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1.
本文报道了采用黄原酯棉(CCX)在煮沸过的王水介质中富集分离金的研究。确定了CCX吸附金的最佳条件和解脱金的方法,并拟定了应用火焰和无火焰原子吸收测定金的方法。本法简单快速、选择性好、准确度高。方法的灵敏度为:火焰法:2μg、无火焰法:5ng。经样品验证,结果满意。  相似文献   

2.
葛艳梅 《岩矿测试》2014,33(4):491-496
原子吸收光谱法(AAS)应用于高品位金矿石中金的测定,有效地解决了火试金重量法和氰醌容量法等分析方法有毒化学试剂用量大、测试条件局限性大等诸多问题。泡沫富集-火焰原子吸收光谱法(泡沫富集-FAAS法)就能够测定金品位达到500μg/g的金矿石,但该方法在常规FAAS方法基础上增加了滤渣分离、滤液稀释及泡沫灰化、复溶等过程,由于操作环节的增多,分析效率不高,且引入测量误差的机率随之加大。本文建立了一种高品位金的快速分析方法,样品用王水溶解,分离残渣,滤液定容后无需分离富集直接采用FAAS测定金量,方法精密度(RSD)为1.6%,优于FAAS本身精密度,满足了高品位金矿石样品快速分析监控的要求。通过实验对黑龙江省某岩金矿矿样(生产监控样)、金矿石外检样品及金矿石国家标准样品采用本法、泡沫富集-FAAS法、氰醌容量法、火试金重量法进行综合分析,结果表明样品基体中铁含量的高低直接影响到本法测定高品位金量的准确性。当金量为50~110μg/g时,允许样品中铁含量为10%;金量为110~164μg/g时,允许样品中铁含量为20%;金量为164~218μg/g时,允许样品中铁含量为25%。研究认为,本法普遍适用于测定金品位达到50μg/g以上、铁含量小于10%的金矿石。铁在地壳中的平均含量为5.63%,大部分金矿石国家标准样品的铁含量均在此平均值附近,一般金矿石的铁含量也很少达到较高水平,因此本法具备较强的应用性;且与泡沫富集-FAAS法相比,省去了泡沫富集-灰化-复溶的操作过程,大大提高了金量的分析效率。  相似文献   

3.
孙文军 《岩矿测试》2012,31(5):829-833
传统的发射光谱、化学光谱、泡塑富集分离-原子吸收光谱法测定化探样品中的金和银,分析结果不稳定,效率低。本研究提出用50%的王水分解化探样品,负载二苯硫脲泡塑吸附金银,石墨炉和火焰原子吸收光谱法对金和银进行联合测定。在二苯硫脲浓度、吸附酸度、吸附温度、振荡时间等优化的实验条件下,金和银的回收率分别达到97.9%和98.8%,检出限为0.25 ng/g和0.038μg/g,准确度(RE,n=9)为2.0%~14.0%和7.7%~13.3%,精密度(RSD,n=9)为3.1%~12.4%和5.1%~13.2%。经国家标准物质分析验证,测定值与标准值基本相符。该方法实现了在同一份溶液中同时测定金和银,与现行的石墨炉原子吸收光谱测定金、发射光谱测定银的方法相比,称样量达到10 g,样品的代表性显著增加,提高了准确度和精密度,简化了金银分析的程序,化学试剂用量少,分析成本低。  相似文献   

4.
采用微色谱柱技术对环境样品中的铀进行分离富集,分析了影响其分离富集的条件,并以ICP-AES为检测仪器,对环境样品中铀的含量进行了准确测定,建立了D293固相萃取分离/ICP-AES在线测定环境样品中铀的方法。实验表明,pH=1.5时,铀可被树脂完全吸附,10mL0.9mol/LNH4NO3-0.1mol/LHNO3可完全解吸铀,浓缩物用ICP-AES进行测定,检出限、相对标准偏差和相对误差分别为0.05μg/mL,0.8%~2.9%和0.4%~9.8%。方法简便、快速、准确,适合于各种环境样品中微量铀的测定。  相似文献   

5.
试样经650℃灼烧,王水(1+1)冷浸泡分解试样,利用泡沫塑料富集金,采用硫脲溶液解脱金,用火焰原子吸收光谱法测定矿样中的金,本法适用岩石矿物中0.05×10-9以上金的测定。  相似文献   

6.
样品经室温烧至650℃后保持2个小时,用王水溶解,用聚氨酯泡沫塑料吸附富集样品中的金,经过硫脲-盐酸溶液水浴解脱,使金释放出来,解脱液于火焰原子吸收光谱仪上用标准曲线法测定。该方法灵敏度高、检出限低,加标样回收率在98%~101%。  相似文献   

7.
石墨炉原子吸收光谱法测定地质样品中的痕量铂、钯   总被引:1,自引:0,他引:1  
本文提出了用717阴离子交换树脂富集铂、钯的石墨炉原子吸收光谱分析方法。对富集铂、钯的条件,共存离子的干扰情况以及在GF-2000型石墨炉中测定铂、钯的最佳条件进行了研究。样品用王水分解后,在10%的王水介质中,用717阴离子交换树脂富集铂、钯,以热的硫脲溶液解脱,在拟定的工作条件下,于石墨炉原子吸收光谱仪上进行测定,大量的共存离子不干扰测定。方法简便快速,检出限分别为Pt8.8×10~(-9)g/ml,Pd3.4×10~(-9)g/ml,方法的相对标准偏差分别为Pt7.09%Pd11.48%,适用于地质样品中铂、钯的测定,结果令人满意。  相似文献   

8.
近年来由于金的普查找矿和成矿规律研究的需要,对金的分析测定提出更高的要求,需要测定地质样品中0.001克/吨,甚至更低含量的金。火焰原子吸收法难以满足这一要求,无火焰原子吸收法测定矿物中微量金已有不少报导。各方法的差异仅是分离富集手段不同。目前广泛采用的分离富集手段有溶剂萃取、离子交换、共沉淀、活性炭吸附和反相萃取色层法等。这些方法均能获得满意的分离富集效果。  相似文献   

9.
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   

10.
提出用VS-Ⅱ型强碱性阴离子交换纤维定量富集、硫脲解脱,流动注射在线分离富集—火焰原子吸收光谱法测定地质样品中痕量金银的分析方法。该方法检出限低,金为1.4μg/mL,银为0.35μg/mL,相对标准偏差均小于2%,采样频率为120次/h,用于地质样品中痕量金银的直接测定,结果令人满意。  相似文献   

11.
研究了甲基膦酸二甲庚酯(P350)减压微色谱柱对Au的萃取性能。减压条件下,2mol/LHCI或浓度<25%的王水介质中的Au被萃取在P350(Φ3mm)微色谱柱上,再用小体积的1%Na_2SO_3定量洗脱。与常规柱相比,减压微色谱柱分离具有柱效高、洗脱体积小、速度快、节省大量试剂等优点。经标准样品验证,方法可用于含Au 0.025~200g/t地质样品的分析。  相似文献   

12.
萧莲萍  王作华  陈义 《吉林地质》2011,30(3):96-97,101
本文采用泡塑富集化探样品中痕量金,用石墨炉原子吸收法测定痕量金。试样经灼烧,王水密封溶矿,泡塑富集,硫脲解脱等过程进行了改进及条件控制,该方法具有检出限低,灵敏度高,操作简便,速度快,劳动强度小,适用地质化探样品中痕量金的测定。  相似文献   

13.
地电化学(泡塑)样品中金与锑的预处理   总被引:3,自引:1,他引:3  
通过模拟实验获得附载金、锑的泡塑样品,并对其进行了硫脲解脱法、灰化法、硝酸加氧化剂消解法的比较实验,确定采用硫脲解脱法是地电化学(泡塑)样品金、锑的最佳解脱方法,通过正交实验及其结果分析确定了最佳实验条件。利用硫脲解脱一原子吸收光谱法对某隐伏金锑矿床82件地电化学(泡塑)样品进行了测试,分析结果显示出有明显的金、锑异常,指示了重要的勘探靶区。  相似文献   

14.
刘加召  王琳  吕有成 《山东地质》2013,(10):107-108,112
利用泡沫塑料对地质样品中微量金进行富集,已经是非常成熟的富集方法。常量金经过泡沫塑料吸附后,用硫脲脱附原子吸收测定也是近几年许多实验室常用的方法。而用等离子体光谱仪测定常量金鲜有报道,该方法简单、快捷,通过对国家一级标样的分析试验,对于金含量为0.05-50.00g/t的样品能够满足要求。  相似文献   

15.
在前人研究泡塑吸附金分离的基础上,用聚氨酯泡沫塑料吸附,利用石墨炉原子吸收法测定了痕量价态金的含量,探讨了溶矿介质、解脱时间、吸附温度、Fe~(3+)加入量等对测定结果的影响,确定了最佳测定条件,详细讨论了Fe~(3+)在溶矿和吸附过程中的作用,并将该方法用于土壤中痕量价态金的测定。方法检出限为0. 01 ng/g,测定范围为0. 03~300 ng/g,价态金回收率分别是Au~(3+)97. 3%、Au~+95. 8%、Au098. 9%,价态金分离精密度(RSD,n=12)为7. 3%~18. 8%。用石墨炉原子吸收光谱法测定价态金,不但有效地抑制了共存元素的干扰,而且能降低检出限,提高灵敏度和准确度,自动化进样减少了劳动强度,提高了分析测试效率,适合大批量样品的测试。  相似文献   

16.
Two types of gold deposit with both good homogeneity and a high-grade of gold were selected to prepare four gold ore reference materials (GAu-19,GAu-20,GAu-21 and GAu-22) by the Institute of Geophysical and Geochemical Exploration (IGGE),China.Seven laboratories participated in the certification programme. Volumetric methods for GAu19-21 and atomic absorption spectrometry for GAu-22 were used for the homogeneity testing,the coefficient of variation being found to be less than 3%.After sample digestion and preconcentration,the samples were analysed by flame atomic absorption spectrometry (AAS),colorimetry,neutron activation analysis (NAA)and volumetric analysis. The certified values for the gold concentration in GAu19-22 are 18.3 μg g -1, 32.3 μg g -1, 53.0 μg g -1 and 5.72 μg g -1,respectively.  相似文献   

17.
The Pacific Border Ranges of the southern Alaskan Cordillera are composed of a number of allochthonous tectonostratigraphic terranes. Within these terranes are widespread volcanogenic, massive sulfide deposits in and adjacent to portions of accreted ophiolite complexes, bands and disseminations of chromite in accreted island-arc ultramafic rocks, and epigenetic, gold-bearing quartz veins in metamorphosed turbidite sequences. A geochemical pilot study was undertaken to determine the most efficient exploration strategy for locating these types of mineral deposits within the Pacific Border Ranges and other typical convergent continental margin environments.High-density sediment sampling was carried out in first- and second-order stream channels surrounding typical gold, chromite and massive sulfide occurrences. At each site, a stream-sediment and a panned-concentrate sample were collected. In the laboratory, the stream sediments were sieved into coarse-sand, fine- to medium-sand, and silt- to clay-size fractions prior to analysis. One split of the panned concentrates was retained for analysis; a second split was further concentrated by gravity separation in heavy liquids and then divided into magnetic, weakly magnetic and nonmagnetic fractions for analysis. A number of different techniques including atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and semi-quantitative emission spectrography were used to analyze the various sample media.Comparison of the various types of sample media shows that in this tectonic environment it is most efficient to include a silt- to clay-size sediment fraction and a panned-concentrate sample. Even with the relatively low detection limits for many elements by plasma spectrometry and atomic absorption spectrometry, anomalies reflecting the presence of gold veins could not be identified in any of the stream-sediment fractions. Unseparated panned-concentrate samples should be analyzed by emission spectroscopy and atomic absorption spectrometry for Ag and Au. If, however, magnetic and nonmagnetic concentrate fractions are used in a reconnaissance program, semiquantitative emission spectrography is adequate for all analytical work.  相似文献   

18.
化探样中的痕量银和镉(0.0xppm)不经分离直接用无火焰原子吸收法测定银和镉是困难的。宫本益夫曾用dowex 1×8阴离子树脂分离和富集电解铜中的银;辽宁地质局中心实验室曾用717阴离子树脂分离和富集化探样中的镉,F.Bea.Barredo和c.Polo polo曾用dowex1×8阴离子树  相似文献   

19.
The Okinawa Trough is located between the shelf-sea area of the East China Sea and the deep-sea area of western Pacific Ocean. More than 60 chemical elements in the sediments from the shelf area of the East China Sea, the Okinawa Trough and western Pacific Ocean were determined by advanced techniques including neutron activation analysis, X-ray fluorescence spectrometry, atomic fluorescence spectrometry and atomic absorption spectrometry. Quantitative comparisons of the element abundances of the sediments were made in terms of the enrichment coefficients (K) of the elements.K > 1.5 indicates enrichment (K = 1.5–2, weak enrichment; K = 2–4, strong enrichment) andK > 4, anomalous enrichment. The results show that the Okinawa Trough sediments are characterized by Hg anomaly and the enrichment of such elements as Au, Ag, Se, Te, Sb, Cd, Mn, Mo, etc. Detailed studies show that the excess Hg comes from hydrothermal solutions rather than from the continent, sea water, marine organisms, cosmic dust or volcanic rocks. Attributed to modern hydrothermal activities on the sea floor, Hg anomaly can be used as a geochemical indicator of modern seafloor hydrothermal activity. This project was granted by the National Natural Science Foundation of China.  相似文献   

20.
After acid digestion, gold is extracted with MIBK and determinated by flameless atomic absorption spectrometry. The results for six USGS reference samples and fourteen French geochemical standards are presented and discussed. The agreement with working values for these standards is in the range of pm 5%.  相似文献   

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