Extraction-chromatographic system TBP-HBr in radiochemical neutron activation analysis of high-purity materials

The extraction and extraction-chromatographic behaviour of a variety of elements in the TBP-HBr system with concentrations from 0.1 to 7M HBr has been studied. The results allowed the development of simple procedures for radiochemical neutron activation determination of 22 impurity elements (Na, K, Sc, Cr, Mn, Fe, Co, Ni, Cu, Ga, As, Se, Rb, Sr, Zn, Mo, Ag, Sb, Te, Ba, La, Hf and W) in high-purity cadmium and indium samples with detection limits from 1 g g^–1 for Fe and Zr to 0.01 ng g^–1 for Na, Sc, Mn with relative standard deviations < 0.15. To increase the selectivity of the extraction-chromatographic separation, use was made of extraction suppression and co-extraction effects. The procedure for the extraction-chromatographic separation of scandium from a number of other elements is described as an example. The procedure can be used for simultaneous quantitative separation of impurity radionuclides from radiation produced long-life scandium radionuclides in the neutron activation analysis of titanium and vanadium.     

Determination of impurities in titanium and titanium oxide by radiochemical neutron activation analysis

A radiochemical neutron activation analysis has been applied to 2N–4N grade titanium metal and its oxide. Twenty two impurities were separated in a group from scandium by a radiochemical separation method using cation exchange resin with HBr and HCl. The contents of the elements were calculated by a single comparator method using two monitors. The analytical results agree well within 10% deviation with those obtained by instrumental method. Eighteen elements, Na, Fe, Co, As, Se, Sr, Mo, Sb, La, Eu, Tb, Yb, Lu, Hf, Ta, W, Th and U, are determined in titanium oxides and 17 elements, Na, Cr, Fe, Co, Se, As, Zr, Mo, Sb, Cs, Ce, Tb, Yb, Hf, Ta, W and Th, in titanium metals.     

Improvement of analytical sensitivities for the determination of antimony,arsenic, cadmium,indium, iodine,molybdenum, silicon and uranium in airborne particulate matter by epithermal neutron activation analysis

As part of an ongoing Great Lakes deposition study, we have determined a series of heavy metals in air filter samples collected near Lake Ontario. To decrease our detection limits for key elements used in our receptor modeling, we have employed instrumental epithermal neutron activation analysis (NAA) and Compton suppression techniques. Our detection limits were much better than those with thermal NAA, typically, 0.3 ng for Sb, 0.7 ng for As, 8 ng for Cd, 0.2 ng for In, 14 ng for I, 5 ng for Mo and 2 ng for U. Silicon, which is usually not reported in conventional NAA results for air filters, was routinely determined at the 60 g level. Accuracy was corroborated by analyzing the certified reference material concurrently.     

Determination of trace elements in petroleum by neutron activation analysis

Instrumental neutron activation analysis (INAA) and Ge(Li) spectrometry have been used to determine Sc, Cr, Fe, Co, Ni, Zn, As, Se, Sb, Eu, Au, Hg, and U in crude petroleum. The technique involves no chemical separations and no pre-concentration of the samples by ashing is necessary, thus avoiding contamination or loss of volatile elements. The estimated detection limits in ppb for the elements are Sc (0.1), Cr (0.16), Fe (400.0), Co (0.6), Ni (1.1), Zn (200.0), As (6.0), Se (23.0), Sb (1.0), Eu (0.58), Au (0.11), Hg (4.3), U (1.5). Precision values ranged from 0.1% to 15% (relative standard deviation). Interferences in the Co and Fe determinations due to fast neutron reactions (n, p) and (n, α) on Ni isotopes are small and are easily corrected. Losses of As, Se, and Hg due to escape of volatile gases during irradiation are negligible     

Routine determination of mercury,arsenic and selenium by radiochemical Neutron Activation Analysis

A method for the determination of mercury, arsenic and selenium by neutron activation analysis is described. Radiochemical separations are performed by selective distillation followed by electrolysis of mercury on gold and precipitation of arsenic and/or selenium by reduction to the elemental form. The chemical yields are 80–90% for mercury and 90–100% for arsenic and selenium. Interference tests have been carried out with reference to those elements most likely to interfere with the analysis. Detection limits for mercury, arsenic and selenium using 0.1 g of sample are 0.2 ng g^–1, 2 ng g^–1 and 3 ng g^–1, resp. Detection limits can be improved using greater sample size and neutron flux density. Results from the analysis of several NBS standard reference materials are given.     

Accumulation and distribution of elements in rice /seed,brand layer,husk/ by neutron activation analysis

Various rice samples /seed, brand layer, husk/ from Vietnam were analyzed for Se, Hg, Cr, Ni, Sc, Rb, Fe, Zn and Co by neutron activation analysis. The concentration values found /seed/ were the following: Se 0.04–0.07 ppm, Hg 0.02–0.07 ppm, Cr 2.13–8.65 ppm, Ni 1.56–4.95 ppm, Sc 0.02–0.06 ppm, Rb 0.84–2.71 ppm, Fe 26.31–96.07 ppm, Zn 10.65–27.39 ppm and Co 0.02–0.15 ppm. The values were reported in ppm /dry weight/. Statistical analysis /t-test, t=0.05/ showed that the content of elements varies between sorts of rice; the content of Rb, Fe, Ni, Cr of rice husk was significantly higher than in rice seed and brand layer.     

A comparative study of trace elements in water from various sources in surrounding areas of Nagpur city (India) by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) has been used for the determination of 27 elements (Ag, Au, Ba, Br, Ce, Co, Cr, Cs, Eu, Fe, Ga, Hg, Hf, K, La, Mn, Na, Sb, Sc, Se Sr, Th, P, Ta, Tb, Zn and Zr) in 15 water samples collected from different sources (reservoirs, well, borewell, sewage tank, river, rain) in and around Nagpur city (central India) including doubly distilled and a sea water sample from Bombay. Sample residues after evaporation were irradiated at a thermal neutron flux of 10¹²–10¹³ n·cm^–2·s^–1 for 10 min, 1d and 1wk and counted using a HPGe detector and an 4k MCA at different intervals. Several environmental standards from NIST (USA), NIES (Japan) and USGS rock were also analysed for quality assurance. Wide variations in elemental concentrations have been observed in water samples from different sources. Most elemental concentrations in drinking water from various sources, are within ISI/WHO limits. Sea water showed very high concentrations of Ba, Cr, Co, Fe, Hg, Sb, Se and Zn. For doubly distilled and rain waters, however, very low elemental concentrations of Ba, Ce, Fe, Sc, Hg, Se, Sr and Th were observed.     

Instrumental neutron activation analysis of high-purity gallium,arsenic, and gallium arsenide

Instrumental neutron activation analysis (INAA) has been applied to obtain useful data on impurity concentrations in ultra-pure materials whose matrix elements are strongly activated and create severe interference for several weeks after irradiation. An analytical procedure has been developed and used to determine Sc, Fe, Co, Zn, Se, Zr, Ag, In, Sn, Sb, Te, and Hg in high-purity gallium, arsenic, and gallium arsenide. Detection limits ranged from 50 ng/g for iron to 0.001 ng/g for scandium. Problems of contamination control, blank level, and standardization are discussed.     

Determination of trace amounts of cadmium, cobalt, chromium, iron, molybdenum, nickel, selenium, titanium, vanadium and zinc in blood and milk by neutron activation analysis

The concentrations of Cd, Co, Cr, Fe, Mo, Ni, Se, Ti, V and Zn in biological fluids, human blood serum and market milk were determined by neutron activation analysis, with enrichment by coprecipitation. The pre-concentration of these trace elements was accomplished by converting the dissolved trace metal ions into their pyrrolidinedithiocarbamate (1-pyrrolidinecarbodithioate) chelates, followed by coprecipitation with a metal carrier such as Ni, Pb or Bi. The coprecipitation was carried out prior to irradiation for the short-lived nuclides (V, Ti and Se) and after irradiation for the other elements. The validity of the method was checked using certified biological reference materials; the concentrations of trace elements found by the proposed method agreed well with the published certified data. The limits of detection for Cd, Co, Cr, Fe, Mo, Ni, Se (obtained through the long-lived isotope 75Se) and Zn under the present experimental conditions were found to be 5, 5, 10, 520, 5, 70, 10 and 150 ng, respectively, for 5 ml of biological liquor. The limits of detection for Ti and V obtained (through their short-lived radionuclides 51Ti and 52V, respectively) were found to be 180 and 1.4 ng, respectively, for 50 ml of market milk, or 70 and 0.7 ng for 1 ml of blood serum.     

A comparison of two separation techniques using NaI(Tl) and Ge(Li) spectrometry for trace element determination in biological materials by neutron activation analysis

A comparison of two group separation techniques using either NaI(Tl) or Ge(Li) spectrometry is presented for trace element determination in biological materials by neutron activation analysis. The capabilities of both procedures are described in terms of detection limits, precision and accuracy for the determination of the elements As, Cd, Co, Cr, Cu, Fe, Hg, Mo, Ni, Sb, Se, Sn, and Zn in various types of biological samples. For this purpose the (standard) reference materials NBS SRM-1577 Bovine Liver, Bowen's Kale, IAEA Pig Kidney H-7 and IAEA Milk Powder A-11 were analyzed. An attempt was also made to minimize blank values for several elements.     

Analysis of toxic trace elements in sea food samples by neutron activation

The aim of this study is to investigate the contents of toxic and essential trace element such as As, Hg, Se and Zn by neutron activation analysis in coastal fishes consumed by the general population of Malaysia. The mean values of the elements analysed expressed in mg/kg fresh weight ranged 1.42–5.61, 0.06–0.42, 4.2–20.6, 0.41–1.28 for As, Hg, Zn and Se, respectively. The maximum permissible limit for As in food was set at 1.0 mg/kg under the Malaysian Food Regulations. Our results showed that consumption of coastal fishes is not permitted under the regulations, while the levels of Hg, Se and Zn were within the permissible limits. The daily dietary intake of As and Hg at 400 g and 30g respectively are still within the tolerance levels.     

Extraction and neutron activation analysis of humic substances

Methods are described for the isolation of humaic substances from a soil samples. The produres and based on extractions with sodium hydroxide or sodium pyrophosphate. Four of the humic samples were dried and then analysed by thermal neutron activation analysis. The humic samples along with three standard rocks were irradiated for 15 hours in a flux of 10¹² n·cm^–2·s^–1. Counting was carried out using both a large volume Ge(Li) detector and a high resolution LEP detertor. Quantitative analysis was based on the known element concentrations in the standard rocks. The elements determined were Sc, Cr, Fe, Co, As, Se, Br, Mo, Sb, La, Ce, Eu, Hf, Ta, Th, and U. concentrations ranged from 0.02 ppm (La) to 7900 ppm (Fe).     

Use of INAA,PGAA, and RNAA to determine 30 elements for certification of an SRM: Tomato Leaves, 157a

Analyses for certification have been made for the determination of 30 elements in the National Institute of Standards and Technology (NIST) Tomato Leaves renewal reference material, SRM 1573a. Three of the analytical techniques used were instrumental neutron activation analysis (INAA), radiochemical neutron activation analysis (RNAA), and prompt gamma activation analysis (PGAA). These techniques provided data on 19 elements by INAA, 10 elements by PGAA, and 7 elements by RNAA, with some overlap between techniques. For example, INAA was able to obtain overall analytical uncerainties (at the 95% confidence level) averaging ±2.2% for major and minor constituents (Ca, Mg, K), ±3.3% for constituents from 1 to 1000 g/g (Na, Fe, Al, Mn, Ba, Zn, Rb, La, Cr), and ±6.4% for elements between 10 and 1000 ng/g (Co, V, Se, Th, Sc, Sb), using sample dry weights of approximately 150 mg. These analyses represent the most extensive use to date of nuclear analytical techniques in the certification of a trace element SRM at NIST.     

Multielemental Analysis of Agroindustrial By-Products Employed in Animal Feeding by INAA

Instrumental neutron activation analysis (INAA) with gamma-ray spectrometry was applied to determine As, Ca, Cd, Cl, Co, Cu, Cr, Fe, Hg, K, Mg, Mn, Mo, Na, Sb, Se and Zn in the Brazilian agroindustrial by-products. These materials are widely used in ruminant feeding. The results obtained were compared with requirement and maximum tolerable concentrations. The general conclusions from the data obtained were: (1) many by-products presented concentrations of some essential elements lower than the requirement concentrations, while in some concentrations of Cr, Fe, Mg and Se exceeded by a little the maximum tolerable concentrations, (2) the elements As, Cd, Hg and Sb, generally considered toxic, showed concentrations lower than maximum tolerable values.     

Characterization of Inorganic Components in Plastic Materials

Plastic products may contain high levels of trace elements, which, upon final incineration, may affect the environment. In the case of packing material, may affect food quality. In this work, instrumental neutron activation analysis was applied to the determination of As, Ba, Br, Cd, Co, Cr, Fe, Sb, Sc, Se, Ti and Zn in plastic materials originated from household and hospital wastes. Toxic elements such as Cd and Sb were found at the levels of mg·kg^–1 in some food containers and also high levels of Ti were found in opaque packages. The accuracy and the precision of results were also evaluated by interlaboratory comparison.     

Radiochemical activation analysis of arsenic,selenium and antimony in biological samples

A method for the neutron activation analysis of arsenic, selenium and antimony has been developed. A radiochemical separation is performed by distillation followed by precipitation of the individual elements. Selenium and arsenic are precipitated by reduction to the elemental form while antimony is precipitated as sulfide. The chemical yields and detection limits using 0.5 g samples are the following: As 90–100%, 0.4 ppb, Se 80–100%, 8 ppb and Sb 50–70%, 0.2 ppb. Results from the analysis of nine international biological standard samples are given.     

Instrumental neutron activation analysis of sediment reference materials using the k0-standardization method

An instrumental neutron activation analysis technique has been developed for the determination of As, Au, Ba, Co, Cr, Fe, Hf, Sb, Ta, Th, U, W and Zn in large (10–15 g) geological samples using in-pool irradiation with a SLOWPOKE-2 reactor. The technique allows for the simultaneous irradiation of multiple samples using a neutron flux of between 4·10¹³ and 8·10¹³ n·m^–2·s^–1. The detection limits obtained using the analytical methodology described in this paper are acceptable for exploration geochemistry and the technique has been used to analyze samples collected as part of a metallic minerals survey of Jamaica.     

Instrumental neutron activation analysis of blood serum

Instrumental neutron activation analysis has been used to determine 15 trace elements in twelve blood serum samples taken from healthy students at Bilkent University in Ankara. The method allowed the determination of Sc, Cr, Mn, Fe, Co, Zn, Se, Rb, Cs, Ce, Eu, Tb, Hf, Ta and Hg, which occur at the g.ml^–1 to ng.ml^–1 levels. There are no values reported for Tb, Hf, Ce, Eu and Ta before. The other results are compared with the values reported in the literature. Most are in the range of the reported values except for Fe, Zn, Se and Cs.     

Availability of essential trace elements in medicinal herbs used for diabetes mellitus and their possible correlations

Four plant parts (leaves, roots, fruits and seeds) of twenty samples of sixteen antidiabetic herbs including three commercially marketed capsules have been analyzed for 6 minor (Na, K, Ca, Cl, Mg, and P) and 21 trace (As, Ba, Br, Ce, Co, Cr, Cs, Cu, Eu, Fe, Hg, La, Mn, Rb, Sb, Sc, Se, Sm, Th, V and Zn) elements by instrumental neutron activation analysis (INAA). Further, Ni, Cd and Pb contents were determined by AAS. Elemental data were validated by simultaneously analyzing reference material (RM), MPH-2 Mixed Polish Herbs. Several elements such as Cr and V (1–2 μg/g), Rb (10–40 μg/g), Cs (80–300 ng/g), Se (∼100 ng/g) and Zn (25–60 μg/g) play an important role in diabetes mellitus. Interelemental linear correlations have been observed for Cu vs. Zn (r = 0.89) and Rb vs. Cs (r = 0.87). K/P ratio varies in a narrow range with a mean value of 6.2 ± 1.4. Toxic elements As and Hg were found in <1 μg/g whereas Cd and Pb were in ∼5 μg/g and <10 μg/g, respectively.     

Trace and minor elements in four commercial honey brands

Instrumental neutron activation analysis was used to measure the concentrations of 24 elements in four honey brands commercially available in Austin, Texas (USA). The measured elements (and concentration) were: As, (<30 ng/g); Ba, (<2 g/g); Br, (0.24–0.49 g/g); Ce, (<20 ng/g); Co, (9–180 ng/g); Cr, (37–64 ng/g); Cs, (<3–45 ng/g); Fe, (<4–15.9 g/g); Hf, (<3 ng/g); Hg, (1 ng/g); K, (91–230 g/g); La, (<4 ng/g); Na, (20.3–25.3 g/g); Ni, (0.39–0.77 g/g); Rb, (68–340 ng/g); Sb, (13–61 ng/g); Sc, (<0.3–200 ng/g); Se, (<20 ng/g); Sm, (<9 ng/g); Sr, (<2 ng/g); Th, (<4 ng/g); U, (<30 ng/g); Zn, (3.36–4.61 g/g); and Zr, (<0.5–0.84 g/g). The results obtained were compared to the concentration of the same elements in honey produced or commercially available in Turkey, Mexico, El-Salvador, China, Czechoslovakia and Yugoslavia.