis (tobacco rolled in wrapper leaves), 15 brands of chewing tobacco and 15 brands of snuff tobacco were analyzed by nuclear and allied techniques. The elements measured into tobacco can be grouped into seven categories from less than 1 ppm to 5% by weight. Concentration level varied from 0.5-5% for (Ca, K, Cl), 400-1500 ppm (Fe), 200-600 ppm (Na), 100-300 ppm (Ti, Mn, Br and Sr), 10-100 ppm (Cu, Zn and Rb), 1-10 ppm (Cr, Ni, Pb and La) and less than 1 ppm (As, Co, Cd, Sb, Hg and Eu). Among the above elements Cr, Ni, As, Cd, Pb, Hg and Sb are considered toxic. The percentage transfer of the elements from cigarette tobacco to smoke particles during smoking was also estimated using a smoking machine and collecting the smoke particles on a filter paper. The results show that Br, Cr, Sb and Zn have high percentage transfer from tobacco to its smoke of the order of 2-15%. Out of these Sb has the highest 15%. Cobalt, Fe and Sc have lowest percentage of transfer of the order of less than 1%. The percent transfer of these elements from tobacco to tobacco smoke is higher in case of bidis (1.5-3.0 times) as compared to cigarettes. In cigarettes also non-filter cigarettes have higher transfer (2-3 times) as compared to filter tip cigarettes.     

A study of trace element distribution in the solvent refined coal (SRC) process using neutron activation analysis

Twenty-two trace elements have been measured by INAA in materials produced in the Solvent Refined Coal (SRC) pilot plant. The elements As, Sb, Se, Hg, Ni, Br, Na, K, Cr, Sc, Fe, Co, Cs, Ce, Rb, Th, Sr, Ba, Tb, Eu, Sm and Lu were measured in coal, SRC, insoluble residues, solvents, and process waters. The liquefaction process produces a fuel lower in toxic trace elements than the parent coal. Elemental balances indicate that except for As, and Hg the SRC and insoluble residues contain more than 80% of the trace elements found in the coal. Evidence is presented indicating significant organic binding of As, Se, Hg, Br, Ni, and Co in the SRC.     

INAA and AAS of different products from sugar cane industry in Pakistan: Toxic trace elements for nutritional safety

Instrumental neutron activation analysis (INAA) have been used to determine As, Br, Hg, Sb and Se in combination with atomic absorption spectrometry (AAS) as a complementary technique for the quantification of Cd and Pb in jaggery, brown sugar, white sugar and molasses. All sugar cane products were collected from the local sugar cane industry of Pakistan. The highest concentration of these potentially toxic elements was quantified in molasses; however, molasses together with jaggery, brown sugar and white sugar contains trace amounts of all of these elements. Due to very low concentration of Cd it could only be detected in molasses. To evaluate the percentage contribution of these elements in the sugar cane products to the weekly recommended values, intakes on weekly consumption of 100 g of each item have also been calculated which follow the pattern Br>Se>Pb>Hg>As>Sb. The elevated Br contents may be attributed to the use of Br-containing chemicals for fumigation; however, these contents are well within the tolerance levels. The estimated weekly intake of all toxic elements is very low indicating that sugar cane products can be safely ingested as part of the diets.     

Determination of trace elements in biological standard kale by neutron activation analysis

Fifteen elements at trace levels have been determined by neutron activation analysis in the biological standard kale distributed byBowen. La, Br, As, Se, Sc, Ag, Zn, Co, Cr, Sb, Eu, Fe, and Zr have been determined by a nondestructive technique using a high-resolution Ge(Li) detector. Two more elements, Au and Hg, have been determined after radiochemical separation. The nondestructive procedure is shown to yield data in generally good agreement with those obtained by destructive techniques. Potential sources of error in the nondestructive technique are discussed.     

INAA and ETAAS of toxic element content of fruits harvested and consumed in Pakistan

Instrumental neutron activation analysis (INAA) and electro-thermal atomic absorption spectrometry (ETAAS) were employed to determine the toxic elements in fourteen fruits harvested in Pakistan. As, Br, Hg, Sb and Se were determined using INAA. Cadmium and Pb were determined using ETAAS. The intake levels of all toxic elements have been calculated. The data show that dates supply the maximum amount of most of the toxic elements. Peels of apple and pear have also been investigated and were found to contain higher concentration of toxic elements than their edible parts. The reliability of the techniques has been established by the use of standard reference materials. This study shows that all investigated fruits cultivated and consumed in Pakistan are safe for human consumption.     

Determination of impurities in semiconductor grade silicon by instrumental neutron activation analysis

Instrumental neutron activation analysis has been applied to semiconductor grade silicon to study the concentration levels of impurity elements, the contamination during the single crystal growing process, and the vertical and radial distributions of impurities, along with the decontamination effect in the analysis. Twenty elements of Au, Br, As, W, Cr, Co, Na, Eu, La, Se, Zn, U, Th, Hf, Fe, Sb, Ag, Ce, Tb and Ta have been analyzed in p- and n-type wafers, single crystals and a polycrystal by a single comparator method using two comparators of gold and cobalt. Considerable surface contamination has been found and could be removed by etching the surface with nitric and hydrofluoric acid before and after irradiation. The impurity concentration has been found to be generally increased in the process of single crystal growth. The vertical and radial distributions of impurities have revealed that some impurity elements were more concentrated in the top region of a single crystal rod than in the middle region, and that Br, Cr, La, Eu and Sb were enriched in the central region and As, U and Fe in the outer region.     

Use of combined NAA and SIMS analyses for impurity level isotope detection

Instrumental neutron activation analysis (INAA) and electro-thermal atomic absorption spectrometry (ETAAS) were employed to determine the toxic elements in fourteen fruits harvested in Pakistan. As, Br, Hg, Sb and Se were determined using INAA. Cadmium and Pb were determined using ETAAS. The intake levels of all toxic elements have been calculated. The data show that dates supply the maximum amount of most of the toxic elements. Peels of apple and pear have also been investigated and were found to contain higher concentration of toxic elements than their edible parts. The reliability of the techniques has been established by the use of standard reference materials. This study shows that all investigated fruits cultivated and consumed in Pakistan are safe for human consumption.     

Source identification of trace elements emitted into Athens atmosphere

The source identification of trace elements emitted into Athens (Greece) atmospheric environment has been studied by the Enrichment Factor (EF) and by Principal Component Analysis (PCA). The prevailing wind direction is related to EF data in order to identify the possible pathways of trace elements, in the Athens basin. As gas pollutants and trace elements could be emitted from the same source, the possible relation between these two groups is studied by PCA and correlation relations. According to EF data, the trace elements Fe, Sm, Th, Co, Sc, Cr and K have a crustal origin while the elements Zn, As, Sb, Ag, Br result of anthropogenic pollution. The study of the prevailing wind direction showed that the existing geophysical channel in the northern area of Athens basin could be a pathway for the entrance of Fe, La, Sm, Th, Co, Cr, Na and Ag into Athens atmosphere. On the contrary, the sea breeze could be a potential cleaner of the atmosphere from the same elements. Six source factors were resolved by PCA for all the Athens area explaining the 90% of the total variance. They could nominated as soil dust, central heating, movement of cars, car tires, car break abrasion and sea breeze. After the application of PCA and the linear regression model, the concentration of atmospheric ozone shows to have a positive significant correlation with Na and Zn and a negative significant correlation with As, Br, Ce, Co, Cr, Fe, La, Sb, Sc, Sm. A possible explanation of the mechanism for the decrease of atmospheric ozone concentration in relation to trace metals is given according to the existing literature data. This revised version was published online in July 2006 with corrections to the Cover Date.     

Dietary evaluation of toxic elements through integrated diet

Several potentially toxic trace elements, namely, Hg, Pb, Cd, As, Sb, Br and Se have been measured by INAA in combination with AAS techniques in the integrated diet representative of the inhabitants of Gujranwala, a highly industrialized city of Pakistan. The dietary intake values for these elements have been estimated from the prevailing concentration level in the summer and winter season diets, which reveals that present intake data are well within the reported WHO values and can be considered to be safe. Posslble sources of food contamination by the toxic elements and their adverse impacts on human heaith are briefly discussed.     

Concentration and distribution of toxic elements in rice and husk

Five varieties of rice have been analyzed to study the prevailing concentration and distribution of 10 trace elements in rice and rice husk. NAA in combination with AAS has been utilized for the determination of Hg, Pb, Cd, As, Br, Sb, Se, Ni, Al and Cs. The elemental ratios of rice to husk and within rice have been calculated to get information regarding their uptake channels. The daily supply of the elements to the human body has been estimated and from these the safety of the diet has been assessed by comparing with the suggested tolerance levels. A global distribution pattern of some of these elements in rice has also been evaluated.     

Elemental characterization of some Nigerian gemstones: tourmaline, fluorite and topaz by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) was employed in the determination of the major and trace element constituents in tourmaline, fluorite and topaz collected from the gemstone mineralization within a SW–NE trending pegmatite zone, central Nigeria. Cost, turnaround time, high sensitivity for certain elements, the non-destructive nature of analysis and its precision and accuracy have combined to make INAA an indispensable method for multi-element determination in virtually all geological matrices. The major element constituents in tourmaline were Al (119,800 ppm), Mn (4,348 ppm), Na (15,540 ppm) and Fe (34,290 ppm). For fluorite, Ca was the major element with a concentration of 552,000 ppm. In topaz, Al was the major constituent with a concentration of 322,800 ppm. The data suites reveal the presence of As, Br, La, Sc, Co, Hf, Ta and Sb in tourmaline, Na, As, Br, La, Yb, Co, Zn, Eu, Hf, Th in fluorite and Mg, Mn, Na, Br, La, Sc, Co and Ta as trace contaminants. No attempt was made to identify the molecular structure of the gemstones as oxygen, fluorine and silicon contents in any of them were not determined.     

Analysis of FDA in-house food reference materials with anticoincidence INAA

In-house reference material (IRM) cocoa powder (CCP) has been in use at US Food and Drug Administration laboratories for about 15 years. A single lot of commercial material was originally characterized for 32 elements by several laboratories and five techniques. A unique approach for basis weight determination based upon ambient relative humidity was developed for CCP, eliminating the need for dry weight determinations. The CCP Reference Sheet is updated by incorporating new results approximately every 5 years. The last update occurred in 2006. As part of an effort to revalidate and update values for CCP, anticoincidence instrumental neutron activation analysis (INAA) was used to determine mass fractions for 16 of the originally characterized elements, as well as to provide information on 16 other elements. Results were in very good agreement with 2006 Reference Sheet values. A new candidate IRM, fresh-frozen swordfish (FFSF) powder, was produced by adding inorganic As, Cd, Cr, Hg, Pb, Sb, and Se to liquid nitrogen-frozen commercial swordfish filets which were then homogenized. Portions of FFSF were analyzed by INAA to provide mass fraction and homogeneity information for As, Cd, Cr, Hg, Sb, and Se as well as for eight other elements occurring naturally in the material. Non-homogeneities were ≤2.5 % for As, Br, Cd, and Cs, and ≤1.8 % for Cr, Hg, Rb, Sb, and Se. Certified reference materials DORM-3 Fish Protein powder and fresh-frozen SRM 1947 Lake Michigan Fish Tissue were analyzed as controls.     

Assessing soil pollution from a municipal waste dump in Islamabad, Pakistan: a study by INAA and AAS

INAA and AAS techniques have been employed to determine 40 elements in soil of a municipal waste dump in sector H-11, Islamabad. Background soil was also analyzed to study the extent of contamination of the dump site soil. Most of the major elements in these soils represented the geochemical composition of the soil in this area. The enrichment factors for quantified elements identified high Sb and Mg contents that could be attributed to the presence of PET and food materials in the waste. Geo-accumulation Index (I _geo), Pollution Index (PI) and the Integrated Pollution Index (IPI) have also been calculated for all elements. The values for these indices show that municipal waste has distorted the soil ambiance and the soil of waste dump site is slightly to moderately polluted as compared to the background soil. The dump soil was found to be moderately polluted by the elements Ba, Br, Ga, Rb, Zn, Ni and Pb. Significantly high Cu, Mg and Sb contamination was observed for the waste soil that is likely to pose an environmental issue if current waste disposal procedures are continuously employed.     

Determination of antimony,arsenic, bismuth and copper by inductively coupled plasma atomic emission spectrometry in the electrorefining of copper

Inductively coupled plasma atomic emissionspectrometry (ICP-AES) has been applied as a rapid and routine method for the analysis of process electrolytes in the electrorefining of copper. Antimony, arsenic, bismuth and copper have been selected as major electrolyte constituents. For these elements profound statistical studies of spectral and interelement effects have been carried out. For As, Bi and Sb two analyte wavelengths have been selected, and for Cu one relatively insensitive analyte line has been chosen due to the high Cu concentration in samples. Best analytical lines were: As at 193.759 nm, Bi at 306.772 nm, Sb at 206.833 nm and Cu at 216.953 nm. Multiple linear regression proved to be very capable in the search of the best analytical wavelength and identifying interfering elements. Using simple acid based standards all elements investigated can be determined separately in complicated matrices with satisfactory results. Differences between true values and measured values can be partly eliminated by appropriate calculational methods.