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21.
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
22.
Digestion with aqua regia in Carius tube is commonly employed for determination of PGEs in geological samples. However, silicates cannot be completely dissolved by aqua regia and PGEs might partially remain in silicate residue. In this study, an ultramafic reference material was used to investigate the efficiencies of a new re-usable Carius tube after digestion at 220 and 240℃, and an autoclave-lined Carius tube at 260 and 280℃. The results show that about 10% of PGEs retained in the silicate residues at 220 and 5% still r℃ emains even digestion temperature increases to 280℃. These results agree with previous works that increasing the digestion pressure and temperature can achieve more effective dissolution. Thus, a modified digestion procedure for determination of PGEs in ultramafic rocks by the re-usable Carius tube was proposed in this study. 相似文献
23.
Zongqi Zou Zaicong Wang Huai Cheng Tao He Yinuo Liu Kang Chen Zhaochu Hu Yongsheng Liu 《Geostandards and Geoanalytical Research》2020,44(3):501-521
Desilicification elevates extraction of Re and platinum‐group elements (PGEs) from many geological reference materials (RMs), but the extent to which it affects less chalcophile elements has been investigated rarely. To further evaluate the effect of desilicification, mass fractions of elements with variable chalcophile affinities (In, Cd, Cu, Ag, S, Se, Te, Re and PGEs) in different RMs were obtained by isotope dilution and digestion procedures involving HF‐HNO3 in bombs versus HNO3‐HCl in Carius tubes. The results show that the extraction efficiencies of HF‐desilicification vary in different RMs and for different elements. HF‐desilicification led to a significant increase (30–70%) for In and Cd mass fractions in all analysed RMs, but it played a negligible role in other strongly chalcophile elements in many samples (e.g., UB‐N and WGB‐1). Noticeably, desilicification led to a 10–30% increase in the mass fractions of Cu, Ag, S, Se and Te in BHVO‐2 and BIR‐1a, but less so in BCR‐2. These results could be attributed mainly to the variable chalcophile affinities of elements and their relative budget in sulfides, alloys and silicates. Desilicification should thus be preferred to determine chalcophile elements for most samples, except in cases where they are negligibly hosted in silicates. 相似文献
24.
电感耦合等离子体光谱法测定黄铁矿和黄铜矿中的铁铜硫 总被引：2，自引：1，他引：1
样品用王水水浴和HCl-HNO3-HF-HClO4敞开酸溶两种溶矿方式分解,电感耦合等离子体发射光谱法(ICP-AES)测定黄铜矿和黄铁矿中铁、铜、硫。应用称重法配制标准溶液,明显地降低了在标准溶液在逐级稀释过程中由于体积读数等原因产生的误差。样品用王水水浴分解,消解时间短,试剂加入量少,分析步骤简单;由于硫化矿石中Fe的一部分可能与Si结合,王水无法将其全部溶解,对于Fe的测定采用混合酸敞开酸溶。王水水浴溶矿方式选择浓王水作为溶剂,在混合酸敞开溶矿方式的溶解盐类阶段选择浓HCl作为溶剂。确定了ICP-AES法测定高含量(x%～xx%)的铁、铜、硫适用的光谱谱线,稀释倍数为1000。两种样品处理方法操作简便,准确度好,精密度高。经国家一级标准物质GBW 07267(黄铁矿)、GBW 07268(黄铜矿)验证,经混合酸敞开酸溶处理后硫的测定结果偏低,准确度分别为-9.48%和-18%,铁和铜的精密度(RSD,n=5)均小于2%。GBW 07268(黄铁矿)、GBW 07267(黄铜矿)用王水水浴法处理,连续测定10次的短期稳定性,精密度(RSD)小于2%。 相似文献
25.
应用石墨炉原子吸收光谱法测定地球化学样品中的痕量银,一般采用盐酸-硝酸-氢氟酸-高氯酸电加热溶样,铱、铂为基体改进剂,以硫脲作为介质可能会导致大量铜与硫脲发生沉淀,干扰测量结果,分析流程繁琐、成本高。本文采用50%的王水水浴溶样,以湿加方式加入50 g/L硫脲基体改进剂,避免了铜在溶液中与硫脲络合,消除了干扰。方法检出限为0.01 μg/g,准确度和精密度好,内外检合格率符合地质矿产行业标准。该方法简化了样品处理步骤,提高了工作效率,分析成本降低,适合批量样品的分析,且溶解样品的溶液还可继续用于氢化物发生法测定砷、汞、铋、锑等元素。 相似文献
26.
We used samples from six Finnish ore deposits to evaluate the efficiency of sample pretreatment procedures — crushing, splitting and grinding — and to compare three analytical methods based on the atomic absorption determination of gold following: (1) classical lead fire assay (FA); (2) the aqua regia leach (AR) followed by Hg coprecipitation of Au; and (3) the sodium cyanide (NaCN) leach. Sample size used for the method comparison is 20 g. The Au deposits and ore types were: Suurikuusikko and Osikonmäki, refractory ores in which Au is associated with arsenopyrite and pyrite; Pampalo and Kutemajärvi ores with metallic Au and Au tellurides; and Jokisivu and Pahtavaara ores containing coarse-grained metallic Au. After crushing, the samples were split into three parts, one of which was put aside into storage. Two splits were further divided into two subsamples which were ground to two grades of fineness (<0.03 and <0.06 mm). The four subsamples thus obtained were analysed for Au using the three analytical methods. Each determination was performed five times on each of the four subsamples. According to t-tests on the FA results of the two splits, crushing and splitting produced samples of equal Au content in all six cases. Grinding to a finer grain size gave a significant difference in Au results only for the Pahtavaara ore sample. If the FA results are assumed to represent 100% recovery of Au, we obtained greater than 95% recoveries for all but the Suurikuusikko sample (87% recovery) by the AR leach method. We also obtained recoveries of over 95% by the NaCN leach method for the Pampalo, Kutemajärvi and Pahtavaara samples, whereas recoveries for the other three samples varied between 73 to 92%. The AR leach was also performed on 1-g samples and the NaCN leach on 250-g samples. For three of the ore samples, decreasing sample size from 20 g to 1 g did not cause a significant difference in the variance of the Au results. Increasing the sample size from 20 g to 250 g significantly improves the representativity of only the Pahtavaara sample. For the Kutemajärvi, Pahtavaara and Jokisivu ores, a sample larger than 250 g is needed in order to obtain a precision equivalent to that for reference samples. 相似文献
27.
Soil O and C horizon samples (N = 752) were collected at a sample density of 1 site/36 km2 in Nord-Trøndelag and parts of Sør-Trøndelag (c. 25,000 km2), and analysed for Pb and three of the four naturally occurring Pb isotopes (206Pb, 207Pb and 208Pb) in a HNO3/HCl extraction. Soil O and C horizons are decoupled in terms of both Pb concentrations and Pb isotope ratios. In the soil C horizon the Grong-Olden Culmination, a continuous exposure of the Precambrian crystalline basement across the general grain of the Caledonian orogen, is marked by a distinct 206Pb/207Pb isotope ratio anomaly. No clear regional or even local patterns are detected when mapping the Pb isotope ratios in the soil O horizon samples. Variation in the isotope ratios declines significantly from the soil C to the O horizon. On average, Pb concentrations in the O horizon are four times higher and the 206Pb/207Pb isotope ratio is shifted towards a median of 1.15 in comparison to 1.27 in the C horizon. It is demonstrated that natural processes like weathering in combination with plant uptake need to be taken into account in order to distinguish anthropogenic input from natural influences on Pb concentration and the 206Pb/207Pb isotope ratio in the soil O horizon. 相似文献
28.
王水溶样-等离子体质谱法同时测定地质样品中砷锑铋银镉铟 总被引：16，自引：13，他引：3
采用王水溶样-等离子体质谱法测定地质样品中砷、锑、铋、银、镉、铟6个元素,探讨了测定过程中对砷、银、镉、铟干扰的消除问题。方法检出限(10SD,μg/g)分别为:砷0.2、锑0.01、铋0.005、银0.01、镉0.01、铟0.005;精密度(RSD,n=12)分别为砷1.3%~3.0%、锑0.65%~2.3%、铋1.2%~2.6%、银3.2%~6.6%、镉3.7%~8.0%、铟1.1%~5.0%;加标回收率分别为砷96.8%~106%、锑102%~108%、铋102%~106%、银99.7%~104%、镉103%~108%、铟97.9%~100%。用拟定方法测定了国家一级标准物质中砷、锑、铋、银、镉、铟,结果与标准值相符。方法适用于岩石、土壤、水系沉积物等地质样品的测定。 相似文献
29.
索氏提取-原子荧光光谱法测定含油岩心中的汞和砷 总被引：1，自引：1，他引：0
原油对测定含油岩心中的汞和砷有很大影响,目前去除原油等有机物的方法主要有高温烧制、强酸高温氧化等,要求反应温度较高,会造成汞和砷的损失而使测定结果偏低。本文采用索氏提取法,以氯仿作为提取剂在75℃下低温提取分离岩心中的原油,再用50%的王水溶解剩余样品,原子荧光光谱法测定汞和砷的含量。该方法对汞和砷的检出限分别为0. 003mg/kg和0. 10mg/kg,相对标准偏差分别为7. 3%和5. 1%,加标回收率均大于92. 5%。与传统方法相比较,该方法避免了由于原油的疏水性造成样品与王水接触不充分、样品分解不完全和反应温度过高导致汞元素损失的问题,测定汞的相对标准偏差由33. 0%降低至7. 3%,测定砷的相对标准偏差由25. 0%提高至5. 1%,为含油岩心中其他元素的检测提供了借鉴。 相似文献
30.
反王水消解法测定土壤中重金属的方法研究 总被引：3，自引：0，他引：3
反王水消解法测定土壤中重金属元素含量,使用化学试剂少,操作简便,省去了国标方法中的剧毒、剧腐蚀试剂,受到土壤科学工作者的关注;但有必要对该方法的准确度和精密度进行评价。本文采用反王水压力消解罐消解,原子吸收分光光度计测定了土壤标准物质和待测样品中Cu、Pb、Cr、Cd等元素的含量,并进行了加标回收试验。测定结果显示,标准物质测定值与标准值之间无显著性差异,相对标准误差为-4.8%~5.3%;多次测定的变异系数为0.31%~2.83%;回收率为88.5%~96.7%。表明该方法的准确度和精密度均符合要求。因此,该方法在土壤重金属全量分析中有很好的适用性。 相似文献