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1.
X射线荧光光谱法测定稀土精矿中的稀土元素分量 总被引：1，自引：1，他引：0
氟碳铈矿、独居石、磷钇矿和风化壳淋积型稀土矿四种稀土精矿样品采用化学法预分离富集,X射线荧光光谱法测定样品中稀土元素和伴生的铀、钍元素含量,选择以硼酸盐为主的混合熔剂高温熔融制样,消除矿物间存在的矿物结构影响,通过加大熔剂稀释比降低元素间的基体效应,人工标准样品绘制标准曲线,用数学校正方法校正元素间的谱线重叠效应。对淋积型稀土矿样品重复测定12次,方法检出限为0.9～42.1μg/g,待测组分的相对标准偏差(RSD)均小于10%,测定结果与电感耦合等离子体质谱法的测定值基本吻合。此方法应用于国家一级标准物质稀土标准样品定值工作,检出限和精密度能够满足分析要求,报出数据被采用率达到100%。 相似文献
2.
电感耦合等离子体发射光谱法测定钼矿石和铜矿石中的铼 总被引：3，自引：0，他引：3
采用氧化镁-硝酸钠-过氧化氢处理试样,不需分离富集,电感耦合等离子体发射光谱法直接测定钼矿石及铜矿石中的铼,筛选了不同溶矿方法和仪器参数条件。方法检出限为0.014μg/g,相对标准偏差(RSD,n=11)小于5.00%,经国家一级钼矿石及铜矿石标准物质分析验证,结果与标准值吻合。 相似文献
3.
流动注射-火焰原子吸收光谱法测定地质样品中的常量金 总被引：4，自引：3，他引：1
样品经室温烧至650℃高温后灼烧保持1.5 h,用浓王水溶解。用泡塑分两次吸附富集样品中的常量金,将富集同一样品中金的两块泡塑置于盛有10 mL 10 g/L硫脲溶液的玻璃试管中,沸水浴保持20 min,使金释放出来,所得溶液应用原子吸收分光光度计采用流动注射测定。对仪器的测定条件进行了优化比较。方法检出限(3σ)为0.022μg/g,精密度(RSD,n=11)小于8.0%,测定范围为0.05～60μg/g。经国家金矿石分析标准物质验证,其测定值与标准值基本一致。 相似文献
4.
Determination of total sulfur in geothermal water by inductively coupled plasma-atomic emission spectrometry 
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下载免费PDF全文 Sulfur speciation and concentration in geothermal water are of great significance for the research and utilization of the water resources. In most situations, it is necessary to determine the total sulfur in geothermal water. In this study, the method was established for the determination of determining total sulfur content — the inductively coupled plasma-atomic emission spectrometry (ICP-AES), with the wavelength of 182.034 nm selected in spectral line of sulfur. It was identified that the optimal working conditions of the ICP-AES instrument were 1 200 W for high frequency generator power 9 mm for vertical observation height, 0.30 MPa atomizer pressure, and 50 r/min analytical pump speed. The matrix interference of the method was eliminated by the matrix matching method. Using this method, sulfur detection limit and minimum quantitative detection limit were 0.028 mg/L and 0.110 mg/L, respectively, whilst the linear range was 0.0–100.0 mg/L. The recovery rate of sample was between 90.67% and 108.7%, and the relative standard deviation (RSD) was between 0.36% and 2.14%. The method was used to analyze the actual samples and the results were basically consistent with the industry standard method. With high analysis efficiency, the method has low detection limit and minimum quantitative detection limit, wide linear range, good precision and accuracy, and provides an important detection method for the determination of total sulfur in geothermal water. 相似文献
5.
Mineralized quartz diorites of the Santo Tomas II porphyry copper-gold deposit, carry high Au contents (average: 1.8 ppm) as well as 160 ppb Pd and 38 ppb Pt. Values of other platinum-group elements (PGE) and rhenium are below the analytical detection limits. There is a significant positive correlation between Au and Cu. The highest Pd values were detected in the most Au- and Cu-rich rocks. Platinum-group minerals (PGM) occur exclusively as inclusions in chalcopyrite and bornite. Potential Pd and Pt contents in sulphide concentrates are estimated at 1.5 g/t and 0.4 g/t, respectively. The precious metal assemblages consist of merenskyite (main PGM), kotulskite, moncheite, native gold, electrum, hessite and petzite. Polyphase fluid inclusions in quartz veinlets, associated with a PGM-bearing bornite-chalcopyrite-magnetite assemblage, are characterized by high salinity (35 to > 60 eq. wt% NaCl) and high trapping temperatures (between 380 and 520 °C). They may represent primary magmatic-hydrothermal fluids, which have been responsible for the transport of Pd, Pt and Au as chloride complexes. 相似文献
6.
沸水浸提-ICP法直接测定土壤有效硼 总被引：2，自引：0，他引：2
土壤中有效硼的含量直接影响到植物的生长情况,因而有效硼的提取方法至关重要.目前最常用的是国家标准测定方法姜黄素比色法和亚甲胺比色法.但这些方法操作流程长,结果易受外界因素的影响,不宜控制.而用沸水浸提ICP法(ICP即电感耦合等离子体发射光谱技术)来代替比色法,不仅能克服这些缺点,更能使有效硼的分析趋于自动化,使得高效、大规模的土壤有效硼的测定分析成为现实.该法为:称取10g土样,按水土比2:1用沸水浸提15min,稍冷却,立即干过滤,滤液即待测液,直接上ICP测定.实验、实践证明,用该法的结果是可靠的,测定限为0.01μg/g. 相似文献
7.
建立了高温燃烧水解-离子色谱测定植物样品中不同含量范围氟的分析方法,色谱条件为Dionex IonPacAS18分离柱(4 mm×250 mm),Dionex IonPac AG18保护柱(4 mm×50 mm),ASRS ULTRAⅡ自动再生微膜抑制器,电导检测器。采用纯水作为吸收介质,使样品溶液与标准溶液基体一致,过滤后可直接测定。样品溶液中常见的Cl-、NO3-、SO24-、PO43-、CO23-、HCO3-等阴离子不干扰F-的测定。为消除样品热解过程中产生的乙酸干扰,对氟含量较高(xx～xxxμg/g)的样品,采用20 mmol/L的NaOH淋洗液等度淋洗,进样体积为25μL;对氟含量较低的样品(0.x～xμg/g),进样体积为100μL。方法具有较宽的线性范围和较好的稳定性,检出限为0.5 mg/kg,适用于痕量分析;应用于灌木枝叶和茶叶等4个氟含量较高(xx～xxxμg/g)的植物标准物质的测定,相对标准偏差(RSD)<6%(n=6);应用于低氟的小麦粉和大米粉样品测定,加标回收率为90%～110%,可以满足不同氟含量植物样品中氟测定的需要,具有自动化程度高、操作简单、对环境友好等特点。 相似文献
8.
Measurements of low-level dissolved-sulfide concentrations in estuarine water from San Francisco Bay have been made using
the sulfide-specific electrode after preservation, separation, and preconcentration of the sulfide species. The separation
and preconcentration were acheived by coprecipitation of ZnS with Zn(OH)2 followed by collection and dissolution of the precipitate, giving concentration factors up to 160-fold Preconcentration provided
sulfide solutions that were adequately measurable within the practical working range of the specific-ion electrode The sulfide
detection limit with the preconcentration step is 0 02 μg/l Spike recoveries in the range of 81 to 10 1% have been achieved
for laboratory-prepared samples having S2− concentrations as low as 0 6 μg/l and 84 to 100% for an estuarine sample spiked in the field with 2 μg/l (S(−II) Positive
correlations have been found between dissolved S(−II) concentrations and concentrations of dissolved Cd, Cu, and Ni, negative
correlations have been found between bisulfide (HS−) activity and activities of Cd2+, Cu2+, and Ag+ species 相似文献
9.
Heavy mineral concentrates (SG 3.3) from the Huai Hin Laep, a tributary of the Huai Kho Lo River in northern Thailand, contain strongly anomalous concentrations of gold. In contrast, the gold content of the associated < 149 μm and <53 μm fractions of the sediment is generally less than the 5 ppb detection limit obtained by a conventional fire assay-atomic absorption spectrometry method. To test for the presence of a gold anomaly at concentrations < 5 ppb, we have used an aqua-regia digestion followed by an Amberlite XAD-8 column preconcentration technique that, when used with a spectrometer that enables full display of the analytical spectrum to optimize baseline analysis, gives a detection limit of 0.1 ppb Au.Gold content of the < 53 μm sediment fraction ranges from 1.0 to 3.1 ppb compared to concentrations that typically range from 1000 to more than 100,000 ppb in the heavy mineral concentrates. However, despite gold concentrations in the sediment being several orders of magnitude lower than those in the heavy mineral concentrates, the downstream dispersion patterns are similar, with gold concentrations increasing at high energy sites and downstream away from the assumed source. These results identify the presence of a greatly diluted gold anomaly in the < 53 μm fraction of the sediments and suggest that transport and deposition of this fine grained gold is controlled by the same sedimentological factors that control the behavior of gold in the sand-size range, between 53 μm and 425 μm. Most important from an exploration standpoint, is that by using a sufficiently sensitive analytical method, meaningful gold dispersion patterns can be recognized at concentrations below 5 ppb. 相似文献
10.
针对野外现场分析的要求,选择微珠比色技术用于江河天然水样和化探样品中铁的分析。以向红菲啰啉为显色剂,硫代硫酸钠掩蔽铜的干扰,方法摩尔吸光系数为1×105L.mol-1.cm-1,精密度(RSD,n=10)为2.5%,适用于0.001μg/g以上的铁的测定。方法用于江河天然水样和化探样品中铁的测定,结果与分光光度法相符。方法在拟定的过程中注意了降低环境污染、降低成本和提高方法的可操作性。建立的方法干扰少,选择性好,对实验环境条件要求不高,满足野外现场分析应用。对于天然水可直接测定;但一般的化探样品由于铁含量较高,需要稀释后再测定。 相似文献
11.
自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲 总被引：2，自引：1，他引：1
铌、钽在氢氟酸介质中能够形成稳定的溶液,使用耐氢氟酸进样系统的电感耦合等离子体发射光谱(ICP-OES)有利于提高分析的准确性。本文采用模块化的小罐型、多罐体组合(70罐/组)酸溶罐体的微波消解溶样模式,结合ICP-OES仪器的耐氢氟酸进样系统,建立了测定铌钽矿中铌、钽的分析方法。本方法加快了酸溶的溶样速度,溶样时间从原来的48 h减少至1 h,且在氢氟酸介质中测定,避免了高含量铌、钽在低酸度介质中容易水解的影响。方法检出限为铌5.58 μg/g,钽5.87 μg/g。本方法应用于测定铌钽精矿(19%Nb2O5,27%Ta2O5)的分析结果与碱熔方法一致,能够测定Nb2O5含量在42 μg/g~19%和Ta2O5含量在86 μg/g~27%高低品位的铌钽矿,尤其对于铌、钽在百分含量以上的铌钽矿具有优势。 相似文献
12.
中亚造山带中斑岩铜钼矿的Re，Pt，Pd和Au含量 总被引：1，自引：1，他引：1
Anita N．Berzina Alexander F．Korobeinikov 《岩石学报》2007,23(8):1957-1972
Precious metal(Pt,Pd and Au)and Re contents in rocks,ores and flotation concentrates of Siberian(Russia)andMongolian porphyry Cu-Mo and Mo-Cu deposits were studied.The following deposits are discussed:Early Devonian porphyry Mo-CuSora deposit(Kuznetsk Alatau Mountains,Russia)and porphyry Cu-Mo Aksug deposit,(northeastern Tuva,Russia);Triassicporphyry Cu-Mo Erdenetiin Ovoo deposit(northern Mongolia).The samples analyzed include unaltered host rocks of plutons,porphyryrocks of ore-bearing series,different types of altered rocks,mineral separate analyses of molybdenite,chalcopyrite and magnetite,aswell as flotation concentrates.Pt,Pd,Au and Re contents were determined using ICP/MS,AAS and inversion voltammetric analysis.PGE abundances in rocks and poorly mineralized samples span a large range from below detection limit to 65 ppb Pt and 74 ppbPd.Re concentrations in whole rock samples range from below detection limit to 89 ppb.Molybdenite has been shown to be the majorhost phase for Re.The results presented show that Aksug deposit reveals elevated PGE and Au contents in ore minerals and flotationconcentrates.High Pd contents in ores of the Aksug deposit are in accordance with the presence of palladium mineralization in the formof palladium telluride merenskyite(Pd,Pt)Te_2.The variety of precious metals and Re contents in the studied deposits could be caused by a complex interplay of several factors,including importance of primary metal concentrations derived from the source,transport of metals to the deposition area,physicochemical properties of the fluid(fo_2,pH,fs,T,P),and depositional conditions.Higher Re contents in molybdenite andchalcopyrite separates are typical for copper-rich Aksug and Erdenetiin Ovoo deposits.Rhenium concentration in sulfides frommolybdenum-rich Sora deposit is significantly lower.Highly oxidized,Cl-rich fluid style at Aksug and Erdenetiin Ovoo was favorable forhigh rhenium solubility and transport to depositional area.The occurrence of significant precious metals contents at Aksug were likelydue to:1)PGE and Au enriched source,2)favorable fluid style(high fo_2,high Cl-activity),promoting high solubility andtransportation of precious metals in ore-forming fluid as chloride complexes;3)moderately reducing depositional conditions from PGE-bearing solutions containing As and Te,facilitating PGM deposition.As for the porphyry systems at the Sora and Erdenetiin Ovoodeposits,they were probably devoid of precursors favorable for the enrichment in PGE and Au or the role of such precursors wasinsignificant. 相似文献
13.
将碱熔后的样品酸化,在磷酸介质中,以硼氢化钾为还原剂,用原子荧光光谱法测定锗的含量。该法的检出限为0.1μg/g,,测定的六个国家一级土样与推荐值相符,并且各自测定12次的RSD均小于10%。 相似文献
14.
应用S930树脂富集薄样-X射线荧光光谱现场分析环境水体中8种重金属的方法研究 总被引：1，自引：1，他引：0
使用便携式X射线荧光光谱法结合富集技术已能分析液体样品中近20种金属元素,但检出限相对较高(0.1~100μg/L)、富集操作繁多、一种富集法可测元素种类较少等因素制约了该技术的发展。本文研究了一种适应于现场测试环境水样的XRF分析方法。使用20 mg S-930螯合树脂对100 m L水体中8种重金属(V、Mn、Fe、Co、Ni、Cu、Zn和Pb)进行预富集,控制溶液p H=4,搅拌30 min,经真空抽滤系统过滤制得均匀薄样,再使用自制的双层膜包夹样品盒并利用小型台式波长色散XRF测定。结果表明,8种元素标准曲线的相关性R20.997,检测范围为10~1000μg/L,检出限为1.0~6.2μg/L,方法精密度(RSD,n=12)小于5%,加标回收率为80%~120%;标准水样和模拟水样的测定结果分别与标准值和理论值基本一致。本方法巧妙地使用双层聚丙烯膜包夹薄试样的制样方法,较好解决了薄膜样品的污染等问题,简化了水样的预富集操作,制备的树脂薄样可直接供XRF测量。方法检出限较低,稳定性较好,适用于检测Ⅰ~Ⅴ类水体中Fe、Co、Ni和Cu,Ⅱ~Ⅴ类水体中V和Zn,Ⅲ~Ⅴ类水体中Mn和Pb,基本具备对8种重金属污染水体进行环境监测、水质调查等现场分析的能力。 相似文献
15.
采用新型手持式光度计检测天然水中痕量铀 总被引：1，自引：0，他引：1
利用自行研制的高灵敏度手持式光度计对环境水样中的痕量铀进行了分析测定,讨论了波长、pH值、显色剂等主要因素对分析结果的影响,建立了应用手持式光度计进行环境水样中痕量铀测定的新方法。实验结果表明,与普通分光光度计相比,本方法具有仪器简单小巧,功耗低,灵敏度高,精密度好等特点。方法的检出限为0．05μg／L,线性范围为0．05～100μg／L,应用于自来水、湖水、河水、矿泉水和尾矿坝水样中痕量铀的测定,相对标准偏差为RSD=1．04％～2．78％（n=3）,加标回收率为95．7％～100．4％。 相似文献
16.
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
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
17.
顶空进样-固相微萃取测定饮用水源水中吡啶 总被引：2，自引：1，他引：1
用75μm CarboxenTM-Polydimethylsiloxane(CAR-PDMS)固相微萃取头顶空萃取15 mL水样中的吡啶,萃取物用气相色谱-质谱法进行分离和检测,采用内标法和质谱的选择离子监测模式进行定量分析。优化了顶空进样-固相微萃取条件,获得较佳的萃取温度(58.0℃)和萃取时间(40 min)。在优化的条件下,方法检出限为1.5μg/L,标准曲线的线性相关系数为0.9994,线性范围为2.5～50.0μg/L;饮用水源水和纯水加标平均回收率为75.6%～81.3%,相对标准偏差(RSD,n=6)为9.60%～12.21%。使用顶空萃取方式可避免样品基体的复杂性,有利于保护萃取头涂层,同时无需使用有机萃取溶剂;使用质谱检测器可减小假阳性带来的影响。顶空进样-固相微萃取操作简单、环保、灵敏度高,适合用于饮用水源水中吡啶的监测分析。 相似文献
18.
19.
Eric L. Hoffman 《Journal of Geochemical Exploration》1989,32(1-3)
Various methods are described for the analysis of Au and the Pt-group elements (PGE) using different geochemical media commonly collected by the exploration geochemist. The methods described utilize primarily the Instrumental Neutron Activation Analytical technique (INAA) in use at a commercial INAA laboratory.Rocks and soils are routinely analyzed by using a Pb fire-assay preconcentration on a 20-g sample and then analyzing the resultant Ag dore bead by INAA to a detection limit of 1 ppb. Growing rapidly in popularity is the analysis of a 30-g aliquot of sample for 34 elements including Au, solely by INAA. The elements included provide a wealth of information of a geological nature.Due to the very inhomogeneous nature of Au occurring in heavy-mineral concentrates it is imperative to analyze the whole concentrate. The only method which can provide a multielement analysis and still retain the sample intact is INAA.Biogeochemistry using either humus or vegetation as the sample media is rapidly becoming widely used. INAA provides a very sensitive means of determining Au and 34 other elements rapidly and at relatively low cost.These and other methods using the INAA technique for Au and the Pt-group will be described. 相似文献
20.
J. B. McHugh 《Journal of Geochemical Exploration》1984,20(3):303-310
A method has been developed using electrothermal atomization to effectively determine the amount of gold in natural water within the nanogram range. The method has four basic steps: (1) evaporating a 1-L sample; (2) putting it in hydrobromic acid-bromine solution; (3) extracting the sample with methyl-isobutyl-ketone; and (4) determining the amount of gold using an atomic absorption spectrophotometer. The limit of detection is 0.001 μg gold per liter. Results from three studies indicate, respectively, that the method is precise, effective, and free of interference. Specifically, a precision study indicates that the method has a relative standard deviation of 16–18%; a recovery study indicates that the method recovers gold at an average of 93%; and an interference study indicates that the interference effects are eliminated with solvent extraction and background correction techniques. Application of the method to water samples collected from 41 sites throughout the Western United States and Alaska shows a gold concentration range of < 0.001 to 0.036 μg gold per liter, with an average of 0.005 μg/L. 相似文献