Neutron activation analysis of 35 elements in Chinese standard rocks (GSR) and soils (GSS) using the SLOWPOKE reactor

Concentrations of 35 elements in Chinese Standard Rocks (GSR-1 to GSR-3) and Soils (GSS-1 to GSS-8) have been measured with INAA using the SLOWPOKE reactor. At the same time, the U. S. NBS reference standards: SRM-1632a (Bituminous Coal), SRM-1633a (Coal Fly Ash) and SRM-1646 (Estuarine Sediment) were also analyzed in order to cross-check the accuracy of this method. The results obtained indicate that the reproducibility of the method is satisfactory for most of the elements, namely the precision in general, is better than ±10%. Comparison of our values for NBS SRM-1632a, 1633a and 1646 with the certified values of NBS or with values cited in the literature indicates good agreement. The results were found to be accurate within ±10% error of the established results.     

Determination of 34 elements in Chinese geochemical standard reference materials by instrumental neutron activation analysis

Thirty four elements (Al, As, Ba, Br, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Gd, Hf, Ho, K, La, Lu, Mg, Mn, Na, Nd, Rb, Sb, Sc, Sm, Ta, Tb, Th, Ti, U, V, W, Yb) were determined by instrumental neutron activation analysis in the second set of Chinese geochemical standard reference materials (sediments from GSD-9 to GSD-12, soils from GSS-1 to GSS-8, rocks from GSR-1 to GSR-6) using both thermal and epithermal irradiations. Irradiation schemes designed to utilise short, medium and long-lived nuclides were employed in order to analyse major, minor and trace elements with different half-lives. The gamma-ray spectra were measured by Ge(Li) and HP(Ge) detectors. Relevant nuclear data and possible interferences are listed, and analytical results are presented and discussed.     

GF-AAS法和HG-AFS法测定土壤中铅的分析方法比较

为验证土壤中铅的氢化物发生原子荧光光谱法(HG-AFS)的有效性,对3种土壤标准样品(GSS-2,GSS-3及GSS-7)进行测定,同时用国家标准方法GB/T 17141—1997[石墨炉原子吸收光谱法(GF-AAS)]进行比较测定。试验结果表明:两种方法的测定结果均与认定值一致。在精密度、回收率及检出限等方面,HG-AFS法均达到与GF-AAS法相当的水平。但HG-AFS法具有操作简单、分析快速等优势。     

电感耦合等离子体质谱(ICP-MS)法与氢化物发生-原子吸收光谱(HG-AAS)法测定土壤中硒含量的对比研究

基于氢化物发生器与原子吸收光谱联用(HG-AAS),测定土壤样品中硒的含量,并与电感耦合等离子体质谱(ICP-MS)法测定值进行了对比。在两种仪器的最佳工作条件下,测定土壤硒的含量,实验结果表明:ICP-MS法和HG-AAS法对土壤硒含量测定的线性范围分别为0.85~100.00μg/L和0.08~16.00μg/L,检出限分别为0.25μg/L和0.02μg/L,精密度分别为1.3%和2.1%;用加标回收实验和测定国家标准土壤样品(GSS-7)对这两种方法的准确性进行了验证,ICP-MS法和HG-AAS法的加标回收率分别为96.7%~99.4%和94.9%~99.5%,GSS-7标准土样的结果均在标准值范围内,说明这两种测定土壤中硒含量的方法是准确可靠的。HG-AAS法测定线性范围窄,部分样品需要稀释,而且氢化物发生系统是手动进样,导致操作复杂,分析周期长;ICP-MS法仪器测定快速,但是仪器昂贵。     

Cold ultrasonic acid extraction of copper, lead and zinc from soil samples

A cold ultrasonic acid method for extracting Pb, Cu and Zn from soil samples has been studied. This work focused on studying the experimental condition for extrating trace metals from soil samples at ambient temperature (≈25 °C) using Syrian soil samples; the same conditions were applied to reference soil samples(SL-1, Soil-7, SDM, and BCR-32). A short exposure time (4 h), and 2 ml of concentrated hydrochloric acid were found to be best. Under the applied conditions Pb, Cu and Zn were quantitavely extracted, while Sr, Mn, Fe, Al, Cr, Co, and Ni were partialy extracted. The advantages of the cold ultrasonic extraction method are as follows: it is selective, it is matrix free, the extraction time is short, the amounts of consumed chemicals are small, the by-products of the process are negligible and it is environmentally clean, since no fume emissions are emitted. The only disadvantage is that it is not a real total digestion method. Comparable results for the proposed ultrasound method and the hot-plate acid digestion method for Cu, Pb and Zn in certified refrence soil samples(SL-1, SDM, Soil-7, BCR-32, Soil-6) and some Syrian soil samples are obtained.     

微波消解-电感耦合等离子体质谱法测定土壤中微量稀土元素

研究了电感耦合等离子体质谱（ＩＣＰ－ＭＳ）测定土壤中微量稀土元素（ＲＥＥｓ）的方法。详细讨论了测定稀土元素的质谱干扰及基体的抑制效应,采用高斯消除法可有效地校正质谱干扰,内标法可以补偿基体的抑制效应。     

Neutron activation analysis of reference materials by the k0-standardization and relative methods

Instrumental neutron activation analysis with the k₀-standardization method was applied to eight geological, environmental and biological reference materials, including leaves, blood, fish, sediments, soil and limestone. To a first approximation, the results were normally distributed around the certified values with a standard deviation of 10%. Results obtained by using the relative method based on well characterized multi-element standards for IAEA CRM Soil-7 are reported.     

Investigate the capability of INAA absolute method to determine the concentrations of 238U and 232Th in rock samples

This work aimed to study the capability of INAA absolute method in determining the elemental concentration of ²³⁸U and ²³²Th in the rock samples. The INAA absolute method was implemented in PUSPATI TRIGA Mark II research reactor, Malaysian Nuclear Agency (NM). The accuracy of INAA absolute method was performed by analyzing the IAEA certified reference material (CRM) Soil-7. The analytical results showed the deviations between experimental and certified values were mostly less than 10 % with Z-score in most cases less than 1. In general, the results of analysed CRM Soil-7 show a good agreement between certified and experimental results which mean that the INAA absolute method can be used accurately for elemental analysis of uranium and thorium in various types of samples. The concentration of ²³⁸U and ²³²Th ranged from 1.77 to 24.25 and 0.88 to 95.50 ppm respectively. The highest value of ²³⁸U and ²³²Th was recorded for granite rock sample G17 of ²³⁸U and sample G9 of ²³²Th, whereas the lower value was 1.77 ppm of ²³⁸U recorded in sandstone rock and 0.88 ppm of ²³²Th for gabbro. Moreover, a comparison of the ²³⁸U and ²³²Th results obtained by the INAA absolute method shows an acceptable level of consistency with those obtained by the INAA relative method.     

测定土壤中重金属元素时前处理方法的改进

建立了一种微波消解前处理技术的半消解法消解样品,采用原子吸收光谱法和原子荧光光谱法同时测定土壤中主要重金属元素铜、锌、镉、砷、汞的方法,检测土壤标准物质GSS-3、GSS-5、GSS-20,结果显示测定均值在标准差允许范围内,相对标准偏差小于8.5%(n=4),是土壤重金属元素快速检测的可选方法。     

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%.     

Extraction Chromatographic Separation of Ree and Y By P507 Containing Resin and Their Icp-Aes Determination In Chinese Soil Standard Samples

Abstract

This paper describes a procedure for the determination of REE and Y in soils by ICP-AES, the optimum conditions for separation of REE and Y from major elements have been investigated by precipitation with sodium hydroxide-triethanolamine and by extraction-chroroatography with P507 containing resin. Results are given for eight Chinese soil standard samples GSS-1 to GSS 8 and compared with recommended values.     

Determination of trace metals in sediment standard reference materials by graphite-furnace atomic absorption spectrometry with a stabilized temperature platform

Trace elements (As, Be, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, V, Zn) in NBS 1645 (river sediments), NBS 1646 (estuarine sediment), MESS-1 and BCSS-1 (marine sediments), IAEA SL-1 (Lake Sediment) and IAEA Soil-5, are determined by graphite furnace atomic absorption spectrometry with the L'vov platform. The samples (ca. 0.25 g) are dissolved in a mixture of nitric, perchloric and hydrofluoric acids in a PTFE bomb. Results based on direct calibration with simple aqueous solutions are in good agreement with those obtained by the method of standard additions and with recommended values. The relative standard deviations are generally 5–10%. Chromium determinations are also evaluated by inductively-coupled plasma/atomic emission spectrometry.     

双通道原子荧光光谱法同时测定土壤中的砷和汞

对现有国标检测方法(GB/T 22105.1-2008和GB/T 22105.2-2008)进行改进,采用王水水浴浸提-双通道原子荧光光谱法同时测定土壤样品中砷、汞的含量。采用土壤国家一级标准物质GSS-3,GSS-8,GSS-9与山西农田土壤样品为试验对象,筛选得到检测砷、汞元素含量最佳实验条件及仪器工作条件。砷、汞的质量浓度分别在0~150μg/L,0~2μg/L范围内与荧光强度成良好的线性关系,线性相关系数均大于0.999,砷、汞的检出限分别为0.021,0.0015 mg/kg。测定结果的相对标准偏差为1.81%~4.64%(n=8),砷、汞的样品加标回收率分别为92.7%~103.0%,82.0%~95.5%。经国家一级标准物质验证,该法检出限、准确度和精密度均满足检测要求。改良后的方法可以同时准确、快速地测定土壤中砷、汞,极大地提高了工作效率,可以更好地适应当前大量的土壤分析工作。     

Assessment of three digestion procedures for Zn contents in Pakistani soil by flame atomic absorption spectrometry

Evaluation of three different digestion procedures for accurate determination of elemental concentration in soils was undertaken. The digestion procedures, two leaching and a total dissolution processes were compared for twenty-one soil samples. The soil standard reference materials (SRMs), IAEA Soil-5 and IAEA Soil-7 were analysed for quality control purposes. Zinc (Zn) was analysed using flame atomic absorption spectrometry (FAAS). Precise analysis was accomplished in the SRM and soil samples, which was better than 4.7% for leaching and total dissolution procedure. Compared with the elemental concentration in soil samples, HF–HClO₄ procedure achieved greater accuracy, where as HNO₃–H₂O₂ and HNO₃–H₂SO₄–HCl procedures were comparable with slight variation in a few samples.     

Rapid multielemental analysis of Chinese reference soils by laser ablation inductively coupled plasma-source mass spectrometry

Summary Laser ablation inductively coupled plasma-source mass spectrometry has been used to determine thirty elements (Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, As, Rb, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Dy, Ho, Yb, Hf, Ta, W, Th, U) in seven Chinese reference soils. The Surrey prototype spectrometer was employed with sample ablation by a free-running ruby laser. Concentrations in the soils (GSS-2 to GSS-8) were calculated from elemental responses and sensitivities derived from another soil in the series, namely GSS-1. Comparisons with previous neutron activation analyses are made. Rapid semiquantitative analyses are proved feasible. About eighty percent of the LA-ICP-MS determined concentrations were within a factor of two of the concentrations measured by INAA, and many were considerably closer than this. Precisions were typically in the range 2–10% RSD, but some were considerably poorer for elements present at trace levels.     

Th,U and trace elements determination in Egyiptian Lake sediments by INAA and laser fluorimetry

A study was undertaken to determine element concentrations in Aswan High Dam Lake sediments. Sediment samples were collected from 40 to 500 km upstream of the dam to follow the sedimentation process and the distribution of Th, U and the trace elements in the lake. INAA was applied for the determination of Sm, Ce, Lu, Th, Cr, Yb, Au, Hf, Ba, Nd, Cs, Tb, Sc, Rb, Fe, Zn, Co, Eu, and Sb, while Laser Fluorimetry was applied for U determination. The accuracy and the reproducibility of the techniques were tested with IAEA standard materials (SL, Soil-7). The U values ranged from 4 ppm to 18 ppm, Th values were between 2 and 10 ppm, and showed a very good correlation with the rare earth elements and Fe. The distribution of most of the elements in the lake follows the same trend as the distribution of the clays in the sediments. Ba showed a negative correlation with most of the elements under investigation.Paper presented at the 3th International Conf. on Nuclear and Radiochemistry (NRC-3), Vienna, 1992.     

Instrumental neutron activation analysis of environmental samples using thek 0-standardization method

The use of thek ₀-standardization method in instrumental neutron activation analysis gives good accuracy and precision. The analysis time can be reduced drastically by employing software for thek ₀-standardization calculations. In this work samples were irradiated in a TRIGA reactor and the gamma spectrum was analysed by Sampo 90 and thek ₀-standardization by the KAYZERO/SOLCOI code (DSM Research). The efficiency measurement and the peak to total ratio at the reference and other geometries were measured and tested for their accuracy by analysing some reference materials. Reference materials such as SRM 1572 (Citrus leaves), SRM 1573 (Tomato leaves), SRM 1575 (Pine needles), IAEA Soil-7 (Soil) and SRM 1646 (Estuarine sediment) were analysed for the major, minor and trace element contents. The results were in good agreement with the certified or literature values. The recently released IAEA 140 (Sea plant homogenates) was also analysed for 28 elements.     

Interacalation of pyridine and its derivatives into crystalline bismuth molybdenum hydrous oxide

The use of thek ₀-standardization method in instrumental neutron activation analysis gives good accuracy and precision. The analysis time can be reduced drastically by employing software for thek ₀-standardization calculations. In this work samples were irradiated in a TRIGA reactor and the gamma spectrum was analysed by Sampo 90 and thek ₀-standardization by the KAYZERO/SOLCOI code (DSM Research). The efficiency measurement and the peak to total ratio at the reference and other geometries were measured and tested for their accuracy by analysing some reference materials. Reference materials such as SRM 1572 (Citrus leaves), SRM 1573 (Tomato leaves), SRM 1575 (Pine needles), IAEA Soil-7 (Soil) and SRM 1646 (Estuarine sediment) were analysed for the major, minor and trace element contents. The results were in good agreement with the certified or literature values. The recently released IAEA 140 (Sea plant homogenates) was also analysed for 28 elements.     

A proposed k0 based methodology for neutron activation analysis of samples of non-standard geometry

An internal mono-standard method has been proposed for multi element analysis. This method gives the relative concentration of the elements in a sample of non-standard shape and size. It utilizes an in-situ relative efficiency calibration and hence, does not need the cumbersome procedures, otherwise required to correct for -attenuation in the sample. To validate this method, the relative concentration of elements in IAEA RM's SL-3 and Soil-7 were analyzed with sample amounts ranging from a few milligrams to grams. The samples were counted in different non-specific geometries. The results are in good agreement with the recommended values, suggesting that this methodology could be applied for the analysis of samples of non-standard size and shape, and in principle, for the analysis of large samples.     

等离子炬-质谱技术测定白菜、萝卜、大豆、土壤中的痕量锰、钴、镍、铜、锌、砷、钼和锶

营养学家们已经确定了锰、钻、镍、铜、锌、砷、钼和锶等10多种人体所必需的痕量元素,它们对于维持人体的健康和长寿起着重要的生理作用。本文首次应用等离子炬-质谱技术测定了白菜、萝卜、大豆和土壤中这八种痕量元素的含量,并报告了它们的测定结果和标准偏差,其中土壤样品的测定值与参考值相比较,经 T 检验,两者之间在统计学上,没有显著性差异。实验证明该方法可对多种痕量元素同时定性、定量分析。操作简便、快速,灵敏度高;方法准确可靠,重现性好。为开展食品卫生学、营养学的研究,提供了更为先进的测试技术。