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1.
姚玉玲  吴丽琨  刘卫  李刚 《岩矿测试》2015,34(2):224-228
电感耦合等离子体发射光谱法(ICP-AES)在铌钽测定方面获得广泛应用,但灵敏度较低、检出限较高,不能满足矿石和选冶样品中的低含量铌钽的检测要求。本文优化了ICP-AES测试过程中多种有机试剂的增敏效果,结果表明:样品采用氢氟酸-硝酸-硫酸敞开酸溶,选择乙醇作增敏剂,雾化效率最佳,当乙醇浓度为6%时,原子线Nb 292.781 nm、Ta 240.063 nm的灵敏度分别增强了180.5%和265.5%;铌的检出限由不加乙醇的5.85μg/g降低到3.22μg/g,钽的检出限由不加乙醇的10.65μg/g降低到5.03μg/g;Nb2O5回收率为97.7%~101.9%,Ta2O5回收率为96.8%~97.2%;方法精密度(RSD)6%。本方法适用于低含量和高含量铌钽的同时测定,尤其有利于选冶流程样品中同一批次的精矿、中矿和尾矿的同时测定,克服了以往分别采用光谱法和质谱法测定所产生的仪器间误差导致回收率吻合程度不好的缺陷。  相似文献   

2.
在线萃取流动注射法快速测定水体中阴离子表面活性剂   总被引：1，自引：0，他引：1  
王丽平  田芹  江林  张卓勇 《岩矿测试》2009,28(6):553-556
采用在线萃取预处理功能模块,配合流动注射分析法对水体中阴离子表面活性剂进行了快速测定。通过对萃取模块结构的优化,解决了测试过程中峰形拖尾、接口处氯仿渗出以及萃取膜频繁更换的问题。方法检出限为10.2μg/L;阴离子表面活性剂的浓度在50.0~1 000.0μg/L有良好的线性(相关系数0.999 3);精密度(100μg/L,n=7)为2.5%;实际水样的加标回收率为97.8%~112.6%;检测频率为18个样/h。方法操作简便,与传统的亚甲基蓝分光光度法比较,样品测试速度快,分析效率高,可以满足现场水质快速批量检测的要求。  相似文献   

3.
稀有多金属矿各类选矿样品中同一元素的含量相差较大,且同一样品中各元素的含量也有较大差异,如铌钽锂铍在尾矿和原矿中的含量只有几十至几百g/g,而在精矿中的含量达到百分之几至百分之几十,伴生元素如钾、钠在不同样品中也有较大差异。应用ICP-OES法测定铌钽锂铍等元素通常采用三酸或四酸分解样品,多是测定尾矿、原矿及部分中矿样品中较低含量的铌钽锂铍,且同一测定体系中只测定了一种或两种元素。本文采用氢氟酸-硝酸-盐酸-高氯酸-硫酸分解样品,以3~4滴氢氟酸+5%硫酸+5%过氧化氢提取体系替代常规的有机酸(酒石酸等)提取体系,实现了应用ICP-OES同时测定稀有金属矿选矿试验各阶段产品中不同含量的铌钽锂铍钾钠铷铁钛等元素。各元素的谱线强度在0~500μg/mL浓度范围内呈良好的线性关系,相对标准偏差为0.61%~4.77%(n=6)。该方法提高了选矿全流程样品中各类元素的分析效率,已在选冶试验流程样品分析中得到了应用。  相似文献   

4.
稀有多金属矿各类选矿样品中同一元素的含量相差较大,且同一样品中各元素的含量也有较大差异,如铌钽锂铍在尾矿和原矿中的含量只有几十至几百!g/g,而在精矿中的含量达到百分之几至百分之几十,伴生元素如钾、钠在不同样品中也有较大差异。应用敞口酸熔-电感耦合等离子体发射光谱法(ICP-OES)测定铌钽锂铍等元素通常采用三酸或四酸分解样品,多是测定尾矿、原矿及部分中矿样品中较低含量的铌钽锂铍,且同一测定体系中只测定了一种或两种元素。本文采用氢氟酸-硝酸-盐酸-高氯酸-硫酸分解样品,以3~4滴氢氟酸+5%硫酸+5%过氧化氢提取体系替代常规的有机酸(酒石酸等)提取体系,实现了应用ICP-OES同时测定稀有金属矿选矿试验各阶段产品中不同含量的铌钽锂铍钾钠铷铁钛等元素。各元素的谱线强度在0~500μg/mL浓度范围内呈良好的线性关系,相对标准偏差为0.37%~4.77%(n=6)。该方法提高了选矿全流程样品中各类元素的分析效率,已在选冶试验流程样品分析中得到了应用。  相似文献   

5.
针对煤层气排采过程中煤粉产出易造成卡泵、埋泵等问题,以韩城区块太原组11号煤为研究对象,采用阴离子分散剂十二烷基硫酸钠SDS,以煤粉粒径、分散剂用量、煤粉浓度等作为影响因素,探究了分散剂对煤粉分散稳定性的影响规律,分析了分散剂与煤粉之间的相互作用机理。结果表明:不同粒径煤粉悬浮液煤粉分散效果不同,随着煤粉粒径增大,SDS悬浮液煤粉浓度出现不同程度下降;适宜的SDS分散剂用量,低的煤粉浓度,有利于煤粉在悬浮液中稳定分散,SDS分散剂质量浓度1.5~2.5 g/L,煤粉质量浓度小于30 g/L时较为适合煤粉稳定分散;分散剂的加入改变了悬浮液黏度,黏度的升高增加了携粉能力,同时不会影响洗井工艺中洗井液的返排。   相似文献   

6.
利用火焰光度法测定水样中钾离子,高含量钠对钾测定有一定的影响。为此,本文通过对0.50 mg／L、2.00 mg／L、5.00 mg／L、10.00 mg／L、20.00 mg／L钾的标准溶液中分别加入50 ~ 3 000 mg／L不同浓度的钠进行了实验,探讨了不同浓度的钠对钾测定的影响,即对于钾的浓度小于5.00 mg／L时,钠的浓度对钾的测定结果影响不明显;对于钾的浓度大于5.00 mg／L时, 钠的浓度将影响钾的测定结果,且随着钾离子含量增加,高含量钠对钾的测定影响越明显,造成测定结果偏低。  相似文献   

7.
地下水中钙和镁的离子色谱法同时测定   总被引：2，自引：0，他引：2  
改进了离子色谱分析地下水中钙和镁的方法。以IonPac CS12A为分离柱,稀盐酸为淋洗液,电导检测器检测,对地下水中的锂、钾、钠、钙和镁进行同时测定。方法具有较宽的线性范围和较高的灵敏度,钙、镁的浓度分别在0～500mg/L和0～250mg/L内呈良好的线性关系;钙的检出限为1.50μg/L,镁的检出限为0.89μg/L。对不同浓度钙、镁水质标准样品进行分析测定,同时对实际样品进行不同稀释倍数分析验证,方法精密度(RSD,n=8)为0.19%～1.89%,无显著的基体效应影响。方法可满足全国地下水调查评价规范要求,适于地下水样品中锂、钾、钠、钙和镁离子的同时测定。  相似文献   

8.
文章描述了一种火焰原子吸收光谱法测定矿物及精矿中铌钽的方法。样品经KHSQ_4熔融,柠檬酸提取,在1000μg/ml Al存在下直接喷入N_2O—C_2H_2火焰。Al的存在不仅对Nb、Ta吸收信号有较强的增敏作用。而且还能消除Nb、Ta相互干扰及Ca、Ti、V对Nb、Ta的干扰。本法测定Nb、Ta的炅敏度分别为8.8μg/ml和13.7μg/ml。与使用有毒、危害较大的HF方法灵敏度相当或有所提高(Nb 22μg/ml、Ta 11μg/ml)。此法适合于矿物及精矿中含量大于5％Nb_2O_5和Ta_2O_5的测定。  相似文献   

9.
混合表面活性剂对长石、石英浮选分离的影响   总被引：1，自引：0，他引：1  
采用单矿物浮选、Zeta电位和芘荧光探针,研究由DDA和SDS组成的阴阳离子混合表面活性剂在不同的浮选条件下对长石、石英分离效能影响以及表面活性剂在矿物表面的吸附行为。结果表明:在相同浓度阴阳离子混合表面活性剂中,长石的疏水性要强于石英;Zeta电位在DDA∶SDS=1∶1时主要由阳离子决定,在DDA∶SDS=1∶2、1∶3时由阴离子决定。芘荧光探针结果表明:在pH=2.0,长石和石英表面极性在低浓度混合表面活性剂中与浓度呈负相关;在DDA∶SDS=1∶1、浓度为4×10-4 mol/L时,混合表面活性剂在矿物表面形成半胶束,且长石表面形成半胶束浓度低于石英。当DDA∶SDS=1∶2、1∶3时,长石表面形成半胶束浓度提高,而石英未能在实验条件内形成胶束。综合而言,在同一混合表面活性剂条件下,长石表面疏水性强于石英。  相似文献   

10.
混酸溶解矿石样品,在酒石酸介质中,用电感耦合等离子体发生光谱法(ICP-AES)测定溶液中的铌钽。该方法ρ(Nb2O5)和ρ(Ta2O5)在0～20 μg/mL时,铌钽原子发射光谱强度与浓度呈良好的直线关系,Nb、Ta标准曲线相关系数尺分别为0.999 9和0.999 7。检出限分别为0.023 μg/mL和0.072 μg/mL。本方法测定标准样品,测定值与认定值相符。对实际样品分析,Nh、Ta的相对标准偏差(n=6)分别为0.42％～2.3％和1.8％～3.3％,加标回收率均为97％～103％,适合地质找矿、选冶等领域的样品测试。  相似文献   

11.
滇黔地区的"白泥塘层"与锰矿具有密切的成因联系,前人对其地球化学特征研究时关注的主要是硅质灰岩全岩,并非硅质成分本身,而硅质岩全岩能否真实地反映"白泥塘层"中硅质的来源有待研究。本文以滇黔地区"白泥塘层"硅质灰岩为研究对象,用盐酸去除硅质灰岩中的碳酸盐矿物,获得成分较为单一的硅质组分,采用ICP-MS和ICP-OES测定全岩与去除碳酸盐的硅质组分中的微量元素,通过对比两者的微量元素地球化学特征研究"白泥塘层"中硅质的来源问题。结果表明:去除碳酸盐的硅质组分的Th/U=0.02~0.05,低于全岩的Th/U值(0.08~0.2),Eu/Eu*=0.86~1.54(均值1.15),显示为正Eu异常,此特征不同于全岩(全岩的Eu/Eu*=0.87~0.93,均值0.90,显示为弱的负Eu异常);硅质组分及全岩的稀土含量均表现为轻稀土较重稀土富集,但硅质组分中的轻稀土所占比重大于全岩。以上特征确切地表明了"白泥塘层"硅质灰岩中的硅质成分来自于热水,对于解释二叠系时期锰矿的形成具有重要的指示意义。  相似文献   

12.
The aim of this study was to select the appropriate surfactant for the remediation of dichlorodiphenyltrichloroethane-contaminated soil using an in situ foam-flushing technique. The research investigated the performance of the nonionic surfactants polyethylene glycol octyl phenyl ether, polysorbate, and polyoxyethylene lauryl ether, as well as the anionic surfactant sodium dodecyl sulfate, in foam static characteristics, solubility enhancement of dichlorodiphenyltrichloroethane, adsorption loss onto soil, and dichlorodiphenyltrichloroethane desorption from contaminated soil using a foam-flushing approach. Considering the above four criteria, the overall performance suggested polyethylene glycol octyl phenyl ether should be selected for the remediation of dichlorodiphenyltrichloroethane-contaminated soil due to its better foamability and stability, relatively high solubilization ability for dichlorodiphenyltrichloroethane, and greatest contaminant desorption efficiency from soil via foam flushing. Results of the dichlorodiphenyltrichloroethane desorption experiments showed that desorption efficiency of dichlorodiphenyltrichloroethane by different surfactants was largely influenced by foam static characteristics and solubility enhancement of dichlorodiphenyltrichloroethane rather than adsorption loss onto soil, which indicated that foam static characteristics and solubilization ability of surfactants were two key criteria for selection of high-performance foam surfactant.  相似文献   

13.
Surface tension of sedimentary fulvic acid (FA) and humic acid (HA) with molecular weight from < 10,000 to > 300,000 was measured at 5°C and 25°C, over a wide range of concentrations (0.114-107.4 g/l) at pH 8. HA was in the form of sodium humate. Surface tension decreases with an increase in HA and FA concentration and both HA and FA were found to be surface active materials with FA exhibiting the lowest surface tension (31 dynes/cm).Plots of surface tension vs. log concentration gave two straight lines with a break at a certain concentration similar to surfactants. From the concentration at the break point, aggregation concentration (AGC) was determined. For HA with molecular weight above 10,000, the AGC decreased with an increase in molecular weight. The more hydrophobic the HA, the greater was the tendency to form aggregates. Surface excess (surface concentration) was determined (2.3 × 10?10?5.5 × 10?10mol/cn2) from the slope of the plot of surface tension vs. log concentration for concentrations lower than the AGC. Adsorption of HA into the surface layer increased with increasing molecular weight of HA.  相似文献   

14.
The maximum flotation response for three naturally occurring calcium minerals, apatite, calcite and fluorite with sodium oleate collector correlated directly with the minimum interfacial tension of the air/solution interface. For fluorite and apatite the minimum surface tension occurred about the mid-pH region and was attributed to the formation of pre-micellar associated species in solution. In the case of calcite the minimum was observed at high pH since the presence of high concentrations of calcium ions in solution appeared to reduce the concentration of amphililic species in the low and mid-pH regions.Microelectrophoresis data demonstrated that the three minerals acquired a negative charge in sodium oleate solution, resulting from adsorption of oleate species on the mineral surfaces.The flotation behaviour of the systems were shown to be related to the species distribution diagrams suggesting that the role of the acid soap dimer, soap dimer, molecular and lattice species could make a significant contribution to the character and composition of the interfacial films.High flotation response was explained by strong adhesion between the hydrophobic particle and bubble. It was suggested that the reduction in surface tension may not be the major factor contributing to the flotation efficiency but indicated the presence of associated surfactant species in solution which could also synergistically adsorb at the solid/liquid interface, increasing the hydrophobic character of the mineral surface. This would maximize the magnitude of the contact angle and hence the strength of the adhesion between particle and bubble. This adsorption behaviour is not in general agreement with conventionally non-hydrolyzable collector theory which is usually based on electrostatic models.  相似文献   

15.
An experimental study was made to identify surfactants which are effective for removal of copper from dilute aqueous solution (100–500 ppm) by precipitate flotation as the sulfide, and which at the same time can be recovered from the CuS product for recycle. Batch flotation experiments confirmed that a cationic surfactant was necessary for flotation of CuS from such dilute suspensions; however, no satisfactory way could be found for recovering cationic surfactants from the CuS. This led to consideration of amphoteric surfactants, which are cationic at low pH and anionic at high pH. It was found that a change to negative, rather than simply neutral, charge was required for efficient surfactant recovery. It was further found, through the assistance of experiments in which the CuS suspension was agitated with solvents, that certain functional groups which interact chemically with the CuS surface should also be absent from the surfactant molecule. Following this logic, Amphoterge K-2 (Lonza Chemical Co.) was identified as a suitable surfactant, provided CuS was precipitated with S2? in excess. Tests established that 95% of adsorbed Amphoterge K-2 could be recovered by raising the pH to 11 and boiling the suspension for one hour, followed by decanting. Surfactant thus recovered was effective in a second flotation test. Foamate solids settled rapidly; such behavior would help reduce the consumption of chemicals for the pH change.Column flotation studies were made using Amphoterge K-2 for removal of Cu2+ present at 100 ppm and pH = 2. High removals of CuS could be obtained at concentrations of surfactant above about 25 ppm, for which conditions a substantial fraction of the surfactant remains in solution rather than being adsorbed onto the CuS. The recovery of CuS would be improved by introducing the surfactant in a separate feed, below the feed of CuS suspension. Adding some surfactant in the CuS feed, as well as in a lower feed, gave an even better recovery of CuS (99.8%) at sufficiently high surfactant loadings.  相似文献   

16.
研究了不同表面活性剂对不同等级水镁石纤维的松解效果，通过对纤维悬浮液叩解度、粘度、纤维表面Zeta电位、纤维混凝土强度等的研究，并经扫描电镜分析，证明了化学松解工艺对水镁石纤维具有较好地劈分作用。表面活性剂种类及用量对纤维的叩解度、纤维的表面电位、悬浮液粘度均有影响，对不同等级纤维的影响有差异。随表面活性剂用量增加，纤维的叩解度、纤维表面的负电荷量、悬浮液的粘度一般均呈增加趋势。经过化学分散试验，水镁石纤维得到了较好松解，纤维直径由微米级下降至纳米级。将水镁石纤维应用于混凝土，抗折强度随纤维叩解度的增加而提高，说明纤维的化学分散有利于纤维对混凝土增强作用的发挥。  相似文献   

17.
The complex mineral assemblages of silica and Fe minerals play a significant role in the transport of compounds in soils and sediments. Five coated sands including Goethite, Lepidocrocite, Ferrihydrite, Hematite and Magnetite were synthesized by a heterogeneous suspension method and characterized by FTIR spectroscopy, XRD, BET surface area and chemical analyses. The synthesis results showed that the degree of coating (mg Fe/g sand) varied with the mineralogy of Fe coating phases, which may have different affinities towards the silica surface. Batch experiments were conducted with two compounds (2,5-dihydroxybenzoic acid and 1-hydroxy-2-naphthoic acid) to quantify the contributions to adsorption from different oxide coatings and compare adsorption characteristics of selected organic acids. Sorption of these compounds to coated sands was examined versus a wide range of conditions (time, pH, ionic strength and sorbate concentration). Because of the attachment of Fe oxide, the coated sand had higher specific surface area, involving a better adsorption efficiency of organic compounds. Mineral surface charge and pH proved to be important for the adsorption of these compounds. The batch results indicated that the degree of coating was the most significant factor enhancing the sorption of aromatic compounds on the surface of sand and the mineralogy of the Fe phase was of less importance.  相似文献   

18.
In this research, effect of temperature, pressure, salinity, surfactant concentration, and surfactant type on interfacial tension (IFT) and critical micelle concentration of Saudi Arabian crude oil and various aqueous phases were investigated. The temperature ranged from ambient condition to 90°C, and the pressures were varied from atmospheric to 4,000 psi (27.58 MPa). Surfactant solutions were prepared using several aqueous phases, i.e., purified water, 10% brine consisting of 100% NaCl, 10% brine consisting of 95% NaCl and 5% CaCl2, and 10% brine consisting of 83% NaCl and 17% CaCl2. Out of 13 commercial surfactants, only three surfactants showed good solubility in pure water and brine. Those are Zonyl FSE Fluorosurfactant®, Triton X-100®, and Triton X-405®. Therefore, they were investigated thoroughly by measuring their efficiency in reducing the crude oil-aqueous phase IFT. Based on this screening process, laboratory surfactant flooding experiments for crude oil recovery were conducted using Triton X-405 and Triton X-100. The chemical flood was made at both original oil in place and at residual oil in place subsequent to conventional water flooding. Based on the obtained results, both surfactants were efficient, and more oil was recovered than that obtained through water flooding. Comparing both surfactant solutions, it was observed that Triton X-405 was more efficient than Triton X-100 at the same surfactant concentration and reservoir conditions.  相似文献   

19.
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20.
One of the environmental concerns in recent decades is the prevalence of different pollutants in soil. Hence, the importance of remediation has led to the development of various methods to remediate polluted soil. Among these methods, soil washing has gained significant attention to treat polluted soils. In this paper, the response surface methodology was applied in order to determine the optimal conditions for total petroleum hydrocarbon remediation using nonionic surfactant Brij35 in soil environment. The effect of different factors in soil washing process including surfactant solution concentration and volume, washing time, age of pollution and frequency of washing are evaluated. The predicted values for total petroleum hydrocarbon remediation efficiency by the response functions are in a very close agreement with experimental data (R-2= 98.75 %). The second order model was developed as experimented response and optimal conditions were obtained by analyzing the contour and surface plots and also by solving the regression equation using LINGO 9.0 software. The optimal concentrations (8 g/L), volume of surfactant solution (500 mL), washing time (75 min), age of pollution (29 days) and frequency of washing (three times) are determined. In this optimal condition, the removal efficiency has been observed to be 93.54 % which conforms to the results of process optimization using response surface methodology. Based on the results, it can be concluded that the response surface methodology is a suitable approach to determine the optimal conditions of soil washing to remediate organic hydrophobic pollutants using the nonionic surfactant Brij35 from the soil.  相似文献   

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