GOLD IN TWENTY-SIX JAPANESE GEOCHEMICAL REFERENCE SAMPLES

Gold has been determined in 26 geochemical reference samples with graphite furnace AAS after digesting the samples with aqua regia and hydrofluoric acid and extracting gold by methyl isobutyl ketone (MIBK). This method yields clearly higher values than those by the partial attack using aqua regia digestion.     

Flameless atomic-absorption determination of gold in geological materials

Gold in geologic material is dissolved using a solution of hydrobromic acid and bromine, extracted with methyl isobutyl ketone, and determined using an atomic-absorption spectrophotometer equipped with a graphite furnace atomizer. A comparison of results obtained by this flameless atomic-absorption method on U.S. Geological Survey reference rocks and geochemical samples with reported values and with results obtained by flame atomic-absorption shows that reasonable accuracy is achieved with improved precision. The sensitivity, accuracy, and precision of the method allows acquisition of data on the distribution of gold at or below its crustal abundance.     

Determination of Silver in Seventy-Three Geochemical Reference Samples by Atomic Absorption Spectrometry

The silver content of seventy-three geochemical reference samples has been determined by atomic absorption spectrometry using an air-acetylene flame or a graphite furnace atomizer, after extraction of silver as iodide with methyl isobutyl ketone (MIBK). A comparison with published data shows clearly the need for much more data on most reference samples.     

碘化物萃取原子吸收分光光度法连续测定矿石中的锑和铋

矿石中的锑、铋通常是利用其与碘离子分别生成黄绿色的碘化锑络阴离子SbI_4-、黄色的碘化铋络阴离子BiI_4-而进行比色测定。由于锑、铋在分析化学性质上的差异,试样的分解方法,显色条件亦有所不同,故往往是分别取样测定,有分析周期过长的缺点。利用碘化物萃取原子吸收分光光度法测定铋,已应用于矿石及铁合金中。Luke研究了在含碘化物的5％盐酸介质中,用甲基异丁基酮(MIBK)可定量萃取锑、铋等金属元素。Headrige制定了在     

Fractional Determination of Gold in Twenty Six Geological Reference Materials by Sequential Extraction with Graphite Furnace Atomic Absorption Spectrometry

A method is described to estimate the chemical form of gold (Au) in a variety of geological reference samples, combining a sequential extraction scheme with graphite furnace atomic absorption spectrometry, after extraction of Au as iodide or chloride with methyl isobutyl ketone. The fractions dissolved by sequential extraction are empirically defined as the exchangeable, amorphous, metallic, aqua regia-soluble and residual fractions. The amounts of Au in the amorphous fraction have been derived mainly from oxide or amorphous phases, and the chemical forms of Au are considered to be mostly amorphous and partly metallic. The metallic fraction of Au is likely to exist as submicroscopic grains of native metal which are relatively free from the rock-forming minerals, whereas the aqua regia-soluble or residual fraction of Au may be bound more intimately perhaps as inclusions or solid solutions of either native metal or electrum in most cases. Satisfactory agreement was observed between the sum of the Au values from exchangeable to residual fractions and the reported total Au values, except for a few samples which contained a large amount of reducing materials. Analytical results of Au for twenty six geological reference materials are tabulated, and geochemical and mineralogical features are discussed.     

溶剂萃取—苯芴酮石墨炉原子吸收法连续测定岩石矿物中锗,铟,镓

甲基异丁基甲酮(MIBK)—苯芴酮同时萃取,利用自制的简易石墨炉平台,以镍和钒作基体改进剂测定锗、铟和镓。方法简便、快速,适合于岩石矿物中锗、铟、镓的连续测定。     

Rapid colorimetric determination of phosphorus in geochemical survey samples

A colorimetric method for the determination of phosphorus in batches of geochemical survey samples is described. The powdered material is digested with a nitric-perchloric acid mixture, excess of acid is evaporated off and the residue is leached with water. Aliquots of the leachate are treated with vanadomolybdate reagent and the yellow phosphorus complex is extracted into isobutyl methyl ketone. The colour in the organic phase, which is stable for many days, is matched against a series of similarly prepared standards. Iron, other coloured ions, and titanium do not interfere. Standard deviations of ±0.02% about a mean value of 0.20% P₂ O₅ and ±0.4% about a mean of 11.6% P₂ O₅ were obtained. At least 40 powdered samples may be analysed per working day per person.     

电感耦合等离子体发射光谱法和火焰原子吸收光谱法连续测定化探样品中12个元素

建立了地质化探样品中不同含量和检出限要求的12个元素的连续测定方法。样品经一次取样,用盐酸-氢氟酸-硝酸-高氯酸溶样,电感耦合等离子体发射光谱法测定铜、铅、锌、钴、镍、镉、锶、钡、钒、锰后,加碘化钾-甲基异丁基甲酮萃取分离,火焰原子吸收光谱法测定银、镉。银、镉的相对标准偏差(RSD,n=12)分别为6.5%、4.7%。与现行分析方法相比,建立的方法灵敏度和精密度高、准确度好,降低了生产成本,缩短了检测时间,尤其适合大量化探样品的测定。     

Modeling of air stripping from volatile organic compounds in biological treatment processes

The removal of volatile organic compounds from biological treatment processes occurs through several mechanisms. These include biodegradation, adsorption onto solids, and air stripping or volatilization to the atmosphere. Volatilization results in fugitive emissions to the atmosphere, which is largely uncontrolled. Recent regulations have called for increased evaluation and control of inadvertent volatile organic compounds emissions from treatment processes. The use oxygen as a parallel volatile compound is extremely useful for prediction of volatile organic compounds removal by air stripping. In this study, the simultaneous biodegradation and air stripping of volatile organic compounds, based on steady state mass balance are examined and a general approach to estimating the dominant removal mechanism is developed. A Monte Carlo simulation technique was used to estimate air stripping over a wide range of operating conditions. Several volatile organic compounds were selected for this study. The results showed the values drived from the model correspond with the experimental data for benzene, toluene, methylene chloride, trichloroethylene, and methyl isobutyl ketone.     

Effects of surface forces and film elasticity on foam stability

The thin film pressure balance (TFPB) technique was used to determine the surface forces in foam films stabilized with flotation frothers such as n-pentanol, n-octanol, methyl isobutyl carbinol (MIBC), and polypropylene glycol (PPG). The results were compared with the foam stabilities measured experimentally and the film elasticities calculated using a model developed by Wang and Yoon [Wang, L., Yoon, R.-H., 2006a. Role of hydrophobic force in the thinning of foam films containing a nonionic surfactant. Colloids Surfaces A: Physicochem. Eng. Aspects, 282–283, 84–91.]. It was found that foam stabilities are controlled by both film elasticity and disjoining pressure, the relative contributions from each changing with frother type and concentration. At relatively low concentrations, frother dampens the hydrophobic force, an attractive component of the disjoining pressure, that destabilizes foams. At higher concentrations, elasticity plays a more important role in stabilizing foams.     

Hydrodynamics and scale up in Rushton turbine flotation cells: Part 1 — Cell hydrodynamics

The effect of operating parameters on the hydrodynamics of three geometrically similar Rushton turbine flotation cells with volumes of 2.25, 10 and 50 dm³ was determined. The operating parameters investigated were superficial gas velocity (J_g), impeller rotational speed (N), and frother (methyl isobutyl carbinol, MIBC) concentration.     

纸色谱—硫代米蚩酮目视比色法测定岩矿中微量金

岩矿中微量金的测定,一般采用炭粉吸附、萃取、离子交换等方法分离后,用原子吸收光度法或孔雀绿、硫代米蚩酮萃取分光光度法测定。硫代米蚩酮—异戍醇(或正丁醇)萃取比色法灵敏度较高,但稳定性差,手续烦琐,不易掌握。我们试验用纸色谱分离直接在色谱纸上用硫代米蚩酮显色目视比     

Determination of Indium and Tellurium in Fifty Nine Geological Reference Materials by Solvent Extraction and Graphite Furnace Atomic Absorption Spectrometry

The indium (In) and tellurium (Te) contents of fifty nine geological reference materials, issued by several reference material producers (USGS, CRPG, ANRT, GIT-IWG and GSJ) have been determined by graphite furnace atomic absorption spectrometry, after aqua regia and HF digestion, and extraction of iodide complexes with trioctylmethylammonium (TOMA) - metyl isobutyl ketone (MIBK). Although the interferences from most elements can be minimised by the addition of palladium solution as the matrix modifier, large concentrations of Bi, Cu, Pb or Sn suppress the absorbance of In and/or Te. Samples for analysis were therefore restricted to those in which the concentrations of these interfering elements did not cause a significant interference. The limit of detection was 0.2 ng g⁻¹ In and Te for 1 g test portions. The agreement between the reported results and published data is satisfactory.     

Improved stepwise solvent extraction scheme for geochemical trace analysis using flame atomic absorption

A solvent extraction, flame atomic absorption analytical scheme is reported for the elements Au, Tl, Sb, Ga, Mo, Cu, Ni, Co, Ag, Bi, Cd, Pb, Zn and Mn in geological materials. Results are quoted for NIM standard rocks and for USGS reference samples, and are compared with published values; practical detection limits are generally better than 0.2 ppm. A stepwise solvent extraction and preconcentration process is utilised (chloro complexes, diethyldithiocarbamate and 8-hydroxyquinoline chelates are used with methyl isobutyl ketone and $\text{n-}\text{butyl}$ acetate as solvents) which allows the reproducible isolation of groups of elements which generally occur at similar concentrations geologically. Analytical accuracy is maintained by the chemical elimination, within each step, of other chelate-forming elements present at higher concentrations which would cause spectral interferences during the atomic absorption measurements. The complete stepwise process is reported together with elemental partition data which covers a range of aqueous ionic conditions.     

Gold Dissolution in Dry Salt Melts in the Presence of SiO<Subscript>2</Subscript> as a Function of Р(O<Subscript>2</Subscript>)

The solubility of gold was measured in dry NaCl salt melt at 860°С in closed systems with SiO₂ (silica glass). The reactions do not occur in a closed system without oxidizer. Reaction of SiO₂ with salt in the presence of an oxidizer (KClO₄) results in the formation of water-soluble sodium silicates (a mixture of meta-, ortho-, and pyrosilicates). Gold mobilization by a salt melt is limited by the diffusion of Na in SiO₂. In a closed system with the addition of a strong oxidizer (dry KClO₄ salt), the solubility of gold increase with increasing amount of KClO₄ and the saturation level is estimated to be ~3 wt % Au. For ampoule configurations used in our experiments, 5.5 g of gold dissolved per 1 g of KClO₄. Only cheap, non-toxic reagents were used in our model experiments on gold dissolution in a salt melt, which did not require elevated pressures. The solubility of 30 g Au per 1 kg NaCl will eliminate geochemical problems associated with the compact leaching of gold ores using cyanide.     

Preparation and Certification of High-Grade Gold Ore Reference Materials (GAu 19-22)

Two types of gold deposit with both good homogeneity and a high-grade of gold were selected to prepare four gold ore reference materials (GAu-19,GAu-20,GAu-21 and GAu-22) by the Institute of Geophysical and Geochemical Exploration (IGGE),China.Seven laboratories participated in the certification programme. Volumetric methods for GAu19-21 and atomic absorption spectrometry for GAu-22 were used for the homogeneity testing,the coefficient of variation being found to be less than 3%.After sample digestion and preconcentration,the samples were analysed by flame atomic absorption spectrometry (AAS),colorimetry,neutron activation analysis (NAA)and volumetric analysis. The certified values for the gold concentration in GAu19-22 are 18.3 μg g -1, 32.3 μg g -1, 53.0 μg g -1 and 5.72 μg g -1,respectively.     

Vertical transport of steroid alcohols and ketones measured in a sediment trap experiment in the equatorial Atlantic Ocean

The vertical flux and free steroid alcohol (sterol) and ketone composition of particulate material was determined using sediment traps deployed at 389, 988, 3755 and 5068 m at a station in the equatorial North Atlantic, PARFLUX E. Cholest-5-en-3β-ol (cholesterol) was found to be the dominant sterol in all the traps. This compound had a maximum flux at 988 m, accounting for more than 90% of the sterols at this depth. Inputs from mesopelagic Zooplankton populations living in or migrating to depths between the 389 and 988 m traps appear to be responsible for this distribution. The deeper two traps exhibited an increased flux of phytosterols relative to cholesterol, probably due to (a) the incorporation of labile phytoplankton remains in fecal pellets and rapid transport into the deep sea and (b) differential dissolution of heterogeneous large particles. A maximum of 5–22% of the sterols produced in the euphotic zone were present in the 389 m trap. This value drops to less than 1% for the 5068 m trap, 200 m above the sediment surface.In general steroid ketone fluxes gradually decreased with depth. Δ4-Stenones were found in greater abundance than their saturated counterparts. Cholest-4-en-3-one was the major steroid ketone detected in all the traps. A five-fold increase with depth in the cholest-4-en-3-one to cholesterol ratio is most likely due to microbial oxidation of sterols to steroid ketones, or higher Δ4-stenone inputs relative to sterols from organisms.     

A rapid, partial leach and organic separation for the sensitive determination of Ag, Bi, Cd, Cu, Mo, Pb, Sb, and Zn in surface geologic materials by flame atomic absorption

A solution of dilute hydrochloric acid, ascorbic acid, and potassium iodide has been found to dissolve weakly bound metals in soils, stream sediments, and oxidized rocks. Silver, Bi, Cd, Cu, Mo, Pb, Sb, and Zn are selectively extracted from this solution by a mixture of Aliquat 336 (tricaprylyl methyl ammonium chloride) and MIBK (methyl isobutyl ketone). Because potentially interfering major and minor elements do not extract, the organic separation allows interference-free determinations of Ag and Cd to the 0.05 ppm level, Mo, Cu, and Zn to 0.5 ppm, and Bi, Pb, and Sb to 1 ppm in the sample using flame atomic absorption spectroscopy. The analytical absorbance values of the organic solution used in the proposed method are generally enhanced more than threefold as compared to aqueous solutions, due to more efficient atomization and burning characteristics. The leaching and extraction procedures are extremely rapid; as many as 100 samples may be analyzed per day, yielding 800 determinations, and the technique is adaptable to field use.The proposed method was compared to total digestion methods for geochemical reference samples as well as soils and stream sediments from mineralized and unmineralized areas. The partial leach showed better anomaly contrasts than did total digestions. Because the proposed method is very rapid and is sensitive to pathfinder elements for several types of ore deposits, it should be useful for reconnaissance surveys for concealed deposits.     

微量稀土矿物分析

稀土矿物的种类很多,有磷酸盐,氟碳酸盐,钛铌钽酸盐,硅酸盐及钛硅酸盐等。其中以稀土的磷酸盐和稀土的氟碳酸盐分布最广泛,其次如稀土的钛铌钽酸盐,在矿体也有较广泛的分布。上述矿物均为重要的稀     

煤和泥岩不同温度条件下非烃中咔唑类化合物的演化特征

在密闭体系中,200～450℃的条件下进行了煤和泥岩加水的模拟实验,分析了实验产物非烃中咔唑类化合物的演化特征,并讨论了不同温度条件下非烃中咔唑类化合物的演化的机理.实验结果表明,非烃中咔唑类化合物是沉积有机质成岩过程的产物,其含量和组成受有机质成熟度影响较大.该研究结果不仅加深了对非烃中咔唑类化合物演化机理的认识,而...