共查询到18条相似文献，搜索用时 906 毫秒
1.
地质标准物质的粒度测量与表征实践 总被引：6，自引：4，他引：2
样品粒度是粉体地质标准物质的一项重要特性指标。长期以来地质标准物质的粒度一直是采用筛分法或沉降法检测,最终大多以加工样品通过一定筛目(一般为-200目)的比例来表达;近年来超细标准物质研制引入了以激光粒度仪为代表的粒度检测与分析的现代方法,并可以直观的粒度分布图和简洁明晰的特征粒径等多种方法来表达粒度分布特征,大大提升了粉体地质标准物质粒度分布特性的测量及表征水平。文章在前期采用激光粒度仪测量超细标准物质粒度分布特征工作的基础上,用此法测量了当今广泛使用的典型地质标准物质的粒度分布,为这些标准物质的正确使用和取样不确定度评价提供了重要依据;同时就今后地质标准物质乃至地质分析样品的粒度检测与表征提出建议。 相似文献
2.
微波消解-电感耦合等离子体质谱法测定超细粒度岩石和土壤样品中的稀土元素 总被引：2，自引：1，他引：1
应用电感耦合等离子体质谱法(ICP-MS)分析岩石和土壤样品中稀土元素的含量,取样量可低至数毫克级,但200目样品粒度要求分析取样100mg才能保证代表性,导致ICP-MS灵敏度高、取样量小的优势难以得到充分发挥。本文研究了研磨方式、研磨时间、物料比对超细粒度土壤和岩石样品制备的影响,结果表明采用乙醇作为分散剂进行湿法球磨,200目粒度的土壤、岩石样品分别研磨10min和15min,土壤样品的物料比采用物料7g、研磨球500个、分散剂45mL,岩石样品的物料比选取物料5g、研磨球500个、分散剂45mL,细化程度最佳。在此条件下制备的超细粒度土壤标准物质GBW07404、GBW07447的粒径分布D_(95)可低至7.51μm、7.05μm,超细粒度岩石标准物质GBW07104、GBW07121的D_(95)可低至8.42μm、8.30μm。在硝酸-氢氟酸-过氧化氢酸溶体系中微波消解处理超细粒度岩石标准物质GBW07104,取样量减少至5mg,总用酸量减少至0.25mL,消解时间降低为25min,稀土元素的测定值与认定值基本一致,相对标准偏差在1.64%～5.21%之间。该方法用于分析其他超细粒度标准物质(GBW07404、GBW07447和GBW07121)中的稀土元素,相对误差为0.17%～6.60%,满足《地质矿产实验室测试质量管理规范》的一级标准。 相似文献
3.
几种矿物的超细加工及对建材防氡防辐射性能的影响 总被引：3，自引：0，他引：3
采用湿法搅拌磨和气流磨,对用作防氡防辐射基元材料原料的重晶石、沸石进行超细加工和激光粒度分布测试,结果表明：重晶石、沸石通过湿法和干法粉磨加工,在一定的时间内都可以超细粉碎到d90小于10μm,从粉磨时间以及粉磨成本来比较干磨法要明显优于湿磨法;重晶石进行超细加工后所制备的水泥砂浆的外照射指数从0．51降到0．23,重晶石所配腻子的氡和放射性屏蔽率提高20％～30％。当沸石的粒度减小时,水泥砂浆对氡的屏蔽率提高的屏蔽率最大达26％。沸石从119μm降到18μm时,腻子的防氡率从37．9％提高到53．1％。防辐射性能从整体上来看是粒度越细性能越好。 相似文献
4.
封闭酸溶-等离子体质谱法分析超细粒度地质样品中42个元素 总被引：1，自引：3，他引：1
采用封闭压力酸溶，电感耦合等离子体质谱法（ICP—MS）测定了超细样品的42个元素，研究了样品的粒度、分解条件、取样量对分析准确度和精密度的影响。结果表明，用超细粉碎样品（〈30μm），取样量减小至2mg仍能保证取样代表性，总用酸量可减至0．5mL，反应时间也可大大缩短。采用超细样品可更好地发挥ICP—MS技术高灵敏度的效能，从而达到保护环境、降低分析成本、提高分析效率的目的。 相似文献
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6.
地质标准物质粒度测量与表征的现代方法 总被引：7，自引：2，他引：5
地质标准物质是地质材料分析的计量标准,在分析质量监控、仪器校准和分析方法评价中发挥着重要作用。地质标准物质大多为粉体材料,而粒度是粉体材料的一项重要特性指标。长期以来,地质标准物质的粒度一直采用过筛法检测;近年来在超细标准物质研制中引入了以激光粒度仪为代表的现代粒度分析方法,并以直观的粒度分布图和简洁的特征粒度来表达分析结果,大大提升了粉体地质标准物质粒度特性的测量及表征水平。在此工作基础上,测量了正在广泛使用的典型地质标准物质的粒度分布,获得了前所未知的粒度分布信息,为这些标准物质的正确使用和取样不确定度评价提供了有益的资料。简单地介绍了检测粉体材料颗粒特性的现代方法,讨论了地质分析与粒度分析在概念上的差异,并就今后地质标准物质乃至地质分析样品的粒度检测与表征方法提出了建议。 相似文献
7.
超细粉末压片法-X射线荧光光谱测定水系沉积物和土壤中的主量元素 总被引：4，自引：3，他引：1
X射线荧光光谱分析中,粉末压片法是一种理想的绿色环保制样技术,操作简单、制样效率高,但由于受到粒度效应和矿物效应的影响,其测定误差在5%左右,因而限制了这种技术在常量元素检测方面的应用,目前主要应用于痕量元素的测定以及对分析精度要求不高的分析领域。本文运用行星式粉碎制样机,将水系沉积物和土壤标准物质在几分钟内粉碎至平均粒径4~5μm左右,建立了超细粉末压片制样X射线荧光光谱测定SiO2、Al2O3、Fe2O3、CaO、MgO等主量元素的方法。该方法绝大多数主量元素的测量精密度(RSD)小于2%;检出限为0.003%~0.021%,优于熔融法的检出限(0.006%~0.081%),特别是原子序数小的钠元素,检出限改善4倍。本文针对水系沉积物和土壤研制的超细粉末压片法,由于样品粉碎至几微米,最大限度地减小了粒度效应的影响;X射线衍射分析表明制备样品的矿物成分以石英为主,矿物组成简单,矿物效应可以忽略不计。同时对测量数据加入烧失量进行归一化处理,各元素归一化的测量结果与标准值基本一致,方法准确度比常规压片法获得显著提高。 相似文献
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沉积物环境敏感粒度是进行古环境研究的重要方法之一, 然而华北平原地区很少进行完整的第四纪全取心深孔沉积物环境敏感粒度组分的提取及分析.对天津渤海湾G1和G2孔第四纪沉积物样品进行粒度分析, 采用粒级-标准偏差和主成分分析两种方法进行了沉积物环境敏感粒度组分提取.对比提取结果发现, 两种方法存在差异性的同时还存在一定的兼容性, 沉积层理厚度越薄, 兼容性越明显; 主成分分析方法对沉积物环境敏感粒度组分刻画得更为细致, 粒级-标准偏差方法不适合深孔沉积物整体敏感粒度组分的提取.G1孔环境敏感粒度组分的粒度峰值为6.700μm、15.650μm、36.240μm、176.900μm、282.100μm、716.800μm; G2孔环境敏感粒度组分的粒度峰值为0.578μm、176.000μm, 分别对应6个和3个粒度分布区间, 指示两孔整体上的沉积物来源及沉积环境空间存在差别.G2孔相对于G1孔整体上的沉积强度大且沉积环境较为稳定, 适合于开展高分辨率的古环境重建工作. 相似文献
9.
粉末压片制样-波长色散X射线荧光光谱法测定进口铜矿石中的氟 总被引：3，自引：3，他引：0
地质样品中氟的测定主要采用氟离子选择电极法,但操作复杂、分析时间长,无法满足大量进口铜矿石检测的需求。熔融制样-X射线荧光光谱法可用于测定铜矿石中的主次量成分,但不能测定氟。本文采用粉末压片制样,波长色散X射线荧光光谱测定进口铜矿石中氟的含量。以15个粒度为0.074 mm的实际进口铜矿石样品建立标准曲线,经验系数法校正基体效应,有效地降低了颗粒度效应、矿物效应和基体效应。方法的精密度为0.30%(RSD,n=11),检出限为2.4μg/g,测定范围为0.030%～0.20%。用标准物质验证,测定结果与标准物质的认定值相符;用实际样品验证,测定结果与氟离子选择电极法的测定值相符,能满足进口铜矿石中氟(限量不大于0.10%)日常分析检验的要求。 相似文献
10.
钛铁矿化学成分标准物质研制 总被引：3，自引：3，他引：0
当前我国没有钛铁矿化学成分标准物质,只有与其相似的钒钛磁铁矿石标准物质,国外钛铁矿标准样品主要是钛铁矿精矿,不能有效地进行分析质量控制,因此迫切急需研制钛铁矿化学成分标准物质。本文研制了5个钛铁矿化学成分标准物质。样品采自山东省莒县棋山钛铁矿矿区、山东省沂水常庄钛铁矿矿区和河北省承德黑山钛铁矿矿区,采用流化床对撞式气流粉碎磨将样品细碎至粒度小于50μm,混合均匀后进行均匀性和稳定性检验,代表性元素的电感耦合等离子体发射光谱和电感耦合等离子体质谱分析结果表明方差检验的F值小于临界值,样品均匀性良好;所检验的元素经18个月6次分析,均未发现统计学意义的明显变化,样品的短期和长期稳定性良好;烘样温度(20~60℃)对亚铁(FeO)的稳定性并无影响,亚铁不会发生氧化。选择11家具有资质的实验室,采取经典分析方法与现代仪器分析技术相结合的方式,选用两种以上不同原理的准确度高的可靠方法对该标准物质联合定值,依照JJF 1343—2012和一级标准物质技术规范,5个钛铁矿化学成分标准物质给出了46项组分(包括主量、痕量和全部稀土元素)的认定值和不确定度,TiO2的含量范围为2.97%~19.76%,TFe的含量范围为18.88%~51.30%,基本涵盖了我国钛铁矿成矿类型,能够满足钛铁矿勘查、评价和开发的需求。 相似文献
11.
Investigations into the Preparation of Ultra-Fine Particle Size Geochemical Reference Materials 总被引：1，自引：1，他引：1
Yimin Wang Yushu Gao Xiaohong Wang Shuqi Wu Tiexin Gu 《Geostandards and Geoanalytical Research》2004,28(1):113-121
Although over recent years, sensitivity and precision of modern analytical techniques have continuously improved, traditional analytical specification for the particle size of samples has remained at 74 μm (-200 mesh). For this reason, the uncertainty caused by inhomogeneity in test portions of the sample itself has become a more and more significant contribution to the total analytical uncertainty. Therefore, to reduce this total uncertainty, the first step is to improve the homogeneity by reducing the particle size of a sample. For this purpose, we have investigated a method for the preparation of ultra-fine reference materials. Using the modern ultra-fine crushing technique (jet mill), six marine sediment samples MSAn and MSCS-1 to 5 were prepared and the particle distributions of these samples were measured using a laser particle-analyser. The average particle size of these samples was 4–5 (im and the largest particle size was less than 30 (im. MSAn will be used as the sample for a future GeoPT(tm) proficiency testing round and MSCS-1 to 5 will be prepared as reference materials. All geochemical laboratories are welcome to participate in this co-operative research programme. The processing and use of ultra-fine samples (< 30 μm) will have a significant influence on the future development of geoanalytical techniques as a consequence of the potential reduction in the mass of test portion and the development of new geoanalytical systems. 相似文献
12.
Xiaohong Wang Yimin Wang Yushu Gao Yongyang Huang Zhenyu Wang Xuefa Shi 《Geostandards and Geoanalytical Research》2009,33(3):357-368
We report the preparation and characterisation of five sediment reference materials MSCS-1–5 from the China Sea and continental shelf. The raw samples were individually collected from the East China Sea and the South China Sea. They were first ground by ball mill to a homogenous powder of -200 mesh (< 74 μm). Then, half of each sample was further processed by an ultra-fine powder processing technique, a jet mill, to form a powder with an average particle size of < 4 μm (about 800 mesh). The homogeneity was tested by high-precision WD-XRF and the precision was found to be less than 1% RSD, which is compatible with the precision range for modern analytical techniques. An F-test showed that all five samples were homogeneous. Twelve laboratories participated in the cooperative study and sixty constituents were determined. Between fifty and fifty-two analytes were characterised as recommended values in MSCS-1–5 in compliance with Chinese national norms. The sum of the major and minor elements or components in the five reference materials MSCS-1–5 was 99.91%, 99.86%, 100.43%, 100.12% and 99.66%, respectively. 相似文献
13.
Yimin Wang Xiaohong Wang Wenjun Qu Yushu Gao Tiexin Gu Xingtao Fan S.I. Andreev Xuefa Shi 《Geostandards and Geoanalytical Research》2011,35(3):341-352
Two Co‐rich seamount crust reference materials, MCPt‐1 and MCPt‐2, were prepared using ultra‐fine particle size milling technique and characterised for the platinum‐group elements (PGEs). The raw material for these two reference materials was collected separately from the Magellan seamounts of the western Pacific Ocean and the seamounts of the central Pacific Ocean by Russian and Chinese scientists. First, they were ground by ball mill to a ?200 mesh powder, then further processed by ultra‐fine jet mill and well‐mixed. The particle size distributions of the samples were tested by a laser particle analyser; the average particle size was 1.8 and 1.5 μm (equal to about 2000 mesh) respectively. The homogeneity of six major and minor elements in these two materials was tested at the milligram level of sampling mass by high‐precision wavelength dispersive X‐ray fluorescence (XRF) spectrometry and at the microgram level of sampling mass by electron probe microanalyser. The homogeneity of more than forty trace elements, including Pt, was tested at the microgram level of sampling mass by LA‐ICP‐MS. Except for Rh, all PGEs were determined by isotope dilution‐ICP‐MS. Platinum in MCPt‐1 and MCPt‐2 was characterised as certified values, whereas the other five PGEs in MCPt‐1 and MCPt‐2 were reported as reference values. In addition, the information values of sixty‐two major, minor and trace elements were obtained by XRF, ICP‐AES and ICP‐MS. The minimum sampling mass for the determination of PGEs was 1 g, while the minimum sampling mass for the determination of the other elements was 2–5 mg. 相似文献
14.
介绍了雷蒙磨粉机原理。采用雷蒙磨粉机，对不同含量铜镍铂（族）矿石标准样品加工至粒度小于0．074mm。选择合适的磨球和样品质量比，球磨机磨-混24～72h。样品经粒度筛分试验、均匀度及稳定性检验，证明其中被检验元素分布均匀。 相似文献
15.
Xiaohong Wang Yushu Gao Yimin Wang S.I. Andreev 《Geostandards and Geoanalytical Research》2003,27(3):251-257
A research project involving the preparation of three Co-rich crust reference materials (GSMC-1 to 3) has been preliminarily completed. The samples were collected from the eastern and central Pacific seamount zones and their main chemical composition is MnO2 . After the raw materials were dried in ambient air and at low temperature (60-100 C), they were ground in a ball mill to form a well-mixed powder. The proportion of particle size fractions of < 74 μm and < 3 μm was over 98% and 50% respectively. The homogeneity of the materials was tested using wavelength dispersive X-ray fluorescence spectrometry (WD-XRF). The relative standard deviation (% RSD) of the measurements for all the selected elements in forty sub-samples randomly taken from the bottles was less than 0.4%. Sixteen laboratories from Germany, Russia, France, Australia and China participated in the collaborative analysis programme. Fifty seven elements or constituents were analysed, and among those, forty six elements were certified in each sample. The sum of contents of the major and minor elements or components was 99.5% for GSMC-1, 99.6% for GSMC-2 and 99.2% for GSMC-3. 相似文献
16.
在煤层气开发过程中,煤粉聚集及沉降会堵塞煤层气运移通道及导致卡泵、埋泵等事故。为了查明不同粒度煤粉的聚集及沉降特征,选取粒度>140目（<106 μm）、>70~140目（106~<212 μm）和>50~70目（212~<300 μm）3种粒度范围的煤粉,开展了在去离子水中煤粉的聚集及沉降实验,从煤粉聚集及沉降特征观察、悬浮液中煤粉含量及煤粉粒度分布探究不同粒度煤粉在去离子水悬浮液中的聚集及沉降特征。结果表明,随着静置时间的增加,各粒度煤粉悬浮液的颜色均不同程度地变浅,逐渐出现分层,其中,粒度>140目的煤粉悬浮液最先出现分层。煤粉粒度越小,煤粉悬浮液顶部漂浮的煤粉量越多;煤粉粒度越大,其下沉到煤粉悬浮液底部的煤粉量越多。不同粒度煤粉悬浮溶液中煤粉含量均随着静置时间的增加呈现不同程度的降低,在停止搅拌后3 min内,煤粉含量下降最快,粒度为>70~140目的煤粉悬浮液中煤粉含量最大。根据不同粒度煤粉悬浮液中煤粉粒度分布曲线,将煤粉聚集及沉降过程分为3个阶段:单峰变双峰阶段（煤粉快速上浮及沉降）、双峰变单峰阶段（煤粉快速聚集及沉降）和单峰阶段（煤粉缓慢沉降）。粒度>140目的煤粉在悬浮液中最先达到缓慢沉降阶段,粒度>70~140目的煤粉在悬浮液中最后到达缓慢沉降阶段。从煤粉的受力、扩展的DLVO理论及煤粉的有机分子结构方面探讨了煤粉聚集沉降的机理:煤样含有大量的脂肪烃和芳香烃等疏水性基团,疏水性强,润湿性低;随着煤粉粒度的减小,其比表面积显著增大,煤粉表面吸附大量空气,形成气膜;同时,煤粉颗粒间相互吸附聚集,内部形成很多微孔隙,导致粒度小的煤粉易聚集漂浮在悬浮液面上。实验得到的不同粒度煤粉的上浮、下沉及悬浮情况,为后期煤层气开发中煤粉管控措施提供依据。 相似文献
17.
偏振能量色散X射线荧光光谱法测定硫化物矿石中的铜铅锌 总被引：1，自引：1，他引：0
X射线荧光光谱法用于分析矿石主成分的常规制样方法有粉末压片法与玻璃熔融法,但分析硫含量高的地质样品时,前者存在矿物效应和粒度效应问题、后者可能腐蚀贵金属坩埚。为满足矿产勘查的需要,急需一种适应于硫化物矿石主成分分析的制样方法。本文建立了一种硝酸+氢氟酸封闭消解试样,标准溶液校准,偏振能量色散X射线荧光光谱(PE-EDXRF)同时测定硫化物样品中铜、铅、锌三种元素的分析方法。用GBW 07162~GBW 07168等7种矿石国家一级标准物质进行精密度和准确度实验。结果表明,当样品中铜、铅、锌元素含量大于1%时,几乎所有样品中的铜、铅、锌元素的精密度(RSD,n=6)优于5%,检测结果与标准值一致性良好。本方法通过样品消解、直接液体进样等技术的应用,消除了粒度效应和矿物效应等基体效应对分析结果的影响,解决了因缺乏基体匹配的标准物质而造成的含量校准的问题,使PE-EDXRF技术可以在硫化物矿石分析中得到比较方便的应用。这种分析方法为实验室矿石分析提供了新手段,也为野外现场PE-EDXRF分析高矿化度样品提供了新途径。 相似文献
18.
A centrifugal mill is a high-power intensity media mill that can be used for ultra-fine grinding, employing centrifugal forces generated by gyration of the axis of the mill tube in a circle. The mill charge motion is quite different depending on the ratio of the gyration diameter to the mill diameter (G / D ratio), varying from a motion similar to that of a conventional tumbling media mill to that of a vibration mill. In this study, a centrifugal mill was constructed with an arrangement where the gyration diameter could be readily adjusted. The batch grinding characteristics of three different minerals (limestone, talc and illite) in water with dispersing agent were investigated at various G / D ratios. It was found that the optimum G / D ratio in terms of the specific energy consumption to give a desired fineness of product was different for the three minerals. This was due to their different reactions to the breakage mechanisms provided by the mill charge motion at varying G / D ratios. The size distributions became progressively narrower at increased grinding times, and particles finer than about 0.1 μm were not detected even for prolonged grinding times. Measurement of specific surface areas indicated that this was not due to an artifact of the size measurements by laser diffractometry. This implies that there is a limitation in which particles finer than 0.1 μm are not produced under the conditions tested in this type of mill, but further investigation is needed for experimental verification of this limit of comminution. 相似文献