拉曼光谱在危地马拉翡翠矿物组成中的应用研究

危地马拉是缅甸之外的另一个翡翠的商业性产地,危地马拉翡翠通常是多种矿物成分的集合体,其矿物组成具有特色,与缅甸翡翠的不同。以危地马拉紫色和灰绿色翡翠为研究对象,通过激光拉曼光谱测试分析,对其结构特征及共生矿物组成特点进行了研究。结果表明,危地马拉翡翠中的主要组成矿物为硬玉,并伴有多种共生矿物。危地马拉翡翠的共生矿物包括五类,其中深色共生矿物为角闪石,白云石,绿辉石和绿泥石,浅色共生矿物为磷灰石。其中角闪石,白云石,绿辉石和绿泥石也是缅甸翡翠中常见的共生矿物,而磷灰石在缅甸翡翠中几乎不可见。     

ICP-AES测定金合金中钆和铍含量

通过ICP-AES测定金合金中Gd和Be量各种相关因素的试验研究,建立了一个准确可靠的测定方法以替代原国标方法,适用于AuAgCuMnGd、AuAgCuGd、AuNiGd、AuBe合金中钆、铍量的测定,测定含量范围为:0.2%-2%.方法加标回收率:Gd为95.58%-99.98%,Be为96.11%-103.33%.方法测定精密度结果:Gd为1.02%.Be为4.05%.     

电位法测定循环水中的氯离子

利用氯离子选择性电极法测定循环水中氯离子含量。该方法以氯离子选择性电极为指示电极,应用校准曲线直接测定循环水中氯离子浓度。实验考察了SO42-、HCO-3、PBTCA、HEDP、DCCNa等循环水中干扰因素及pH、温度等测定条件对测定的影响。该方法测量精度的相对标准偏差RSD为1.8%(n=8);加标回收率在95.0%—104%之间,平均回收率为99.1%,加标回收率相对标准偏差RSD为4.0%(n=5)。     

氢化物发生-原子荧光光谱法同时测定磷酸盐中砷和锑

采用盐酸溶解三聚磷酸钠、磷酸氢钙试样,氢化物发生-原子荧光光谱法同时测定砷和锑,对仪器条件、盐酸、预还原剂、还原剂用量、共存离子干扰进行了试验。方法的检出限砷为6.3ng·g-1,锑为6.8ng·g-1,砷的测定精密度为1.14%—5.42%,回收率为99.4%—103.5%,锑的测定精密度为1.25%—1.77%,回收率为98.0%—101.9%。     

氢化物发生-原子荧光光谱法测定食盐中Pb

盐酸处理食盐试样 ,氢化物发生 -原子荧光光谱法直接测定食盐中铅含量 ,试验了不同的酸及酸度对测定的影响。方法的检出限为 9.92 ng/ g,回收率为 95 .1 %— 1 0 5 .3% ,相对标准偏差为 4 .1 4 %。方法操作简便、快速 ,适用于食盐中铅的测定     

非水溶液滴定法测定普卢利沙星的含量

以0.1mol.L-1高氯酸为滴定液,结晶紫为指示剂,用非水滴定法测定普卢利沙星。重复测定普卢利沙星含量平均值为99.4%(n=6),相对标准偏差为0.1%。该方法准确简便、重复性好,可作为普卢利沙星含量测定的有效方法。     

原子荧光光谱法测定土壤和沉积物中铋

建立了王水沸水浴消解-原子荧光光度法测定土壤和沉积物中铋。优化了仪器参数、载流及还原剂浓度,比较了水浴消解、微波消解和电热板消解三种前处理方式处理土壤/沉积物中铋的优劣。实验表明,最佳的消解方式为水浴消解,该方法操作简单方便,结果准确,可靠。采用王水沸水浴消解土壤或沉积物试样,方法的检出限为0.01 mg·kg-1(取样量为0.500 0 g,定容体积为50 mL),检出下限为0.04 mg·kg-1。该方法测定土壤标准样品,测定值都在标准值范围之内,相对误差为-4.7%～-2.0%。该方法用于测定土壤和沉积物实际样品的相对标准偏差分别为2.5%～3.4%和3.1%～3.4%,加标回收率分别为97.6%～102%和99.5%～104%。     

高效液相色谱法测定普卢利沙星胶囊的含量

建立高效液相色谱法测定普卢利沙星胶囊含量的方法。采用高效液相色谱法,以0.01mol.L-1盐酸溶液为溶剂,测定波长为280nm。在10—100μg.mL-1浓度范围内,主峰面积与相应的浓度呈良好的线性关系（r=0.9998）。重复测定峰面积平均值为1215.9（n=6）,相对标准偏差为0.7%。平均回收率为99.77%（n=9）,相对标准偏差为0.26%。该方法准确简便、重复性好,可作为普卢利沙星胶囊含量测定的有效方法。     

红外光谱法测定三唑锡中三环锡

三唑锡中三环锡含量大于等于10%时,以三环锡的红外特征吸收峰强度来直接测定三环锡;当三唑锡中三环锡含量小于10%时,以三唑锡的红外特征吸峰强度来测定三唑锡含量,再以衍生化法气相色谱测定得出的三唑锡和三环锡总量计算出三环锡含量.测定三环锡方法RSD为0.33%,回收率在100.1%-101.7%之间,测定三唑锡方法RSD为0.12%,回收率在100.6%-101.6%之间.     

电感耦合等离子体-原子发射光谱法快速测定土壤中全硫

以王水溶样,电感耦合等离子体-原子发射光谱法快速测定土壤中全硫。方法检出限为0.03μg/g。对实际样品进行连续7次测定,方法精密度为1.18%—1.88%,回收率为97%—108%。经国家标准物质验证,结果与标准值相符。方法快速、准确。     

Ultrasound-assisted cyanide extraction of gold from gold concentrate at low temperature

A sonochemical reactor was developed to study the ultrasound-assisted cyanide extraction of gold from gold ore at low temperature. The effects of ultrasound on gold leaching in low temperature and conventional conditions were investigated. At the low temperature of 10 °C, ultrasound-assisted extraction increased extraction rate of gold by 0.6%–0.8% and reduced the gold content of cyanide tailings to 0.28 g/t in the leaching of gold concentrate and cyanide tailings, respectively. At the conventional temperature of 25 °C, ultrasound-assisted extraction obtained a 0.1% higher extraction rate of gold compared with conventional extraction, with the unit consumption of NaCN reduction of 15%. The analysis of kinetic model also demonstrated that sonication indeed improved the reaction of gold leaching greatly. The mineralogy and morphology of ore were further analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM) and particle size analyzer to explore the strengthening mechanism of gold leaching. The results showed that the ore particles were smashed, the ore particle surface was peeled, the passive film was destroyed and the reaction resistance decreased under ultrasonic processing. Therefore, the extraction rate of gold was improved and the extraction time was shortened significantly in ultrasound-assisted cyanide extraction.     

王水溶矿-电感耦合等离子体-质谱法测定矿石中的金

建立了王水溶矿-电感耦合等离子体-质谱法测定矿石中的常量金的方法。该方法加标回收率94.0%—102.0%,精密度RSD 1.66%—4.01%,与传统的分析方法相比:该方法简单、快速、实用。     

小火试金分离富集火焰原子吸收光谱法测定矿石样品中的金

研究建立了一种有别于传统火试金的分离富集方法--小火试金分离富集矿石中的金，并采用火焰原子吸收光谱仪对金含量进行检测的方法。在小火试金条件的选择中，分别对小火试金熔剂比例、灰吹温度、保护剂用量进行了讨论，确定了这三个参数的最佳值分别为：硼砂-纯碱-黄丹-淀粉比例5∶5∶10∶1，900 ℃，10 mg，将3 g样品经焙烧后，在最佳小火试金条件下分离富集金，铅扣经灰吹得到金、银合金粒，经稀硝酸溶解后，加入盐酸将银与金分离，用火焰原子吸收分光光度计对溶液中的金进行测定，工作中探讨了原子吸收光谱仪测定金的各种影响因素，包括仪器参数优化、线性范围、干扰离子等。干扰实验表明其他共存贵金属元素对金的测量不产生影响，在选定的仪器条件下，对标准样品及某矿送检的金矿石样本中的金进行测定，结果与标准值一致，相对标准偏差（n=11）在0.72%～5.49%之间，方法回收率在98.82%～99.20%之间。此方法稳定可靠，准确度高，对0.X~XX.0 mg·kg-1的矿石中金含量均适用，拓展了火焰原子吸收测量金的含量范围，并且大大降低了传统火试金法对人及环境的伤害和污染，原子吸收光谱法具有响应快、灵敏度高、准确性好等优点，为进一步研究用此法开展其他贵金属的检测奠定了技术基础。     

基于XRD和SEM的含碳微细粒金矿氧化焙烧机理研究

含碳微细粒金矿是世界难处理金矿主要类型,且储量巨大,矿石中的有机碳、石墨碳能吸附溶液中的金氰络合物,因而含碳金矿在浸出之前需进行预处理。氧化焙烧是应用时间最长、可靠性和适应性最好的预处理工艺,已经成功的用于生产实践。针对传统氧化焙烧法存在生产成本高,收尘系统复杂等不足,近年来国内外学者在焙烧工艺和设备方面进行了大量的研究工作,取得了丰硕的研究成果,为氧化焙烧技术的发展注入了新的活力。但关于焙烧理论方面的研究较少,研究方法也比较单一,尤其是对于焙烧过程的相关理论研究比较薄弱,这在一定程度上影响了氧化焙烧技术的发展。焙烧时间是影响焙烧效果的关键因素,决定化学反应进度及物相变化程度。在不同时间条件下(焙烧温度650 ℃),对含碳微细粒金矿石进行焙烧-浸出试验,首次采用X射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)和孔结构分析等手段对含碳金矿及焙砂进行分析表征,进而揭示氧化焙烧过程中碳质物的氧化、矿石晶体结构变化、物相变化等对金浸出效果的影响机理。工艺矿物学研究表明： 矿石中主要矿物有石英、白云石、方解石、绢云母、高岭石、黄铁矿和石墨等;矿石中自然金粒度微细,以5～10 μm粒级为主,部分微粒自然金被石英、碳质组成的碎屑包裹;碳质(有机碳和石墨碳)含量高、粒度细,且与脉石矿物紧密共生。焙烧-浸出试验结果表明： 原矿直接浸出时,金浸出率仅为12.50%,碳质的“劫金”作用显著;随着焙烧时间的增加,金的浸出率先逐渐增大后变化平稳,焙烧时间为2 h时,金浸出率最高;当焙烧时间为1 h 时,绢云母发生了脱羟基变化,高岭石分解生成蒙脱石,黄铁矿氧化为赤铁矿,碳质(有机碳和石墨碳)氧化且产生CO₂,但未完全氧化,此时焙砂中石英的d₁₀₀和d₁₀₁值以及平均孔径较小,不利于浸出剂的扩散,导致金浸出率仅为58.09%;当焙烧时间为1.5 h 时,白云石开始分解,碳质已完全燃烧,产生的CO₂使微孔数量增多,有利于浸出剂的扩散,此时金浸出率增加到73.34%;当焙烧时间为2 h时,白云石分解较完全,焙砂中有MgO生成,此时焙砂中石英的d₁₀₁值达到最大值(4.255 03 nm),焙砂松散密度变大且孔容和平均孔径达到最大值,分别为0.009 954 cm3·g-1和6.640 80 nm,焙砂中产生的微孔最多,增加了浸出剂的扩散通道,有利于金的浸出,金浸出率也达到了最大值(91.28%);当焙烧时间为3 h时,焙砂表面生成Ca₂SiO₄和CaSO₄等在高温时易形成低熔点物质,发生微弱的烧结现象,导致颗粒内部的微孔被填充、闭合,微孔减少,孔容和平均孔径降低,内部结构变得致密,不利于浸出剂的扩散,同时造成金的浸出率下降。     

A197Au and57Fe mössbauer study of the roasting of refractory gold ores

The transformation of chemically bound gold into metallic gold during industrial scale roasting of an arsenical gold ore concentrate from the Fairview Mine, Eastern Transvaal, has been studied quantitatively by¹⁹⁷Au Mössbauer spectroscopy. The iron compounds in the concentrate, mainly FeAsS and FeS₂ and their transformations during roasting have been studied by⁵⁷Fe Mössbauer spectroscopy. The bound gold is found to convert into the metal in parallel to the decomposition of FeAsS and the increase in cyanide leachability. this shows that the refractory character of the ore is caused by the chemical bonding of the gold rather than by the physical inclusion of small, discrete metallic particles in the matrix of FeAsS or FeS₂. The ratio of thef-factors of gold bound in the FeAsS component of a refractory ore and of metallic gold was determined to bef(Au:FeAsS)/f(Au)=1.48±0.09.     

Effect of Selective Excitation of Gold Atoms in a Nonequilibrium Oxygen Plasma of a Combined Glow Discharge

The effect of selective excitation of gold atoms in a nonequilibrium oxygen plasma of a combined glow discharge (CGD) has been revealed. When working with alumina oxide as a matrix where the content of aluminum is about 30 wt.%, the atomic lines of Al are not seen at all in the CGD spectrum. But the atomic lines of gold have a very high intensity. Even when the aluminum and gold atomic lines overlap, gold can be detected at a content of 10^–7%. This effect has been registered both in synthetic and natural ore samples.     

197Au Mössbauer study of gold ores,mattes, roaster products,and gold minerals

The chemical state of gold in gold ores, mattes and roaster products has been studied by¹⁹⁷Au Mössbauer spectroscopy. Gold minerals were studied in order to provide reference data for the ore spectra.⁵⁷Fe Mössbauer spectroscopy was used to monitor the iron compounds always present in gold ores and to follow their transformations caused by smelting and roasting.     

矿石中金的分析不确定度评定

针对原子吸收光谱法测定金矿石中金的实验过程,详细地分析了引入的不确定度来源。测定结果的不确定度由标准配制、样品制备、曲线拟合、样品均匀性及检验重复性4个部分引入的不确定度分量组成,样品制备过程中考虑了活性炭吸附率的影响,求得测量结果的标准不确定度和扩展不确定度分别为0.043μg/g和0.09μg/g。     

Mössbauer investigation of gold-bearing pyrite-rich concentrates

A gold-bearing pyrite-rich concentrate of a refractory ore from the Golden Bear mine, northwestern British Columbia, and a pyrite-rich concentrate from Newhawk's west zone, Brucejack Lake area, northern British Columbia, containing 38 and 316 ppm Au and 0.57% and 0.19% As, respectively, have been investigated using¹⁹⁷Au and⁵⁷Fe Mössbauer spectroscopy. In the Golden Bear sample, the gold is mainly chemically bound in the pyrite with minor amounts present as an Au-Ag alloy, whereas in the Newhawk sample, the gold occurs mainly as an Au-Ag alloy with a composition close to Au_0.5Ag_0.5 and is only partly bound in the pyrite. Having mean isomer shifts of +3.2 and +4.0 mm/s with respect to a Pt metal source, the gold in pyrite exhibits shifts similar to those observed for gold in arsenopyrite. The nature of the lattice sites occupied by the gold in pyrite is discussed.     

Preconcentration and Separation of Gold(III) from Ore Samples by Solid-Phase Extraction Prior to Its Catalytic Fluorescent Determination

ABSTRACT

A new catalytic kinetic fluorescent quenching method for the determination of trace gold(III) was investigated. The method was based on the catalytic effect of gold on oxidation of 3-(3′-methylphenyl)-5- (2′-arsenoxylphenylazo) rhodanine by hydrogen peroxide in potassium hydrogen phthalate–hydrochloric acid (pH = 3.4). Under the optimum conditions, the great decrease of fluorescence intensity has a linear relationship against the concentration of gold in the range of 0 to 12.0 µg·L^?1 with a detection limit of 6.0 × 10^?10g·L^?1. The coexistent metal ions can be separated, and gold can be enriched by TBP resin of solid-phase extraction, which greatly improves the selectivity and sensitivity of the system. The method can be used to determine trace amounts of gold in ore samples successfully with satisfactory results.