氢化可的松纯度标准物质的研制

介绍纯度标准物质氢化可的松的研制方法.采用高效液相色谱法对该标准物质进行了定值及均匀性、稳定性检验.该标准物质定值结果为99.5%,扩展不确定度为0.2%,其均匀性和稳定性检验结果表明,该标准物质符合国家一级标准物质的技术要求.     

锰纯度定值及其单元素溶液标准物质的研制

以高纯锰为原料研制锰单元素溶液标准物质。采用电感耦合等离子体质谱法、电感耦合等离子体发射光谱法以及元素分析仪3种方法测定高纯锰中杂质元素的含量,并通过杂质扣除法确定了高纯锰的纯度为(99.95±0.04)%(k=2)。采用重量–容量法制备了锰单元素溶液标准物质,以配制值作为锰单元素溶液标准物质的标准值。对溶液标准物质的均匀性和稳定性进行了检验,其均匀性与稳定性良好。对标准物质的不确定度进行了评定。锰单元素溶液标准物质的浓度值为100μg/mL,相对扩展不确定度为0.8%(k=2)。该标准物质的量值准确,可用于锰元素的分析检测、检测方法评价与仪器校准。     

XRF检验标准物质中痕量元素的匀性

本文讨论了用Ｘ射线荧光光谱检验标准物质中痕量元素的均匀性时，可根据峰和背景强度确定能否用ＸＲＦ进行检验，以及相应于一定精度度要求的浓度下限（可检浓度），并以大米和岩石标准物质为例，计算了Ｃ－的可检浓度。还指出，作为均匀性检验量应采用浓度或净强度，尤其是对于痕量元素，最后说明了样品基体对可检浓度和最小样品量的影响。     

耐辐照玻璃成分分析标准物质的研制

采用高温熔融方法制备了玻璃成分分析标准物质.对标准物质的制备技术、均匀性检验、稳定性考察及定值不确定度进行了分析.研制的耐辐照成分分析标准物质具有良好的均匀性和稳定性,各组分不确定度均小于5％.     

铝锰铁合金标准物质的研制

依据GB/T15000.3—2008、GB/T15000.5—1994、YB/T082—1996和相关ISO导则研制了铝锰铁合金化学分析用标准样品。样品经过加工混匀后,按要求进行粒度实验和均匀性检验。采用Minitab软件进行均匀性数据的正态性检验,然后用方差法进行均匀性检验,各元素F值均小于临界值F0.05,表明被检元素的均匀性良好。由7家有资质的实验室采用多种不同原理,准确、可靠的分析方法协作定值分析,对分析结果进行统计和处理,得到了定值元素的认定值。结果表明该标准物质均匀性和稳定性以及定值准确性均达到国家标准物质的性能指标,符合国家计量技术规范的要求。     

稀土矿石成分分析标准物质的研制

介绍两种稀土矿石成分分析标准物质的研制过程。采用X射线荧光光谱法检验标准物质的均匀性和稳定性，标准物质的均匀性和稳定性良好。由8家具有权威性的测试单位协同定值及对数据进行数理统计，确定了该标准物质的标准值及标准偏差。     

离子色谱仪检定用标准物质研制

介绍离子色谱仪检定用4种成分分析标准物质的制备方法.以高纯氯化钠、碘化钾、亚硝酸钠、碳酸锂为原料,采用重量–容量法分别制备水中氯离子、水中碘离子、水中亚硝酸根离子、水中锂离子4种成分分析标准物质,分别采用F检验法和直线拟合法对标准物质进行均匀性和稳定性检验,并对标准物质的定值不确定度进行了评定.研制的4种标准物质具有较...     

ITO成分分析标准物质的研制

研制3种掺杂铁、铜、铅、锌、钙、镁金属元素的氧化铟锡(ITO)成分分析标准物质。采用溶胶凝胶和共沉淀相结合的方法制备标准物质候选物,用电感耦合等离子体发射光谱法对其进行均匀性、稳定性检验及定值分析。采用8家具有资质的实验室对研制的标准物质进行协作定值,对定值结果的不确定度进行评定。结果表明:研制的ITO成分分析标准物质具有良好的均匀性和稳定性,3种标准物质中氧化锡含量在1%~10%之间,相对扩展不确定度为0.7%~6.6%(k=2);6种掺杂元素含量在0.05%~0.30%之间,相对扩展不确定度为3.4%~11%(k=2)。     

丙酮中除虫脲溶液标准物质研制

采用重量-容量法制备丙酮中除虫脲溶液标准物质。准确称量国家二级标准物质除虫脲溶解到色谱纯丙酮中,通过A级容量瓶定容至500 mL,摇匀后分装到2 mL安瓿瓶内共460瓶,每瓶为1 mL,保持低温迅速封口,配制过程中室温保持在(20±2)℃。采用液相色谱法进行均匀性、稳定性检验和定值结果验证。从样品中随机抽取16瓶进行均匀性检验,经F检验表明,在95%的置信区间范围内该标准物质均匀性良好;采用t检验对标准物质稳定性进行检验,标准物质在12月内稳定性良好。对该标准物质的不确定度进行了评定,研制的丙酮中除虫脲溶液标准物质定值结果为100μg/mL,相对扩展不确定度为2%(k=2)。结果表明,该标准物质均匀性与稳定性良好,量值准确,可用于日常分析检测中的方法评价和仪器校准。     

钛合金光谱分析用标准物质的均匀性检验

介绍钛合金光谱分析用标准物质均匀性检验的抽样、测试、检验及判断方法。钛合金光谱分析用标准物质中碳和铝的均匀性检验结果表明此两种元素在试样中的分布是均匀的。该方法已应用于钛合金光谱分析用标准物质的研制过程中。     

Elemental analysis of dust trapped in air conditioner filters for the assessment of Lahore city’s air quality

A study was undertaken to assess the air quality of Lahore by the elemental analysis of air conditioner (AC) filter dust samples collected from 15 different commercial sites. Samples were prepared using the Leeds Public Analyst Method and were analyzed using instrumental neutron activation analysis (INAA) for up to 31 elements. The elements Al, As, Ba, Ce, Co, Cr, Cs, Fe, Hf, K, La, Lu, Mn, Na, Nd, Rb, Sc, Sm, Sn, Ta, Th, Yb and Zn were detected in all 15 samples whereas the remaining elements have been detected in fewer samples; i.e. Mg, Sb and Tb were detected in 14 samples, Br and V in ten samples, U in nine samples and Ca and Ti in eight samples only. Al, Ca, Fe, K, Mg and Na were determined in all samples at percentage levels. The concentrations of most elements were found to lie around the mean values for the 15 samples studied and were not orders of magnitude different. However the concentrations of Ca, Mg, Sn and Zn were found to be more variable and were found to be dependant on activities such as construction, fruit and vegetable handling, tin plating and transport, respectively.     

Determination of the chemical composition of the South Pole aerosol by instrumental neutron activation analysis

Atmospheric particulate samples were collected at the geographic South pole, using cellulose and polycarbonate filters and cascade impactors. The samples were analysed for 40 elements by instrumental neutron activation analysis. From the filter samples atmospheric concentrations for 33 elements could be obtained. The highest atmospheric concentrations were found for S: 49 ng/standard cubic meter (SCM) of air, Na: 3.3 ng/SCM and Cl: 2.6 ng/SCM. In the cascade impactor samples, only a few elements were observed above blank. For these elements it could be concluded that they are associated for over 80–90% with submicron size paricles.     

INAA of ancient glass beads from Sungai Mas archaeological site,Bujang Valley,Malaysia

The multi-elemental content of sixteen glass beads and eight glass samples from archeological site Sg Mas in Bujang Valley (finding from 5 th to 14 th century) were assayed by neutron activation analysis (NAA). Ten beads differed in colour and eight of them were opaque. Contents of twentyfour elements, which might be present in the samples as a flux, stabilizer, colorants or opacifier were examined. The elements Al, Br, Cl, Co, Cr, Fe, Hf, K, Mn, Na, Sc,Th, Zn and Zr were detectable in all samples. On the other hand, concentration of the elements As, Ba, Ca, Cs, Rb, Sb, Ta, Ti, U, and V were below the detection limit in some samples. The concentration of elements found are discussed in terms of color and/or opacity of the glass bead and glass samples. Although the elemental composition does not fully explain the color and opacity of the studied materials, it can still be used as fingerprint of the glass used for the bead making.     

Analysis of rare-earth elements in soil sample by using laser-ablation ion trap mass spectrometry

Laser-ablation ion trap mass spectrometry (LA-ITMS) is applied for the analysis of rare-earth elements in soil samples. The target elements studied in this work were ytterbium (Yb) and samarium (Sm). The isotopic compositions of these elements were analyzed for standard samples with chip shape, the western phosphate rock sample (NIST SRM-694), and soil samples collected near our laboratory. For metal samples of Sm and Yb, isotopes of these elements as well as oxide forms were clearly identified. For the case of soil samples only a tentative assignment on the mass peaks were performed due to the complicated mass spectra that originated from the oxide forms of various rare-earth elements.     

微波消解-ICP/MS测定烤烟中微量元素含量

以3 mL HNO3和2 mL H2O2的混合消解液对烟草样品进行微波消解,采用电感耦合等离子体质谱测定了烤烟中的Mn、Zn、Cu、Se、N i、Co、Cr、As、Cd、Pb 10种微量元素的含量.结果表明：方法的检出限均低于0.02μg/g,各元素测定的RSD（n=5）均小于3%,样品加标回收率为97.35%-101.30%.方法消耗试剂少,快速准确,适合烟草中多种微量元素的同时测定.     

Elemental composition of dust in an iron foundry as determined by instrumental neutron activation analysis

In the workplace of an iron foundry total and respirable suspended particulate matter was daily collected with a network of stationary filtration systems, with Andersen cascade impactors and with personal samplers. The performances of the different sampling systems are evaluated. All samples were analysed by instrumental neutron activation analysis. More than 30 elements were determined. The composition of the particulate samples is compared to that of the major emission sources. For visualising and interpretation of the data computer programs for contour plotting, classification and clustering of the elements and the samples are applied. On the basis of their distribution and particle size the elements can be divided in a number of groups, for which easily determined elements are proposed as indicator elements. The results allow an estimate of the impact of the major emission sources on the air quality in the entire workroom. Suggestions for representative sampling techniques and locations are made.     

Minor and Trace Element Determination of Food Spices and Pulses of Different Origins by NAA and PAA

INAA, RNAA and IPAA were employed to determine upto 26 trace elements in 32 spices of 18 species and 16 pulses of 8 species originating from different localities. The results are compared with each other and the reported values. The concentration levels, their variations and the correlations of the analysed elements in these samples were also investigated. The variability of concentrations among the samples of different origin are small. The levels and ranges of the concentration are highly variable which are found to be characteristic to each element. High elemental correlations exist in some sets of elements, reflecting characteristics of chemical nature of elements and/or of their physiological functions.     

用ICP-AES法测定首饰金的成分

本文报道采用ICP-AES法直接同时测定首饰金中合金无素及主要杂质元素含量,通过计算求得金含量。确定了仪器的最佳工作条件,进行了干扰试验。方法适用于18k～99.99%成色的首饰金。测定的RSD为<0.01%(对于高纯度金祥n=10)～0.2%(对于10k金样n=10)之间,分析结果表明,方法准确、快速、简便且样品消耗量少。     

Identification of glass and ceramics by X-ray fluorescence analysis with a pyroelectric X-ray generator.

Applications of X-ray fluorescence (XRF) analysis with a pyroelectric X-ray generator are presented. Glass and ceramics were analyzed with this novel X-ray generator to examine its capability for analyzing nonmetallic inorganic material. Although the power of X-ray output was a few orders of magnitude lower than conventional X-ray tubes, many elements such as Si, K, Ca, Ti, Cr, Fe, Zn, Sr, Ba, and Pb were detected in glass and ceramic samples. Light elements such as Na, Mg, and Al were not detected because of the low fluorescence yield and the absorption of fluorescent X-rays in air. The elements detected or the relative peak intensities of the elements were different from each other, and the samples analyzed were identified by the XRF spectrum, notwithstanding the low power of the X-ray output. This novel device showed the sufficient capability for preliminary screening before strict identification of analytes. The pyroelectric X-ray generator can also be used to analyze large samples that cannot be put into ordinary XRF spectrometers because the device has no dimensional limitation of analytes.     

Partitionings and kinetic behaviors of major-to-ultratrace elements between industrial waste incineration fly and bottom ashes as studied by ICP-AES and ICP-MS.

The partitionings of major-to-ultratrace elements between industrial waste incineration fly ash (IWIFA) and industrial waste incineration bottom ash (IWIBA) in industrial waste incinerators were investigated by measuring their concentration distributions, where the incineration ash samples were collected from three different types of industrial waste incinerators. The concentrations of the elements in the incineration ash samples were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). As a result, ca. 40 elements in the concentration range from mg g(-1) to sub-microg g(-1) could be determined in both IWIFA and IWIBA samples. The concentration ratios of CF/CB (CF, concentration in fly ash; CB, concentration in bottom ash) for analyte elements were used to evaluate the partitionings of the elements between fly and bottom ashes. Then, the correlations between the CF/CB values of the elements and the dissociation energies of their monoxides were examined to evaluate the kinetic behaviors of the elements during the incineration processes. It was found that lithophile and siderophile elements, which have a large affinity with oxygen, were almost equally distributed between fly and bottom ashes, regardless of the dissociation energies of their monoxides. On the other hand, chalcophile elements with rather large volatility provided different behaviors; the elements with the smaller dissociation energies of monoxides were more partitioned in fly ashes than those with the larger ones.