Determination of Ga,Ge, Mo,Ag, Cd,In, Sn,Sb, W,Tl and Bi in USGS Whole‐Rock Reference Materials by Standard Addition ICP‐MS

A procedure for determining a wide range of chalcophile and siderophile elements in typical crustal rocks using standard addition and ICP‐SFMS (inductively coupled plasma sector field mass spectrometry) is presented. New results for Ga, Ge, Mo, Ag, Cd, In, Sn, Sb, W, Tl and Bi abundances in USGS whole‐rock reference materials AGV‐2, BHVO‐1, BIR‐1, G‐2, GSP‐1 and W‐2 are reported using this analytical procedure. Intermediate precision of means based on multiple dissolved aliquots of each USGS reference material was 10% RSD or better for Ga, Ge, In and Sn in all, and similarly good for Ag, Cd, Sb, Tl and Bi in most reference materials. Poorer intermediate precision of Mo and W measurements in several reference materials is probably due to higher analytical blanks on these elements and powder heterogeneity due to a sulfide‐related nugget effect in the specific case of Mo in GSP‐1. Results for all elements fell within the range of available published data with the exception of Ag, which yielded systematically higher concentrations than found in the literature for five of the six reference materials, likely reflecting interference from unresolved polyatomic species.     

土壤及河流沉积物中Hg、As、Sb的同时测定

Hg、As、Sb是土壤和河流沉积物的常规测定项目。本文采用新型三通道原子荧光分析仪,建立了同时测定土壤和河流沉积物中这三种元素的新方法。通过优化仪器工作条件,选择合适的样品处置方法,得到Hg、As、Sb的检出限分别为0.03mg/kg、0.009mg/kg和0.03mg/kg,精密度分别为3.5%、7.8%和5.5%,准确度分别为95%～103%、91%～107%(加标回收率)和±6.4%。与现有测定方法相比,本方法的样品消化完全,实验简便,分析速度和准确度高,能充分满足分析要求。     

黑海西北部冷泉碳酸盐岩的沉积岩石学特征及氧化还原条件的稀土元素地球化学示踪

黑海西北部罗马尼亚大陆架(水深120m)和乌克兰陆坡(水深190m)发育冷泉碳酸盐岩结壳。XRD测试表明此结壳主要由高镁方解石和文石组成。结壳中与渗漏系统微生物活动有关的凝块和葡萄状文石等特殊的沉积组构非常发育。冷泉碳酸盐岩酸可溶部分(碳酸盐岩相矿物)的稀土元素含量很低(0.068×10-6~2.817×10-6),稀土元素页岩标准化配分模式显示罗马尼亚大陆架冷泉碳酸盐岩具有明显的Ce负异常,乌克兰陆坡冷泉碳酸盐岩具Ce的正异常,表明它们是分别在氧化和还原环境中沉积的。稀土元素和V、Cd和U等微量元素的含量在泥晶中最高,亮晶中最低,可能反映成岩过程对元素含量有控制作用。     

广东茂名高岭土煅烧实验研究

对茂名高岭土进行煅烧，结合X-射线衍射、扫描电子显微镜分析，得到了茂名高岭土在不同温度点煅烧的性能参数，并确定出其非晶化转变的温度是550℃。同时对煅烧过程中的煅烧温度、恒温时间等影响因素进行探讨，结果表明，在茂名高岭土的煅烧过程中，适当延长恒温时间可降低非晶化转变的温度，缩短恒温时间，则非晶化转变温度升高。     

High-pressure X-ray and Raman study of a ferrian magnesian spodumene

The high-pressure behaviour of a synthetic P2₁/c ferrian magnesian spodumene, ^M2 (Li_0.85Mg_0.09Fe²⁺ _0.06)^M1(Fe³⁺ _0.85Mg_0.15)Si₂O₆, has been investigated using in situ single-crystal X-ray diffraction and Raman spectroscopy. No phase transition has been observed within the pressure range investigated. The isothermal equation of state up to 7 GPa was determined. V₀, K_T0 and K, simultaneously refined with a Murnaghan equation of state, are: V₀= 415.66(7) ų, K_T0=83(1) GPa and K=9.6(6). The magnitudes of the principal unit-strain coefficients were calculated and their ratios 1:2:3=1.00:1.85:2.81 at P=6.83 GPa indicate a very strong anisotropy. Monitoring of the intensity of b-type reflections (h+k= 2n+1) confirms that from room conditions up to 7 GPa the primitive lattice is maintained. Raman spectra have been collected up to 7.4 GPa. No change in the number of observed vibrational modes occurs in the pressure range investigated. At high frequency, the Raman doublet relative to the Si–O–Si vibrations of the two distinct tetrahedral chains is a broad band at room pressure, however, the frequency difference between the two modes increases with increasing pressure.Operating system: Windows NT     

我国几个矿区叶蜡石X射线粉晶衍射研究

对我国几个主要类型叶蜡石矿的叶蜡石做了X射线粉晶衍射研究。从大量实验结果发现,所研究叶蜡石存在单斜晶系和三斜晶系两种多型。单斜晶系(2M);空间群G_(2h)~6-C2/c,a=5.175A,b=8.902A,c=18.673A,β=100.1°,Z=4;三斜晶系(1Tc):空间群P_c,a=5.162A,b=8.965A,c=9.346A,a=91.2°,β=99.96°,γ=89.91°,Z=2。     

Quantification of mineral matter in the Argonne Premium Coals using interactive Rietveld-based X-ray diffraction

The mineral matter in the eight reference North American coal samples of the Argonne Premium Coal series has been investigated on a quantitative basis using X-ray diffraction (XRD) techniques. X-ray diffraction data obtained from electronic low-temperature (oxygen–plasma) ash (LTA) residues, from ashes produced by heating the coals in air at 370°C, and also from the raw coals themselves, were evaluated using an interactive data processing system ( ™) based on Rietveld interpretation methods. The results from the three types of material (LTA, 370°C ash and raw coal) were compared for each sample. This allowed the components present in the raw coals in crystalline form to be recognised separately from mineral artifacts produced, particularly in the low-rank coals, from interaction of organically associated elements (Ca, S, etc.) during the two ashing processes.After the allowance for the production of any artifacts, the quantitative mineral assemblages identified from XRD of the raw coals were found to be consistent, even for coals having a relatively low ash percentage (around 5%), with the results obtained from the respective mineral concentrates prepared by the ashing methods. The effects of heating the coal to 370°C could also be distinguished, relative to the raw coal or the LTA, through changes in components such as pyrite and the clay minerals.Although some areas of uncertainty exist, particularly with magnesium in the low-rank coals, the calculated chemical compositions of the coal ash derived from the mineral mixtures identified for each coal were also found to be consistent with the results of direct chemical analysis of the respective coal ash materials.     

多接收器电感耦合等离子体质谱法测定镉标准溶液中镉的同位素组成

建立了多接收器电感耦合等离子体质谱仪对Cd标准溶液同位素组成进行分析的实验方法。仪器的质量分馏校正采用Standard-Sample Bracketing法。实验结果用δ114/110Cd来表达。在此研究基础上,以SPEX Cd标准溶液为参考标准,对国外4种Cd标准溶液进行了测定。结果表明,实验测定的精度在0.07‰~0.13‰(δ114/110Cd),与目前文献报道的结果具有相似的精度。以最新SPEX Cd标准样品(δ114/110Cd=0)为基准,计算的δ114/110CdJMC、δ114/110CdSPEX-1、δ114/110CdBAM1012和δ114/110CdM櫣nster的值分别为0.55‰、0.56‰、-0.65‰和5.14‰,说明不同批次SPEX标准溶液的Cd同位素组成是明显不同的,最新的SPEX Cd标准溶液与SPEX-1 Cd的δ114/110Cd值存在着0.56‰的差别。将以SPEX Cd为参考标准的δ114/110CdBAM1012和δ114/110CdM櫣nster转化为以SPEX-1或JMC为参考标准后,得到的结果与文献报道的结果在误差范围内一致。     

腐殖酸三维荧光光谱特性研究

腐殖质的荧光特性被广泛用来解析其在各种天然环境中的来源及分布.由于荧光光谱分析具有灵敏度高,选择性好,且不破坏样品结构的优点,非常适合用来研究腐殖质的结构和官能团等特征.利用三维荧光激发-发射光谱研究了 Fluka腐殖酸的荧光光谱特性,结果显示,离子强度(0～0.05 mol/L KClO4)对 Fluka腐殖酸的三维荧光光谱特性影响非常小,而腐殖酸的浓度(5～100 mg/L)和溶液 pH(2～12)对其三维荧光光谱特性影响显著.当腐殖酸浓度增大时,荧光峰出现明显红移现象.荧光强度一般随着 pH的升高而增大,当 pH大于 10后呈下降趋势,我们从垃圾渗滤液溶解有机质的实验结果中也得到相同结论;在浓度为 50 mg/L和 100 mg/L的 Fluka腐殖酸中,荧光峰 B(fulvic-like)的荧光强度却在 pH=5.0左右时达到最大值,与前人报道的土壤富里酸的行为一致,质子化常数 lgK′ HL分别为 3.57和 3.13,与二羧基化合物接近,说明荧光峰 B可能与 Fluka腐殖酸结构中的羧基有关;荧光峰 A与荧光峰 B的荧光强度比值 r(A/B)在 0.61～2.59之间,并且在 pH=2～11范围内, r(A/B)与 pH具有较好的线性相关关系,表明荧光峰 A和荧光峰 B随着 pH值的改变有着相同的变化趋势.     

糜棱岩化过程中绿泥石多型与结晶度的演变--以郯庐断裂带南段为例

摘要：根据郯庐断裂带南段韧性剪切带糜棱岩中同构造矿物组合、黑云母的存在以及长石的变形行为，推测其变形．变质温度为400一450oC。bo值分析表明．这些糜棱岩是在低压环境下形成的。在流体作用下。糜棱岩中的绿泥石既可以交代其它矿物而形成，也可以直接从流体中结晶形成。交代其它矿物所形成的绿泥石为Ⅱ型绿泥石，其结晶度值介于0．21^。一0．23^。20．与温度具有较好的对应关系。直接从流体中结晶而产生的绿泥石初始时刻为工型．其结晶度值介于0．236^。-0．341^。20之间，多屑于近变带范畴。其指示温度要低于实际所经历的环境温度。由于糜棱岩化过程中工型绿泥石的不断产生以及工型绿泥石向Ⅱ型绿泥石转化的不充分。导致了在400以上仍然出现工型绿泥石与Ⅱ型绿泥石混合的现象．并且实测的结晶度是不同时刻形成的、具不同结晶度的绿泥石的混合结晶度。