关于澳洲GoLden Grove金精矿磨样方法的研究

金精矿样品的粒度,直接影响金精矿中金含量测定的精密度和稳定性,本文通过对Golden Grove金精矿采用不同的磨样工具和磨样时间,得到不同粒度的样品,对不同样品进行了金含量的测定,并对测定结果的精密度进行了分析。其中磨样方式：滚筒磨样机、磨样时间为5h、磨样粒度为0.040mm(360目)95%以上的B样品,测定精密度最好。C样品测定精密度相对较差,反映出振动粉碎机磨样均匀度相对较差。     

王水回流溶样-火焰原子吸收光谱法测定地质样品中的金

建立王水回流溶样聚氨酯泡沫塑料吸附火焰原子吸收光谱法测定地质样品中金的分析方法。在传统法使用锥形瓶王水溶样的基础上,在磨口锥形瓶上增加回流装置,以长15 cm的玻璃管作为冷却回流管,加入30mL王水溶液(1+1)对样品进行消解,采用火焰原子吸收光谱法测定。金的质量浓度在0～4.00μg/mL范围内与吸光度呈良好的线性关系,相关系数为0.999 3,检出限为0.058μg/mL。金矿石标准物质测定结果的相对标准偏差为2.75～6.41%(n=6),相对误差为–5.00%～0.61%;5种不同矿区金矿石样品测定结果的相对标准偏差为2.02%～9.24%(n=9)。该方法样品消解完全,减少了王水的使用量和氮氧化物的排放,操作简便,结果准确可靠,适用于地质样品的批量分析。     

多晶X射线衍射测量结果的一些影响因素

讨论了多晶X射线衍射测量中实验结果的一些影响因素.分别对粉末样品自身颗粒的大小、粉末装填到样品架中所处的表面平整度以及少量样品采用横式填充还是竖式填充等问题进行了分析和探讨.结果表明,在X射线衍射分析测量中,要想得到理想的衍射数据,试样颗粒应小于50μm,而且装填后样品与样品架表面保持平齐,对少量或微量试样应采取横式填充法.     

电感耦合等离子体原子发射光谱（ICP-AES）法测定铁矿石中钒

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铁矿石中钒含量的分析方法。采用盐酸、硝酸、氢氟酸、高氯酸分解试样,不溶物残渣碱熔融回收,稀盐酸溶解盐类的方式对样品进行分解。对仪器的主要工作参数和分析谱线进行了选择,讨论了基体和共存元素的干扰,以及溶解酸和熔剂等条件实验,确立了最佳分析条件。按实验方法对铁矿石标准样品和试样中钒量进行测定,测定值与标准值或其它方法的认定值基本一致,相对标准偏差RSD<6.5%。     

电感耦合等离子体原子发射光谱（ICP-AES）法测定铁矿石中钒

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铁矿石中钒含量的分析方法。采用盐酸、硝酸、氢氟酸、高氯酸分解试样,不溶物残渣碱熔融回收,稀盐酸溶解盐类的方式对样品进行分解。对仪器的主要工作参数和分析谱线进行了选择,讨论了基体和共存元素的干扰,以及溶解酸和熔剂等条件实验,确立了最佳分析条件。按实验方法对铁矿石标准样品和试样中钒量进行测定,测定值与标准值或其它方法的认定值基本一致,相对标准偏差RSD6.5%。     

电感耦合等离子体原子发射光谱（ICP-AES）法测定铁矿石中钒

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铁矿石中钒含量的分析方法。采用盐酸、硝酸、氢氟酸、高氯酸分解试样,不溶物残渣碱熔融回收,稀盐酸溶解盐类的方式对样品进行分解。对仪器的主要工作参数和分析谱线进行了选择,讨论了基体和共存元素的干扰,以及溶解酸和熔剂等条件实验,确立了最佳分析条件。按实验方法对铁矿石标准样品和试样中钒量进行测定,测定值与标准值或其它方法的认定值基本一致,相对标准偏差RSD<6.5%。     

基于激光剥蚀-电感耦合等离子体质谱技术的生物元素成像分析

生物体内的微量元素具有十分重要的生物功能,也与许多疾病密切相关。现代生物医学的研究亟需能在组织、细胞等不同水平上原位分析生物样品中微量元素的分析方法。本研究建立了激光剥蚀-电感耦合等离子体质谱( LA-ICP-MS)原位分析生物样品的方法。采用线扫描模式和较小的激光输出能量(﹤1 J/cm2),得到了鼠脑切片和金纳米颗粒暴露后单细胞的金属元素成像图。 LA-ICP-MS具有空间分辨率高、检出限好、运行成本较低等优势,有望在生物医学研究中得到更广泛的应用,发挥更重要的作用。     

我们是怎样提高金分析数据合格率的

在黄金生产和试验研究工作中,分析检验工作是重要环节,分析数据是核算经济指标的重要依据。冶金部黄金局在黄金矿山化验技术管理规则中规定:内检合格率达75%以上时基本分析结果为合格,否则基本分析结果全部作废。我们在金的分析中做了些工作,使金分析数据的合格率显著提高。平均合格率1981年为57.0%,1982年为81.3%,1983年为94.3%。为保证化验结果的准确度我们主要注意了以下几点;一、采用准确可靠的分析方法针对试样性质、特点采用相应的分析方法。在投入生产使用之前应作方法考核试验,以验证方法的可靠性和熟悉关键操作,以便正确掌握分析方法。二、采样必须有代表性严格遵守并使用合理的     

超高效液相色谱-四极杆飞行时间质谱分析不同加工何首乌中差异化学成分

建立了超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF-MS)结合多元统计分析技术对不同加工何首乌中化学成分差异的分析方法。何首乌样品采用甲醇在室温下超声提取后,采用UPLC-QTOF-MS进行分析,对采集的图谱通过峰匹配、峰对齐、滤噪处理等进行特征峰提取,然后用主成分分析(PCA)和偏最小二乘法-判别分析(PLS-DA)对数据进行分析。结果显示,不同加工何首乌样品间的化学组成存在显著性差异;根据一级质谱精确质荷比和二级质谱碎片信息,结合软件数据库搜索及相关文献进行成分鉴定,初步筛选并鉴定出33种不同加工何首乌间差异显著的化学成分,其中15种为共有差异化学成分,并呈现出不同的变化规律。研究结果可为揭示不同加工方法对何首乌代谢产物差异性的影响规律提供依据。     

铅铋合金中金 、银分析取样方法的研究

围绕取样代表性和样品加工均匀性等问题,研究了铅铋合金锭中金银分析试样加工粒度对金银品位的影响,锭内金银分布及规律。通过对铅铋合金锭中金、银分布情况的研究结果,制定了铅铋合金锭的采样、样品加工及化验分析方案。     

Improvements in the Grinding of Gold-Bearing Geochemical Samples and Their Sampling for Fire Assay

The effect of fine grinding of gold-bearing geochemical samples on the representative sample size and the recovery of gold and silver in fire-assay fusion was studied experimentally. A method is proposed for the improvement of grinding and sampling procedures in fire assay.     

A high selective ion‐imprinted polymer grafted on a novel nanoporous material for efficient gold extraction

In this work, for the first time, an ion‐imprinted polymer was developed for selective extraction and determination of gold ions. To increase the sorbent efficiency, this polymer was coated on a novel nanoporous carbon‐based material, carbohydrate‐derived Max‐Planck Gesellschaft 1, which is also the first example of grafting imprinted polymer on nanoporous‐carbon material. These particles were applied successfully for preconcentration of ultratrace amount of gold ions, following determination by flame atomic absorption spectrometry. Some effective factors on the efficiency of gold ions extraction, such as concentration and volume of eluent, sample and eluent flow rates, and also effect of interfering ions especially palladium and platinum ions, were investigated. The LOD was determined to be 0.27 ng/mL. Furthermore, the precision of the method was calculated to be 2.14% under optimal conditions with recovery more than 97.3%. The technique was also used to determine the concentration of gold ions in mine stone samples with satisfactory results. The accuracy of this method was investigated by determination of gold ions concentrations in several reference materials with certified gold content.     

云南某金矿金与伴生元素的某些特征

采用中子活化分析方法研究了云南某金矿区内的硅化褐铁矿化石英砂岩类、辉绿岩类、灰岩类和黄铁矿样品的微量元素特征,并利用元素地球化学研究方法对元素间的相关关系进行了分析.结果表明,在该地区利用金的伴生元素来指导找矿,可提高金的找矿效益.     

Determination of trace amounts of gold in acid-attacked environmental samples by atomic absorption spectrometry with electrothermal atomization after preconcentration

A method for determination of trace amounts of gold in environmental samples (rocks, soils, sediments, and waters) by atomic absorption spectrometry with electrothermal atomization (ETAAS) after preconcentration using a chelating sorbent Spheron Thiol 1000 is described. The method accurately determines gold between 0.001 and several tens of grams per ton in samples having complex variations in mineralogy. Pulverized samples are roasted at 650°C to oxidize any sulfide and/or carbonaceous material. Samples are then subjected to a series of acid treatments to eliminate any silica matrix and to dissolve the sample. The Spheron Thiol 1000 is added to the sample solution, and then with sorbed gold is filtered out, washed, and ignited at 550°C. The residue is dissolved in aqua regia, evaporated, dissolved in distilled water, transferred to a volumetric flask, and analyzed by ETAAS.The limits of detection of gold, based on the 3 definition, were 0.5 ng g^–1 for 10-g samples (rocks, sediments, soils) and 0.05 ng mL^–1 for 1-L water samples. Precision of determination expressed by the relative standard deviation varied from 2.9% to 16.4%. The accuracy of the method is verified by analysis of certified reference materials. The obtained analytical results are in good agreement with attested values. The developed method was applied for gold determination in environmental samples affected by the acidification (acid mine drainage which is mainly a product of pyrite oxidation) from an open quartzite mine in the obov region situated NE of the city of Banská tiavnica (Slovakia).     

四川某金矿中非金属单矿物的元素分析及意义

利用中子活化分析法对四川某地区的非金属单矿物(热液脉矿物)的元素进行了测试,并利用元素地球化学研究方法对元素间的相关关系进行了分析。结果表明,在该地区可以利用元素间的伴生关系指导找矿。     

A gold nanoparticle-based immunochromatographic assay: the influence of nanoparticulate size

Four different sized gold nanoparticles (14 nm, 16 nm, 35 nm and 38 nm) were prepared to conjugate an antibody for a gold nanoparticle-based immunochromatographic assay which has many applications in both basic research and clinical diagnosis. This study focuses on the conjugation efficiency of the antibody with different sized gold nanoparticles. The effect of factors such as pH value and concentration of antibody has been quantificationally discussed using spectra methods after adding 1 wt% NaCl which induced gold nanoparticle aggregation. It was found that different sized gold nanoparticles had different conjugation efficiencies under different pH values and concentrations of antibody. Among the four sized gold nanoparticles, the 16 nm gold nanoparticles have the minimum requirement for antibody concentrations to avoid aggregation comparing to other sized gold nanoparticles but are less sensitive for detecting the real sample compared to the 38 nm gold nanoparticles. Consequently, different sized gold nanoparticles should be labeled with antibody under optimal pH value and optimal concentrations of antibody. It will be helpful for the application of antibody-labeled gold nanoparticles in the fields of clinic diagnosis, environmental analysis and so on in future.     

Determination of Al, Cu, Li and Mn in spruce seeds and plant reference materials by slurry sampling graphite furnace atomic absorption spectrometry

An ultrasonic slurry sampling graphite furnace AAS method was developed for the determination of Al, Cu, Li and Mn in spruce seeds, NBS SRM 1575 pine needles and GBW CRM 07602 bush branches and leaves. The only sample preparation was grinding in a Mixer Mill before preparing a slurry by adding 0.14 mol/L nitric acid to a small sample aliquot. Cryogenic grinding was used for the spruce seeds to solve the problem of agglomerating during grinding at room temperature. A modified sample tray was applied allowing the use of both the commercial 1.5 mL vials and home-made 15 mL vials. With optimal conditions for ultrasonic agitation the homogeneity and particle size distributions in the slurries prepared in the two different vials were similar. Several aspects of the slurry sampling approach are discussed and data of important parameters are given, including the total number of particles injected into the graphite furnace, densities of the materials and percentage of analyte extracted into the liquid phase of the slurry. The density of the materials was determined by two methods; by using a Coulter particle analyser and by using a gravimetric method. The two methods gave similar accuracy and precision. The concentration ranges of the elements (in microg g(-1)) were: 80-2100 for Al, 3-15 for Cu, 0.06-2.5 for Li and 50-700 for Mn. External calibration with aqueous standards was employed. Chemical modifiers were not found to be necessary. The relative standard deviations were in the range 1.7-7%. Analyses of the two certified plant reference materials confirmed the accuracy of the method. In addition no significant difference was found for analyses of digested and slurried spruce seeds. The detection limit was 10 ng g(-1) for Li and 170 ng g(-1) for Cu. The characteristic mass (area measurements) was 4.4 pg for Li and 11 pg for Cu. For Al and Mn less sensitive wavelengths were used.     

Determination of Al, Cu, Li and Mn in spruce seeds and plant reference materials by slurry sampling graphite furnace atomic absorption spectrometry

An ultrasonic slurry sampling graphite furnace AAS method was developed for the determination of Al, Cu, Li and Mn in spruce seeds, NBS SRM 1575 pine needles and GBW CRM 07602 bush branches and leaves. The only sample preparation was grinding in a Mixer Mill before preparing a slurry by adding 0.14 mol/L nitric acid to a small sample aliquot. Cryogenic grinding was used for the spruce seeds to solve the problem of agglomerating during grinding at room temperature. A modified sample tray was applied allowing the use of both the commercial 1.5 mL vials and home-made 15 mL vials. With optimal conditions for ultrasonic agitation the homogeneity and particle size distributions in the slurries prepared in the two different vials were similar. Several aspects of the slurry sampling approach are discussed and data of important parameters are given, including the total number of particles injected into the graphite furnace, densities of the materials and percentage of analyte extracted into the liquid phase of the slurry. The density of the materials was determined by two methods; by using a Coulter particle analyser and by using a gravimetric method. The two methods gave similar accuracy and precision. The concentration ranges of the elements (in μg g^–1) were: 80–2100 for Al, 3–15 for Cu, 0.06–2.5 for Li and 50–700 for Mn. External calibration with aqueous standards was employed. Chemical modifiers were not found to be necessary. The relative standard deviations were in the range 1.7–7%. Analyses of the two certified plant reference materials confirmed the accuracy of the method. In addition no significant difference was found for analyses of digested and slurried spruce seeds. The detection limit was 10 ng g^–1 for Li and 170 ng g^–1 for Cu. The characteristic mass (area measurements) was 4.4 pg for Li and 11 pg for Cu. For Al and Mn less sensitive wavelengths were used.     

Novel ion-imprinted polymer coated on nanoporous silica as a highly selective sorbent for the extraction of ultratrace quantities of gold ions from mine stone samples

We have developed a gold ion-imprinted polymer (GIP) by incorporating a dipyridyl ligand into an ethylene glycol dimethacrylate matrix which then was coated onto porous silica particles. The material was used for the selective extraction of ultratrace quantities of gold ion from mine stones, this followed by its quantitation by FAAS. The effects of concentration and volume of eluent, pH of the solution, flow rates of sample and eluent, and effect of potentially interfering ions, especially palladium and platinum, was investigated. The limit of detection is <0.2 ng?mL^?1, the precision (RSD%) is 1.03 %, and recoveries are >99 %. In order to show the high selectivity and efficiency of the new sorbent, the results were compared to those obtained with more simple sorbents possessing the same functional groups. The accuracy of the method was demonstrated by the accurate determination of gold ions in a certified reference material. To the best of our knowledge, there is no report so far on an imprint for gold ions that has such a selectivity over Pd(II) and Pt(II) ions.