Summary of preparation and homogeneity characterization of ten agricultural food reference materials for elemental composition

Summary Preparation and development has been completed of ten agricultural/food reference materials (RMs): bovine muscle powder, corn starch, hard red spring wheat flour, soft winter wheat flour, whole milk powder, wheat gluten, corn bran, durum wheat flour, whole egg powder and microcrystalline cellulose. Homogeneity tests for 14 elements, Al, Ca, Cd, Co, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were performed by the initiating laboratories by application of precise and reliable analytical methods based on flame atomic absorption spectrometry and graphite furnace atomic absorption spectrometry. An extensive set of analytical results obtained from the interlaboratory cooperative characterization campaign was assessed to provide homogeneity estimates for other elements. Estimates of homogeneity from within-laboratory precision indicated that all materials exhibited acceptable homogeneity for virtually all 29 elements (Al, As, B, Ba, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, Hg, I, K, Mg, Mn, Mo, N, Na, Ni, P, Pb, Rb, S, Se, Sr, V, Zn) for which best estimate concentration values are available. Two thirds of all homogeneity coefficients of variation were below 5%.     

Preparation of the bovine liver 12-02-01 reference material and the certification of element contents from an interlaboratory comparison

Summary The preparation of the bovine liver 12-02-01 reference material, its stabilization and homogeneity testing is presented. Evaluation of an interlaboratory comparison in which 31 laboratories took part using several analytical methods is described. From the results of the intercomparison, the contents of the elements Cd, Cu, Hg, Mn, Pb, Se, and Zn were certified, while for the elements Br, Co, Fe, K, Mo, Na, and Rb, information values were derived. Non-recommended values for the elements Ag, As, Ca, Cl, Cr, Cs, La, Mg, S, Sb, Sn, Sr, and V were also evaluated.Denoted as CZIM-liver in the report [23]     

Findings of national proficiency test exercise for the determination of trace elements in edible mushroom reference material

This paper presents the results of the proficiency test exercise conducted in Pakistan for the determination of trace elements in mushroom reference material. Thirteen laboratories from different organizations of the country submitted trace elemental data on Al, As, Br, Ca, Cd, Ce, Cl, Co, Cr, Cs, Cu, Fe, Hg, K, Li, Mg, Mn, Na, P, Pb, Rb Sc, Si, Sm, Sr, Th, Zn. Results for Al, As, Br, Ca, Cd, Cl, Co, Cr, Cs, Cu, Fe, K, Mg, Mn, Na, Rb Sc, and Zn, in the mushroom material were reported by two or more participating laboratories and could be subjected to statistical evaluation. The original data of these trace elements was subjected to a computer program “Histo Version 2.1” provided by IAEA. The four outlier tests, i.e., Dixon, Grubbs, skewness and kurtosis were applied to the data sets. Consensus (overall) mean values, absolute standard deviation, relative standard deviation, standard error, median and range of values for these elements have been reported at a significance level of 0.05.     

Determination of 24 elements in four algae reference materials by neutron activation analysis and inductively coupled plasma mass spectrometry

Four algae reference materials, IAEA-391, 392, 393 and IAEA-140, prepared by the International Atomic Energy Agency for intercomparison under different preparation conditions were analyzed for 24 elements. Conventional neutron activation analysis (NAA) was used to determine Al, Ca, Cl, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Sb, V and Zn and epithermal NAA using BN and Cd as shielding material for I, Br, As, Ni, Mo and Cd. Inductively coupled plasma mass spectrometry (ICP-MS) as a complementary and comparative method was applied to determine Pb, Sn, Ni, Sr, Rb, As, Co, Cr, Cu, Mn, V, Mo and Zn. Two analytical quality control standard reference materials IAEA-V-10 (hay powder) and IAEA-331 (spinach) were analyzed simultaneously with real samples. The results agree quite well with each other and with the certified values.     

Interlaboratory study of trace and other elements in the iaea powdered human hair reference material,HH-1

A powdered intercomparison material for trace element studies was prepared from human scalp hair and distributed to more than 100 laboratories of which 66 reported results for altogether more than 40 elements. By statistical evaluation of these data certified concentration values were derived for 20 elements, namely As, Au, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, Hg, Mg, Mn, Na, Pb, S, Sb, Se, Sr and Zn. The data also made it possible to compare different methods of analysis and to judge the value of different levels of experience on the part of the analyst concerned; these comparisons are presented here with special reference to the elements As, Cd, Hg, Pb and Sb.     

The complementary use of radioanalytical methods and trace analysis methods for the characterisation of environmental IAEA reference materials

The IAEA laboratories have access to both nuclear analytical methods and conventional instrumental methods for trace analysis for the characterisation of its environmental and biological reference materials. A technical concept integrating the homogeneity data, the recommended test portion mass and the uncertainty on the trace element concentrations is explored using a combination of INAA, XRF, ICP-MS, ICP-AES, and AAS. The above approach is illustrated by selected examples of reference materials currently under evaluation for their trace element content. They include some or all of the following elements Al, As, Br, Ca, Cd, Co, Cr, Cs, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, Ni, Pb, Rb, Se, Sr, Th, U, Zn in environmental biomonitor organisms (lichen, algae) and air dust filters.     

Preparation of the Bovine Kidney and Bovine Muscle reference materials and the certification of element contents from interlaboratory comparisons

Results obtained in interlaboratory comparisons on candidate reference materials Bovine Kidney and Bovine Muscle, in which more than 32 laboratories participated employing atomic spectrometry, electrochemical, and nuclear analytical techniques, have been evaluated using combined statistical and analytical considerations. Certified and/or information values for the elements Br, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, P, Pb, Rb, Se, and Zn have been established. Information on contents of the elements Al, As, Au, Cs, Li, Ni, Sb, Sn, Sr, and V is also presented.     

Elemental content in wheat products of Al-Qusim region, Saudi Arabia using the INAA technique

Wheat is one of the most grown crops in Saudi Arabia. It is grown in various regions of the country. Accurate knowledge of the elemental concentrations in wheat and its products (bran and flour) is of great importance from a nutritional point of view. Wheat samples were obtained from the Al-Qusim region, 300 km northwest of Riyadh, and analyzed. Up to 50 elements (Al, Sb, As, Ba, Br, Cd, Ca, Cs, Cl, Cr, Co, Cu, Ga, Au, Hf, In, I, Ir, Fe, Mg, Mn, Hg, Mo, Ni, K, Rb, Sc, Se, Ag, Na, Sr, Ta, Te, Th, Sn, Ti, W, U, V, Zn, Zr, Ce, Dy, Eu, La, Lu, Nd, Sm, Tb and Yb) were determined in the wheat products. It was observed that the elemental content of bran was much higher than that of white flour.     

Determination of trace elements of some Egyptian crops by instrumental neutron activation,inductively coupled plasma-atomic emission spectrometric and flameless atomic absorption spectrophotometric analysis

Instrumental neutron activation analysis was used for the determination of Al, Br, Ca, Ce, Cl, Co, Cr, Cs, Eu, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc, Se, Ti, Th, V and Zn, ICP-AES for the determination Al, Ag, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, K, Li, Mg, Mn, Na, Ni, P, Sc, Sr, Ti, V and Zn and flameless AAS for the determination of Cd, Hg and Pb in egg plant, potatoes, green pepper (Leguminosae), vegetable marrow (Cucurbitaceae), pears, apple (Rosaceae), castor oil plant (Euphorbiaceae), lettuce (compositae), dill, parsley, coriander (Umbelliferae), and in some soil samples collected from Aswan province.     

A trace element study of commercial infant milk and cereal formulas

Three commercial infant milk formulas, one commercial infant cereal formula and one locally grown cereal used for infant feeding in Nigeria were analyzed for 17 trace elements, viz: Al, As, Br, Ca, Ce, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Rb, Sb, Se and Zn. The commercial milk formulas contain adequate amounts of Ca, Cl, Co, Fe, K, Mg, Mn, Na and Zn, the locally grown cereal contains adequate amounts of Co, K, Mg, Mn and Zn and low in Ca, Cl, Fe and Na while the commercial cereal has adequate amounts of Ca, Cl, Co, K, Mg, Na and Zn. None of the samples analyzed was found to contain any elements up to threshold toxicity limits of concentrations.     

电感耦合等离子体原子发射光谱法(ICP-AES)测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K,Na,Ca,Mg,Zn,Fe,Cu,Mn,Se,Pb,Cd和Cr 12种元素。结果表明:方法简便、快速、准确;山药富含对人体有益的K,Ca,Fe,Mg,Zn,Mn,Se等矿物质元素,其肉质中重金属元素Pb,Cd,Cr含量均未超过国家食品卫生标准。     

白族长寿地区硬果仁中19种元素的测定分析

用电感耦合等离子体发射光谱法（ICP－AES）,对云南省白族长寿区的葵花子仁、麻子仁和核桃仁中的Ca、Mg、P、S、Na、AI、B、Fe、Zn、Cu、Mo、Sr、Mn、Cr、Se、Ge、Cd、Pb、As等19种元素进行了测定分析。结果表明,3种硬果仁中含有丰富的人体必需的Ca、Mg、P、S、Na、Fe、Zn、Mn、Se、Cu、Cr、Sr、Mo等有益元素,且P、Mg、S、Ca、Na、Zn、Mn、Fe、Se的含量较高。这些生命元素在3种硬果仁中的含量存在差异。有害元素Cd、Pb均未检出,核桃仁中As含量较高。硬果仁中富含这些生命元素是该地区老人健康长寿的一个重要原因。     

Application of nondestructive X-ray fluorescence analysis to determine the element composition of medicinal plants

A nondestructive X-ray fluorescence technique has been developed to determine Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, Ba, and Pb in plants. The line element intensities were measured by an S4 Pioneer X-ray sequence spectrometer (Bruker AXS, Germany). The inversely proportional relationship was obtained between the analyte line intensity and mass of the plant, pressed on boric acid backing, for elements with an atomic number 11 < Z < 20. It was found that reduction of plant mass from 6 to 1 g leads to an increase in element determination sensitivity. The detection limits for 1 g of pressed plant were evaluated as μg/g: 5–20 (Na, Mg, Al); 1–4 (Si, P, S, Cl, K, Ca, Ti, Ba, Pb); 0.4-0.8 (Cr, Mn, Fe, Ni, Br, Cu, Zn, Rb and Sr). This technique was applied to determine the element composition of violets of Violaceae family, which are used in medicine.     

Trace elements in Variegated Bolete (Suillus variegatus) fungi

Metallic elements such as Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Rb, Sr, and Zn were determined using ICP-OES in a representative set of fifteen fruiting bodies of the edible fungus Suillus variegatus. Fruiting bodies were collected from unpolluted areas near the village of Lubichowo of the Bory Tucholskie forest complex in northern Poland in 2007?C2008. The caps were richer in Ag, Al, Cd, Cr, Cu, Fe, K,Mg, Ni, Rb, and Zn, and the stipes in Ba, Ca, Mn, Na, Pb, and Sr. Cobalt concentration in the caps and stipes was similar. In the caps, the content of the elements decreased in the order (mg per kg of dry weight): K 29000 ± 3700, Fe 1600 ± 80, Mg 990 ± 110, Rb 320 ± 86, Zn 90 ± 19, Ca 75 ± 34, Al 68 ± 32, Na 40 ± 18, Cu 19 ± 7, Mn 13 ± 7, Cd 1.0 ± 0.5, Ni 0.64 ± 0.32, Ag 0.40 ± 0.20, Cr 0.33 ± 0.06, Pb 0.20 ± 0.17, Ba 0.19 ± 0.11, Sr 0.15 ± 0.09, and Co 0.070 ± 0.050. Apparently, S. variegatus collected from background areas are relatively low in Pb and Cd and so are suitable for human consumption.     

Assessment of atmospheric deposition of metals in Ha Noi using the moss bio-monitoring technique and proton induced X-ray emission

Journal of Radioanalytical and Nuclear Chemistry - The concentration of 22 metal elements including Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, As, Br, Rb, Sr, Zr, Ba and Pb in Barbula...     

微波消解/ICP—AES法测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K、Na、Ca、Mg、Zn、Fe、Cu、Mn、Se、Pb、Cd和Cr等12种元素。结果表明：方法简便、快速、准确度高;四种山药均富含对人体有益的K、Ca、Fe、Mg、Zn、Mn、Se等矿物质元素,其肉质中Pb、Cd、Cr含量均未超过国家食品卫生标准。     

TUNA FISH (T-30) – A new proficiency testing material for the determination of As and Hg in seafood

The quality of the aquatic and marine environment can be monitored by the determination of pollutants in organisms living in this environment. Certified reference materials and well-organised proficiency tests are powerful means of ensuring a constant level of quality and verifying the correct application of standardised methods. The preparation of a tuna fish proficiency testing material for the evaluation of quality of As and Hg monitoring in seafood is described. Preparation and characterisation of the material as well as studies on its homogeneity and stability are described. Concentrations of 3.4 ± 0.2 mg/kg total arsenic and 2.91 ± 0.09 mg/kg total mercury have been determined as target values. Moreover indicative values for some trace elements (Cd, Cu, Ni, Pb, Sr) and some major constituents (Al, Br, C, Ca, Cl, Fe, H, K, Mg, N, Na, P, S, Si, Zn) have also been measured.     

INAA of essential micronutrients in <Emphasis Type="Italic">Terminalia arjuna</Emphasis> bark powder: a versatile heart tonic

Five bark powder samples of Arjuna (Terminalia arjuna) having different origins including two commercial brands were analyzed for 8 minor (Al, Na, K, Mg, Ca, P, Cl, Fe) and 19 trace (As, Ba, Br, Co, Cr, Cs, Cu, Eu, Hg, La, Mn, Rb, Sb, Sc, Sm, Sr, Th, V, Zn) elements by INAA. Also concentrations of Ni, Cd and Pb were determined by AAS and of Sn by ICP-MS. Arjuna bark powder is enriched in Ca (34.1 ± 10.6 mg/g), Mg (5.41 ± 1.93 mg/g), K (5.87 ± 2.18 mg/g), Cl (4.0 ± 2.2 mg/g) and Fe (2.99 ± 1.77 mg/g) with significant amounts of Cr (6.9 ± 4.0 μg/g), Mn (75.5 ± 24.8 μg/g), Sr (114 ± 69 μg/g) and Zn (11.9 ± 8.9 μg/g). Several toxic elements such as As (78.6 ± 19.9 ng/g), Cd (5.60 ± 9.04 μg/g), Hg (69 ± 41 ng/g) and Pb (5.0 ± 3.5 μg/g) were also detected.     

Certified reference material for analytical quality assurance of minor and trace elements in food and related matrixes based on a typical Japanese diet: interlaboratory study

A Certified Reference Material (CRM) was prepared at the National Institute for Environmental Studies (NIES), Japan, in collaboration with the National Institute of Radiological Sciences (NIRS), Japan, for the analytical quality assurance of minor and trace elements in food and related matrixes. The starting material for the CRM was all food served in 29 households in Japan over two 3-day periods in 1997-1998, and thus the CRM represented a typical Japanese diet. All foods (meals, snacks, and beverages) were homogenized, freeze-dried, pulverized, blended, dispensed into 1,100 bottles, and sterilized. The within- and between-bottle homogeneity of the prepared CRM was satisfactory for most of the elements. The concentrations of 14 elements (Na, Mg, K, Ca, Mn, Cu, Zn, As, Se, Sr, Cd, Sn, Ba, and U) were certified based on a collaborative analysis involving NIES, NIRS, and 20 other laboratories. Reference values were given for the concentrations of 12 additional elements (P, Cl, Fe, Co, Ni, Br, Rb, Mo, I, Cs, Pb, and Th). The elements certified and those given reference values include minerals, essential trace elements, contaminant elements, and long-lived radionuclides. Thus, this CRM is of practical value in the quality assurance of element analysis of foods and diets in nutritional, environmental, and radiological research.     

Certified reference materials—Hay Powder (CRM 129) and Rye Grass (CRM 281)—for the quality control of analysis of animal feed

Analyses of nutritive elements are routinely performed in grass or hay for animal feed in order to improve the state of health and growth of domestic animals. To control the quality of such determinations, the Community Bureau of Reference (BCR) so far has produced two certified reference materials: Hay Powder (CRM 129) and Rye Grass (CRM 281). After a careful preparation procedure of the materials, a homogeneity study and a long-term stability study, the contents of the elements Ca, K, Mg, P, S, Zn, I, N and Kjeldahl-N were certified in CRM 129, whereas CRM 281 was certified for As, B, Cd, Cu, Hg, Mn, Mo, Ni, Pb, Sb, Se and Zn. This paper presents the certification exercise and especially concentrates on the elements I, B and Mo as examples of analytical work. Indicative values for Co, Cr, Fe, Cl and Na were also obtained.