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硅酸盐和金属氧化物矿物氧同位素组成的CO_2激光氟化分析 总被引：3，自引：0，他引：3
我室采用MIR 10型CO2 激光器 ,在一种富BrF5的氛围中使激光对硅酸盐和氧化物矿物样品加热形成O2 ,经多次纯化后用 5 的分子筛吸收 ,再直接送至气体质谱仪进行氧同位素比值测定。这个实验流程与传统方法相比的改进不仅在使用激光加热技术及样品的放置上 ,而且在直接采用O2 而不是CO2 进行质谱测定。采用O2 进行直接分析的优点不仅避免了向CO2 转化过程中的潜在同位素分馏 ,而且能够得到样品的δ1 7O值 ,因此为宇宙样品分析提供了可能。CO2 激光氟化技术的优点是所需样品量小 (可低达 1～ 2mg) ,因此能够分析微小岩石区域或单矿物晶体内的氧同位素分布。同时 ,激光可以达到非常高的温度 (>40 0 0K) ,因此能够对某些难熔矿物 (如锆石、蓝晶石、橄榄石等 )进行氧同位素分析。 相似文献
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Malorie Dierick Éric Pili Nelly Assayag Pierre Agrinier 《Geostandards and Geoanalytical Research》2017,41(3):397-409
A new method for accurate determination of oxygen isotopes in uranium oxides encountered in the nuclear fuel cycle was developed using the conventional BrF5 fluorination technique. Laser‐assisted fluorination was tested for comparison. We focused on fine powders of triuranium octoxide (U3O8), uranium dioxide (UO2±x with 0 ≤ x ≤ 0.25), uranium trioxide (UO3.nH2O, with 0.8 ≤ n ≤ 2) and diuranates (M2U2O7.nH2O, with M = NH4, Na or Mg0.5 and 0 ≤ n ≤ 6). Fluorination at room temperature and heating under vacuum at 150 °C are shown to eliminate both adsorbed and structural water from the powder samples. Precision fit for purpose of δ18O values (± 0.3‰, 1s) and oxygen yields (close to 100%) were obtained for U3O8 and UO2 where oxygen is only bound to uranium. A lower precision was observed for UO3.nH2O and M2U2O7.nH2O where oxygen is both present in the structural H2O and bonded to uranium and where the extracted O2(g) can be contaminated by NF3 and NOx compounds. Laser‐assisted fluorination gave shifted δ18O values between +0.8 and +1.4‰ for U3O8, around ?0.8‰ for UO3.nH2O and between ?3.9 and ?4.5‰ for M2U2O7.nH2O (± 0.3‰, 1s) compared with the conventional method. 相似文献
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氟化物固体缓冲剂-交流电弧直读发射光谱法测定化探样品中易挥发与难挥发微量元素 总被引：1，自引：1，他引：0
应用电弧直读发射光谱法测定化探样品,样品无需消解,采用固体进样的方式可以同时测定多个元素。但目前化探分析中常采用的固体缓冲剂(如焦硫酸钾、氟化钠)的电弧温度较低,只能分析银、硼、锡、铅、钼、铜等易挥发元素,而不能分析铬、锰、钛等沸点较高的难挥发性元素。本文通过碱金属控制较低的电弧温度,并利用难挥发元素能在高温条件下与氟离子发生化学反应降低其激发温度,配制了一种以氟化铝、聚三氟氯乙烯等氟化效率较高的化合物为主要成分的固体缓冲剂,通过优化分析线对的选择、曝光时间、电极形状等分析条件,实现了一次制样可同时分析地球化学样品中14种易挥发和难挥发元素。方法检出限为0.016~46.93μg/g,相对标准偏差为4.1%~12.3%,通过国家标准物质验证了准确度,测定值与标准值相符,各项参数都能满足地球化学普查规范要求。本方法分析效率高,在化探分析中具有一定的实用性。 相似文献
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本文发展了一种制备稀有6-脱氧-D-古洛七碳糖的新方法。以4,6-O-苄基-1-脱氧-1-C-烯丙基-(-D-半乳糖苷为原料,经糖醛酸脱羧氟代等关键步骤,以13步30%的总收率合成了正交保护的6-脱氧-D-古洛七碳糖氟苷,为稀有高碳糖的合成提供了新的思路。 相似文献
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硅酸盐矿物氧同位素组成的激光分析 总被引：20，自引：0，他引：20
对于红外激光系统和紫外激光系统 ,由于它们加热样品的反应机理完全不同 ,决定了它们在稳定同位素地球化学分析中的不同使用范围。根据对CO2 激光系统分析地球化学样品的实践 ,发现对结果产生干扰的因素有 :(1)石英的粒径效应 ;(2 )微量样品接收电压过低 ;(3)分子筛的吸附能力 ;(4 )系统中的吸附水 ;(5 ) 14 N19F+ 对δ17O值的影响。由于石英的粒径效应而导致细粒石英 (粒径<2 5 0 μm)的δ18O值偏低 ,可以采用不聚焦激光的快速加热法来解决。由于样品量太少而决定了样品气体接收电压过低 ,导致δ18O值出现系统偏高或偏低 ,可以利用校正曲线对结果进行校正。分子筛吸附性能的下降会产生氧同位素的分馏 ,因此确定分子筛的使用寿命非常重要。系统中的吸附水利用氟化物试剂预氟化来去除 ,重要的是应避免在预氟化的过程中产生大量的HF腐蚀激光系统的BaF2 窗口玻璃并与部分矿物样品发生反应。 相似文献
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Some Observations on the Determination of Gold and the Platinum-Group Elements in Black Shales 总被引：2，自引：0，他引：2
Valentin N. Mitkin Alexander A. Galizky Tamara M. Korda 《Geostandards and Geoanalytical Research》2000,24(2):227-240
This research compares various ways of applying oxidative chemical decomposition to the analysis of gold-bearing black shale ores from the Russian Natalka and Sukhoj Log deposits. This study was conducted as part of the certification program for the Russian candidate black shale reference materials SLG-1 and SCHS-1 and also because of the paucity of data available on the determination of the platinum group elements (PGE) in analogous sample types. We report direct evidence of PGE volatilisation from black shale materials when processed in the presence of oxygen. We also developed a comprehensive analytical scheme for the quantitative determination of PGE in all phases (gaseous and ash) produced during slow combustion of carbonaceous materials in oxygen.
This study has shown that during combustion in oxygen at 600 °C, PGE contained in the Natalka black shale ores are lost as gaseous reaction products. Thus, the volatilized PGE (recovered in traps) account for up to 14% Pt, 40% Pd, 40% Ru and 10 % Ir relative to their total concentrations in a carbonaceous concentrate. It was also established that in the process of combustion, Au quantitatively remains in the ash cake.
In order to avoid the deleterious effects of oxygen on the volatility of the PGE, we propose a new comprehensive sample decomposition method based on the application of fluoroxidants such as BrF3 and KBrF4 . This method was validated using samples of black shale ores and their processing products by comparing our results with those obtained independently using sealed autoclave processing of the same materials. It was shown that PGE in black shale ores and their processing products not only exist in commercially exploitable quantities but that a small proportion of PGE compounds are soluble in alcohol. We propose that in gold-bearing black shale ores, PGE are present as organometallic compounds. 相似文献
This study has shown that during combustion in oxygen at 600 °C, PGE contained in the Natalka black shale ores are lost as gaseous reaction products. Thus, the volatilized PGE (recovered in traps) account for up to 14% Pt, 40% Pd, 40% Ru and 10 % Ir relative to their total concentrations in a carbonaceous concentrate. It was also established that in the process of combustion, Au quantitatively remains in the ash cake.
In order to avoid the deleterious effects of oxygen on the volatility of the PGE, we propose a new comprehensive sample decomposition method based on the application of fluoroxidants such as BrF
7.
Valentina G. Tsimbalist Gennady N. Anoshin Valentin N. Mitkin Ljudmila I. Razvorotneva Nadezhda P. Golovanova 《Geostandards and Geoanalytical Research》2000,24(2):171-182
Some recent experiments on the determination of Au and the platinum-group elements (PGE) in geochemical samples are reviewed. Emphasis is given to the determination of ultra-low levels of PGE concentrations in resistant matrices, including chromites, molybdenites and ultrabasic ores. The problems and features of PGE determination in samples of various chemical composition are considered. For each sample type studied, a series of sample preparation techniques are proposed. These techniques included acid digestion, fusion with sodium peroxide, cold sintering with an oxidizing mixture of Na2 O2 + Na2 CO3 and also oxidizing fluorination with bromine trifluoride. A new approach for preparing geochemical material prior to digestion, based on mechano-chemical activation with simultaneous hyperfine grinding, is proposed and studied. The instrumental determination of PGE contents was carried out directly by AAS from extracted organic phases. It was found that a combination of digestion processes was required to achieve geochemical background levels of Au and PGE concentrations with the following detection limits: Pd, Rh - 1 ng g−1 , Pt, Ru - 10 ng g−1 , Au - 0.2 ng g−1 , Ag - 0.1 ng g−1. The uncertainty in PGE and Au determination in geochemical samples is dependent on metal concentration, and also on their distribution in samples. The total analytical uncertainty of the proposed method is between 15-30%. 相似文献
8.
《Chemie der Erde / Geochemistry》2017,77(1):1-43
A number of distinct methodologies are available for determining the oxygen isotope composition of minerals and rocks, these include laser-assisted fluorination, secondary ion mass spectrometry (SIMS) and UV laser ablation. In this review we focus on laser-assisted fluorination, which currently achieves the highest levels of precision available for oxygen isotope analysis. In particular, we examine how results using this method have furthered our understanding of early-formed differentiated meteorites. Due to its rapid reaction times and low blank levels, laser-assisted fluorination has now largely superseded the conventional externally-heated Ni “bomb” technique for bulk analysis. Unlike UV laser ablation and SIMS analysis, laser-assisted fluorination is not capable of focused spot analysis. While laser fluorination is now a mature technology, further analytical improvements are possible via refinements to the construction of sample chambers, clean-up lines and the use of ultra-high resolution mass spectrometers.High-precision oxygen isotope analysis has proved to be a particularly powerful technique for investigating the formation and evolution of early-formed differentiated asteroids and has provided unique insights into the interrelationships between various groups of achondrites. A clear example of this is seen in samples that lie close to the terrestrial fractionation line (TFL). Based on the data from conventional oxygen isotope analysis, it was suggested that the main-group pallasites, the howardite eucrite diogenite suite (HEDs) and mesosiderites could all be derived from a single common parent body. However, high precision analysis demonstrates that main-group pallasites have a Δ17O composition that is fully resolvable from that of the HEDs and mesosiderites, indicating the involvement of at least two parent bodies. The range of Δ17O values exhibited by an achondrite group provides a useful means of assessing the extent to which their parent body underwent melting and isotopic homogenization. Oxygen isotope analysis can also highlight relationships between ungrouped achondrites and the more well-populated groups. A clear example of this is the proposed link between the evolved GRA 06128/9 meteorites and the brachinites.The evidence from oxygen isotopes, in conjunction with that from other techniques, indicates that we have samples from approximately 110 asteroidal parent bodies (∼60 irons, ∼35 achondrites and stony-iron, and ∼15 chondrites) in our global meteorite collection. However, compared to the likely size of the original protoplanetary asteroid population, this is an extremely low value. In addition, almost all of the differentiated samples (achondrites, stony-iron and irons) are derived from parent bodies that were highly disrupted early in their evolution.High-precision oxygen isotope analysis of achondrites provides some important insights into the origin of mass-independent variation in the early Solar System. In particular, the evidence from various primitive achondrite groups indicates that both the slope 1 (Y&R) and CCAM lines are of primordial significance. Δ17O differences between water ice and silicate-rich solids were probably the initial source of the slope 1 anomaly. These phases most likely acquired their isotopic composition as a result of UV photo-dissociation of CO that took place either in the early solar nebula or precursor giant molecular cloud. Such small-scale isotopic heterogeneities were propagated into larger-sized bodies, such as asteroids and planets, as a result of early Solar System processes, including dehydration, aqueous alteration, melting and collisional interactions.There is increasing evidence that chondritic parent bodies accreted relatively late compared to achondritic asteroids. This may account for the fact that apart from a few notable exceptions’ such as the aubrite-enstatite chondrite association, known chondrite groups could not have been the parents to the main achondrite groups. 相似文献
9.
基于开路热刺激放电电流和电荷等温衰减测量系统地研究了等温结晶化条件对氟化孔洞聚丙烯(PP)膜电荷稳定性的影响.结果表明等温结晶化温度和时间对氟化PP膜的电荷稳定性或电荷陷阱的构造具有显著的影响,即使90 ℃,0.5 h的等温结晶化处理也能显著地加深其电荷陷阱、改善电荷的稳定性.而且随着等温结晶化温度的提高和时间的延长,电荷陷阱进一步被加深、电荷稳定性进一步被改善,如130 ℃,2 h以上的等温结晶化情形.衰减全反射红外分析和宽角X射线衍射分析表明,电荷稳定性的改善归因于PP膜的组成和结构变化. 相似文献
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