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1.
自动电位滴定技术精确测定铜矿石中高含量铜的方法研究   总被引：2，自引：2，他引：0  
铜矿石中百分含量铜的分析通常采用手动目视滴定法,该方法借助化学指示剂判定终点,存在终点判断和人为操作等误差,精密度、可靠性相对较差。基于此,本文建立了精确测定铜矿石中高含量铜的分析方法,采用智能型自动电位滴定仪自动判定终点,高分辨加液器精确控制硫代硫酸钠标准溶液加入量至0.001 m L,并且通过加大碘化钾用量使得滴定中产生的碘化亚铜被高浓度的I-溶解,消除对碘的吸附影响。本法应用于铜含量为24.2%~59.09%的铜精矿、黄铜矿、铅黄铜国家标准物质分析,相对标准偏差(RSD,n=10)0.3%,极差仅为0.13%、0.21%、0.29%,优于手动目视滴定法。本法提高了铜矿石分析的自动化程度,适用于精确测定铜含量大于0.5%尤其是10%以上的铜矿石。  相似文献   

2.
自动电位滴定仪具有操作简便、测定速度快的优势,减少了人为操作的影响,本文使用自动电位滴定仪测定海洋沉积物中有机碳的含量,并与国家标准(GB 17378.5—2007)中根据滴定过程中溶液颜色变化用肉眼判定滴定终点的方法进行了对比分析,确定通过仪器自动判断滴定终点实现准确测定的可行性。结果表明:自动电位滴定的方法检出限为0.029%,人工肉眼判定终点的方法检出限为0.086%,在滴定终点判定方面两种方法无显著性差异,但自动电位滴定仪的准确度和精密度更优,在一定程度上可代替肉眼判定滴定终点。实际应用过程中也发现,当滴定的溶液体系由于氧化还原反应、络合作用等影响因素使电位变化较为复杂时,自动电位滴定仪有可能会得到多个等当点而无法判断哪个等当点是真正的目标等当点,此时需要利用肉眼进行辅助确定。  相似文献   

3.
自动电位滴定测定锰矿石中锰的方法研究   总被引：3，自引：3，他引：0  
多批次的锰矿石锰含量滴定分析消耗大量人工,随着自动化电位滴定仪的普及,利用仪器完成容量滴定成为可能,而将手工滴定向自动电位滴定移植是当前需要解决的课题。本文建立了一套自动电位滴定仪测定锰矿石中锰含量的方法,确定了相关滴定参数和等当点识别标准。锰矿石样品采用盐酸、磷酸分解,硝酸去除碳和有机物,高氯酸氧化,形成样品溶液。自动电位滴定仪先用硫酸亚铁铵标准溶液对预先移取的重铬酸钾标准溶液和标定空白溶液分别进行氧化还原滴定,用铂复合电极指示,计算得到硫酸亚铁铵标准溶液浓度,再对样品空白溶液和样品溶液进行氧化还原滴定,得到样品锰含量,方法检测范围为5%～60%。采用本法分析国家一级标准物质,测定结果的准确度和精密度高;分析多个产地不同水平的锰矿石样品,测定结果与手工方法进行对照,经t检验无显著性差异。建立的滴定方法自动化程度高、方法稳健,适用于冶炼企业、港口商检等行业,具有推广价值。  相似文献   

4.
根据亚钛还原钒酸铵滴定法的测定原理,对样品溶样、过滤洗涤、还原氧化、滴定等操作方法做了改进。磷酸-盐酸-过氧化氢混合酸低温溶解样品,离心分离过滤,亚钛还原UO22+,过量亚钛用次溴酸钠氧化,尿素亚硝酸钠混合液进一步氧化未被次溴酸钠氧化的微量低价杂质。在小体积(10 mL)范围内,用低浓度钒酸铵标准溶液进行滴定操作测定微量铀,滴定终点清晰,相对标准偏差(RSD,n=5)为0.05%~0.07%,方法测定下限为0.001%,适于矿石和矿渣中0.001%~0.01%铀的测定。方法简便、快速,能满足生产和科研的需要。  相似文献   

5.
基体分离-电位滴定法测定高硫金属矿中的微量氯   总被引：2，自引：1，他引：1  
使用碳酸钠-氧化锌混合碱焙烧样品,将硫化物矿中的低价硫转化为硫酸盐或高价硫,过滤分离基体,采用电位滴定法测定硫化物矿(铜精矿、锌精矿、硫铁矿)中的微量氯,消除由于硫化银沉淀的产生对氯化银测定结果的干扰。通过电位突越,确定滴定终点,消除色度和浊度对滴定终点的影响。采用电极电位-浓度二次微商滴定曲线,计算滴定终点。对混合碱的选择及加入量、焙烧温度、溶液酸度、测定温度、滴定介质以及基体和共存元素的干扰进行了试验。方法精密度(RSD,n=9)均小于9%,回收率为94.1%~105.6%。  相似文献   

6.
地下水中六项指标(pH、总碱度、氯离子、钙离子、镁离子及硫酸根)的分析需要对每个指标单独进行取样检测,步骤繁琐且效率较低。同时总碱度、氯离子、钙离子、镁离子及硫酸根通常采用手动目视滴定,检测结果存在人为操作误差,精密度和准确度相对较差。本文建立了准确快速测定地下水中六项指标的分析方法,只需2次取样,采用自动电位滴定仪自动判定终点,加液器可精确控制标准溶液加入量至0. 1μL,并且通过调整检测顺序、溶液酸度和加入掩蔽剂的方法消除相互干扰。本方法的加标回收率为93. 5%～120. 0%,相对标准偏差(RSD,n=10)为0. 18%～11. 33%。电位滴定法得到的数据相比标准方法的平行性更好,尤其是当所测定水样较为浑浊或者有颜色时测定数据更稳定。  相似文献   

7.
时晓露  马玲  刘瑱  朱炳文 《安徽地质》2016,26(2):158-160
测定岩石类样品中的Zr含量,酸溶经常结果偏低,碱溶通常较难获得较低的检出限。本文选取了不同岩性的岩石类国家标准物质GBW07104、GBW07106、GBW07107、GBW07114、GBW07835、GBW07836、GBW07837作为实验样品,分别采用酸溶后复溶、Na2O2碱熔、赶硅后Na2CO3和Na2B4O7三种前处理方法,对电感耦合等离子体质谱仪进行参数优化后上机测定,结果表明:对样品赶硅后加入少量Na2CO3和Na2B4O7混合试剂高温熔融处理岩石样品后,锆的测量值准确度高,而且获得了最低的检出限,同时缩短了方法流程,操作快捷。该方法更适用于各类岩石样品锆的测定。  相似文献   

8.
磁铁矿中磁性物成分的测定及可选性评价   总被引：3，自引：3，他引：0  
对磁铁矿样品分别用磁选管和手工内磁选法进行磁选,并对原矿样品和样品的磁性物中TFe、P、S、V2O5、TiO2、SiO2、Al2O3、CaO、MgO、Sn、Cu、Pb、Zn的含量进行测定.分析结果表明,采用手工内磁选和磁选管对磁铁矿进行磁选所得的结果一致,为了简便操作,本文均采用手工内磁选法选出磁性物.A矿区磁性铁(mFe)含量(22.42％)比B矿区mFe含量(22.59％)低,但A矿区样品的磁性物中TFe含量(磁铁精矿品位)大于66％,比B矿区样品的磁性物中TFe含量(小于57％)高,A矿区的磁铁矿选矿效果明显好于B矿区,说明对磁性物中TFe含量的测定能够更好地反映矿石的可选性.原矿样品中P、S的含量分别为0.328％、0.271％,而样品的磁性物中P、S的含量为0.021％、＜0.005％,均达到铁矿石冶炼标准;原矿样品中V2O5、TiO2的含量分别为0.156％、1.37％,而样品的磁性物中V2O5、TiO2含量分别为0.823％、13.62％,达到了铁矿石冶炼标准.原矿样品的(CaO+MgO)/(SiO2 +Al2O3)值为0.876,为自熔性矿石,而其磁性物的(CaO+ MgO)/(SiO2+Al2O3)值为0.453,为酸性矿石.由此说明,单纯测定原矿样品中的各成分尚不能对磁铁矿的可选性进行科学性评价,只有进一步测定磁铁矿的磁性物中各成分的含量,才能够对磁铁矿进行可靠的评价.本文通过对磁铁矿中磁性物成分的测定,为磁铁矿的选冶性能提供了新的评价方法.  相似文献   

9.
改进了三酸(HCl-HNO3-HF)或四酸(HCl-HNO3-HF-HClO4)溶矿对难溶元素分解不彻底及对易挥发元素测定结果不稳定的现象,建立了地质样品中15个稀土元素及其常规微量元素一次溶矿、一次测定的分析方法,提高了分析质量。采用HCl-HNO3-HF-HClO4-H2SO4混合酸一次分解样品,用50%的逆王水复溶提取后定容,以Rh为内标元素,三通在线进样方式,电感耦合等离子体质谱法同时测定地质样品中45个元素的含量。讨论了分解方法对易挥发元素、难溶元素的影响,对岩石标准物质(GBW07106)、水系沉积物标准物质(GBW07303)和土壤标准物质(GBW07429)的测定值与标准值相一致,方法精密度为0.03%～4.97%。方法准确度高,简单、快捷、实用。  相似文献   

10.
电感耦合等离子体发射光谱法测定硫化物矿中的高含量铅   总被引：3，自引：2，他引：1  
铅含量高的硫化物矿在氧化性酸的存在下极易形成硫酸铅沉淀而影响样品中铅的准确测定。文章通过王水-双氧水分解和高温灼烧后王水分解两种不同的样品处理方法,有效地去除样品中的硫,配合使用高盐雾化器采用电感耦合等离子体发射光谱法对硫化物矿石中的高含量铅进行测定。王水-双氧水分解可以测定硫化物矿中的铅、银和锑,高温灼烧后王水分解只能测定铅;两种样品处理方法均操作简便,具有准确度好、精密度高、分析速度快等优点。用这两种样品处理方法10次测定铅精矿(GBW 07167)中的铅,精密度(RSD)分别为0.38%和0.56%,相对误差分别为-0.41%和0.14%;测定方铅矿(GBW 07269)中铅精密度分别为0.76%和0.66%,相对误差分别为0.82%和0.45%。  相似文献   

11.
The saturation surface of pseudobrookite (Fe2TiO5) was determined for melts in the system SiO2-Al2O3-K2O-FeO-Fe2O3-TiO2 at 1400° C and 1 atm. The variation in concentrations of Fe2O3, TiO2 and Fe2TiO5 in liquids can be used to infer relative changes in activity coefficients of these components with changing K2O/(K2O+Al2O3) of the melts. Saturation concentrations of these components are low and relatively constant in the peraluminous melts and increase with increasing K2O/(K2O+Al2O3) in peralkaline liquids. The activity coefficients of Fe2O3 and TiO2 and Fe2TiO5, therefore, are higher in peraluminous liquids than in peralkaline liquids in this system. In addition, the iron redox ratio was measured as a function of K2O/(K2O+Al2O3) for liquids just below the saturation surface; was fixed so all variations in redox ratio are entirely due to changes in melt composition. The redox ratio from unsaturated liquids was applied to saturated liquids where redox analysis of the glass is impossible. The homogeneous equilibrium experiments indicate that the activity coefficient of Fe2O3 relative to that of FeO is significantly greater in peraluminous melts than peralkaline melts. Both the heterogeneous and homogeneous equilibria suggest that in peralkaline liquids K+in excess of that required to charge balance tetrahedral Al+3 is used to stabilize both Fe+3 and Ti+4. Calculations show that ferric iron and titanium compete equally effectively for charge-balancing potassium but neither can outcompete aluminum. The observed changes in solution properties of Fe2O3 and TiO2 in the synthetic melts are used to explain variations in Fe-Ti oxide stabilities in natural peraluminous and peralkaline rhyolites and granites. Since the activity coefficients of both ferric iron and titanium are significantly higher in peraluminous liquids than in peralkaline liquids, Fe-Ti oxides should occur earlier in the crystallization sequence in peraluminous rhyolites than in peralkaline rhyolites. In addition, iron will be reduced in peraluminous granites and rhyolites relative to peralkaline ones under comparable P, T, and . Finally, observed crystallization patterns for minerals containing highly charged cations other than ferric iron and titanium are evaluated in the context of this and other experimental studies.  相似文献   

12.
The uncommon Mg-rich and Ti-poor Zhaoanzhuang serpentine-magnetite ores within Taihua Group of the North China Craton(NCC) remain unclear whether the protolith was sourced from ultramafic rocks or chemical sedimentary sequences. Here we present integrated petrographic and geochemical studies to characterize the protoliths and to gain insights on the ore-forming processes. Iron ores mainly contain low-Ti magnetite(TiO_2 ~0.1 wt%) and serpentine(Mg#=92.42–96.55), as well as residual olivine(Fo=89–90), orthopyroxene(En=89–90) and hornblende. Magnetite in the iron ores shows lower Al, Sc, Ti, Cr, Zn relative to that from ultramafic Fe-Ti-V iron ores, but similar to that from metamorphic chemical sedimentary iron deposit. In addition, interstitial minerals of dolomite, calcite, apatite and anhydrite are intergrown with magnetite and serpentine, revealing they were metamorphic, but not magmatic or late hydrothermal minerals. Wall rocks principally contain magnesian silicates of olivine(Fo=83–87), orthopyroxene(En=82–86), humite(Mg#=82–84) and hornblende [XMg=0.87–0.96]. Dolomite, apatite and anhydrite together with minor magnetite, thorianite(Th-rich oxide) and monazite(LREE-rich phosphate) are often seen as relicts or inclusions within magnesian silicates in the wall rocks, revealing that they were primary or earlier metamorphic minerals than magnesian silicates. And olivine exists as subhedral interstitial texture between hornblende, which shows later formation of olivine than hornblende and does not conform with sequence of magmatic crystallization. All these mineralogical features thus bias towards their metamorphic, rather than magmatic origin. The dominant chemical components of the iron ores are SiO_2(4.77–25.23 wt%), Fe_2O_3 T(32.9–80.39 wt%) and MgO(5.72–27.17 wt%) and uniformly, those of the wall rocks are also SiO_2(16.34–48.72 wt%), Mg O(16.71–33.97 wt%) and Fe_2O_3 T(6.98–30.92 wt%). The striking high Fe-Mg-Si contents reveal that protolith of the Zhaoanzhuang iron deposit was more likely to be chemical sedimentary rocks. The distinct high-Mg feature and presence of abundant anhydrite possibly indicate it primarily precipitated in a confined seawater basin under an evaporitic environment. Besides, higher contents of Al, Ti, P, Th, U, Pb, REE relative to other Precambrian iron-rich chemical precipitates(BIF) suggest some clastic terrestrial materials were probably input. As a result, we think the Zhaoanzhuang iron deposit had experienced the initial Fe-Mg-Si marine precipitation, followed by further Mg enrichment through marine evaporated process, subsequent high-grade metamorphism and late-stage hydrothermal fluid modification.  相似文献   

13.
熔融制样X射线荧光光谱法测定铜矿石中16种主次量元素   总被引：1，自引：1，他引：0  
铜矿石类型繁多,矿石赋存状态各异,成分复杂。在现有的铜矿石熔融制样X射线荧光光谱（XRF）分析方法中,选取标准物质个数和矿石类型少、分析范围宽,与实际样品类型相差太大,且制备的熔融片质量不高。本文选用铜含量既有良好浓度变化范围,又符合铜矿石常见含量的包括铜金银铅锌钼铜镍等各类矿石的24个标准物质,以四硼酸锂-偏硼酸锂-氟化锂为混合熔剂,熔剂与样品质量比为30：1,以溴化锂为脱模剂,改进样品预处理方式,将通常采用样品预氧化后或熔融中加入脱模剂的方式,改进为加入脱模剂后再用混合熔剂完全覆盖的方法制备了高质量的熔融片,建立了XRF测定铜矿石中铜锌铅硅铝铁钛锰钙钾镁钼铋锑钴镍16种元素的分析方法。分析铜矿石国家标准物质GBW 07164、GBW 07169,各元素的精密度（RSD）为0.1%~5.4%。分析国家标准物质GBW 07163（多金属矿石）、GBW 07170（铜矿石）的测定值与标准值相符;分析实际铜矿石样品,铜锌铅钼铋锑钴镍的测试结果与电感耦合等离子体发射光谱法和其他方法的测定值相符。本文方法扩大了基体的适应性,提高了实际应用价值。  相似文献   

14.
The study area forms part of an emerging iron ore province of southern Cameroon. Geochemistry analyses reveal that the siliceous itabirite has a very simple chemical composition, with Fe2O3 and SiO2 representing more than 96 wt.% of the average composition; suggesting chemical precipitates of silica and iron. Low Al2O3 and TiO2 concentrations and a weak positive correlation between them point to a minor detrital component in the precipitated marine sediments. The Si/Al ratio (average 52.7) indicates the hydrothermal origin of the studied itabirite. The Al–Si discrimination diagram supports this interpretation through the plot of all data in the hydrothermal field. The studied samples have low iron content (about 39.32% Fe), high gangue content (40.97% SiO2 and 1.3 % Al2O3) and low concentration of the deleterious elements (0.16 % P and < 0.01% S). The main gangue mineral is silica which can be efficiently removed from iron ores during preparation of raw materials for the blast furnace process. According to commercial standards for crude iron ores, it may be concluded that the Zambi iron ores are a low‐grade magnetic ore that can be profitably exploited for the production of iron for steel production.  相似文献   

15.
宋萍  温宏利 《岩矿测试》2016,35(4):384-388
分析地质样品中的溴碘,目前常用的提取方法有半熔法、稀氨水密封溶样法和热解法,但由于元素含量低、易损失,样品分解和溴碘的提取过程是主要的误差来源。本文改进了传统热解法的吸收装置,用液氮冷凝吸收代替常规的碱溶液吸收,提取地质样品中的溴碘,用电感耦合等离子体质谱法测定其含量。以标准偏差的10倍计算,稀释倍数为50,溴碘的检出限分别为0.06μg/g、0.01μg/g,低于传统热解法和半熔法,略高于稀氨水密封溶样法;精密度(RSD)为6.4%~21.0%。本方法相对于传统的碱溶液吸收热解法,减少了碱试剂的引入,降低了基体空白和稀释倍数,提高了精密度,操作较半熔法简便,可作为稀氨水密封溶样法的一种补充方法。因此,对于土壤和水系沉积物,宜采用稀氨水密封溶样法;对于岩石以及采用稀氨水密封溶样法难以完全提取的样品,可采用本方法。  相似文献   

16.
Karstic bauxite deposits are widespread in Central Guizhou Province, SW China, and high-grade ores are frequently sandwiched with overlying coal and underlying iron-rich layers and form a special “coal–bauxite–iron” structure. The Lindai deposit, which is one of the most representative karstic bauxite deposits in Central Guizhou Province, was selected as a case study. Based on textural features and iron abundances, bauxite ores in the Lindai deposit are divided into three types of ores, i.e., clastic, compact, and high-iron. The bauxite ores primarily comprise diaspore, boehmite, kaolinite, illite, and hematite with minor quartz, smectite, pyrite, zircon, rutile, anatase, and feldspar. The Al2O3 (53–76.8 wt.%) is the main chemical contents of the bauxite ore samples in the Lindai district, followed by SiO2, Fe2O3, TiO2, CaO, MgO, S, and P etc. Our geological data on the Lindai deposit indicated that the ore-bearing rock series and its underlying stratum have similar rare earth elements distribution pattern and similar Y/Ho, Zr/Hf, and Eu/Eu1 values; additionally, all ore-bearing rock samples are rich in MgO (range from 0.16 wt.% to 0.68 wt.%), and the plots of the dolomites and laterites lie almost on or close to the weathering line fit by the Al-bearing rocks in Zr vs. Hf and Nb vs. Ta diagrams; suggesting that the underlying Middle Cambrian Shilengshui Formation dolomite is the parent rock of bauxite resources in the Lindai district.Simulated weathering experiments on the modern laterite from the Shilengshui Formation dolomite in the Lindai bauxite deposit show that hydrogeological conditions are important for karstic bauxite formation: Si is most likely to migrate, its migration rate is several magnitudes higher than those of Al and Fe under natural conditions; the reducing inorganic acid condition is the most conducive to Al enrichment and Si removal; Fe does not migrate easily in groundwater, Al enrichment and Fe removal can occur only in acidic and reducing conditions with the presence of organic matter.The geological and experimental studies show that “coal–bauxite–iron” structure in Lindai deposit is formed under certain hydrogeological conditions, i.e., since lateritic bauxite or Al-rich laterite deposited upon the semi-closed karst depressions, Si can be continuously removed out under neutral/acidic groundwater conditions; the coal/carbonaceous rock overlying the bauxitic materials were easily oxidized to produce acidic (H2S, H2SO4, etc.) and reductant groundwater with organic materials that percolated downward, resulting in enrichment of Al in underlying bauxite; it also reduced Fe3+ to its easily migrating form Fe2+, moving downward to near the basal carbonate culminated in precipitating of ferruginous (FeS2, FeCO3, etc.) strata of the “coal–bauxite–iron” structure. Thus, the bauxitic materials experienced Al enrichment and Si and Fe removal under above certain hydrogeological conditions forming the high-quality bauxite.  相似文献   

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