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在容量法对页岩的等温吸附实验测试中,发现随压力增加吸附量呈现减小趋势,甚至出现负吸附量,测得的吸附常数Langmuir体积和Langmuir压力出现负值,与实际不相符,造成实验结果和吸附常数失去应用价值。从页岩吸附测试方法、吸附测试仪器等方面系统分析了容量法页岩吸附实验出现"倒吸"现象的原因;提出了实验中自由空间体积测试和吸附气含量计算存在的问题;并对页岩吸附实验方法和页岩吸附测试仪器提出相关建议。 相似文献
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煤等温吸附特性测试中体积校正方法探讨 总被引：1，自引：0，他引：1
首先肯定了在等温吸附测试过程中,计算吸附量时应进行体积校正,然后论述了原体积校正方法,认为采用原公式有一定的试验条件,并提出可以分别利用直接法和间接法求出真实吸附量。直接法是利用质量守恒定律,把吸附相体积作为考虑对象直接放在方程中求出真实吸附增量ΔVs,间接法仍以原校正方法为思路,但先对视吸附增量进行修正得到ΔVa修,再利用原校正公式求出ΔVa修。同时指出校正方法基于两个假设条件:即煤体积随吸附过程保持不变;和吸附相密度为恒定值 相似文献
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《地球化学》2019,(6)
为了解高压条件下页岩对甲烷(CH4)、二氧化碳(CO2)及二元混合气体吸附行为,以四川盆地焦石坝地区下志留统龙马溪组页岩样品为研究对象,通过重量法等温吸附实验,研究了不同温度压力条件下CH4、CO2在页岩中的吸附行为。实验表明,在0.01～50 MPa, 40～100℃条件下,页岩对CH4、CO2过剩吸附量随压力增大而增加,直至达到最大值,然后随压力增大而减小;绝对吸附量随压力增大而增加,在40～43MPa之后,吸附量趋于稳定。在高压条件下,页岩对CO2吸附量大于CH4,约为其5倍。利用CH4、CO2单一气体Langmuir吸附量和Langmuir压力,通过扩展的(Extended) Langmuir模型进行拟合,对不同比例CH4/CO2二元混合气体吸附量进行模拟预测,研究表明,二元气体总吸附量随混合气中CO2比例增大而增加。在高压条件下, Langmuir过剩吸附模型能较好地拟合CH4、CO2在页岩中的吸附,扩展的Langmuir过剩吸附模型也能较好地拟合二元混合气体在页岩中的吸附。 相似文献
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提出了一种采用高温高压密闭溶样快速消解荧光粉晶体的前处理新方法。针对目前常用的稀土氧化物和稀土磷酸盐类、碱土金属铝酸盐类、碱土金属硅酸盐类四大类荧光粉,研究了消解时间、温度、消解溶剂种类和用量4个条件对样品消解程度的影响。采用电感耦合等离子体质谱法(ICP-MS)测定了最佳消解条件下消解的荧光粉中杂质元素Cu、Zn、Cd和Pb的含量。结果表明:稀土氧化物和稀土磷酸盐类荧光粉的最佳消解条件为 2 mL HCl溶剂中120℃下消解3 h;碱土金属铝酸盐类荧光粉的最佳消解条件为2 mL HCl溶剂中160℃下消解6 h;碱土金属硅酸盐类的最佳消解条件为2 mL HCl+0.5 mL HF溶剂中160℃下消解3 h。荧光粉中主要共存元素对所测杂质元素Cu、Zn、Cd和Pb的检测无干扰。该法线性范围宽、检出限低、灵敏度高,是荧光粉晶体中元素检测的较佳方法。 相似文献
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基于新疆和山西气煤及瘦煤对H_2S、CH_4和N_2的平衡水条件下的等温吸附实验及Langmuir模型和D-A模型对实验数据的模拟结果,来研究煤矿瓦斯中H_2S气体的吸附特性及其影响因素,并探讨其与H_2S异常矿井的治理关系。结果显示:不同于CH_4和N_2在煤中主要以微孔吸附为主(90%以上),煤中H_2S气体的微孔吸附量仅占Langmuir最大吸附量的36.26%~57.21%,平均为45.99%;气体分子本身的性质是影响煤中H_2S吸附的主要因素,尤其分子直径是影响H_2S气体V_0/V_L远小于CH_4和N2的这种现象的主要原因,也是造成微孔中H_2S气体难以解吸的主要原因;基于H_2S气体在煤中吸附解吸特征,提出应从H_2S气体分子本身入手,结合矿井煤层地质条件来治理煤矿中的硫化氢。 相似文献
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为了阐明CH4与CO_2在高岭石中的竞争吸附机理,采用蒙特卡洛方法构建了高岭石超胞模型,模拟计算了高岭石吸附CH4与CO_2在不同温度及压力条件下的变化规律,分析了不同孔径对高岭石吸附CO_2和CH4的影响。结果表明,不同温度下高岭石对CH4与CO_2分子的吸附量均符合Langmuir模型,在相同压力条件下,高岭石对CO_2分子的吸附量远远大于对CH4分子的吸附量;293.15 K时,高岭石对CO_2的吸附具有明显的竞争优势,CH4在CO_2分子的影响下不再符合Langmuir曲线,说明高岭石与CO_2分子的相互作用强于与CH4之间的相互作用;随着孔径的增大,高岭石对CH4与CO_2的吸附量均减小,表明CH4和CO_2主要吸附在微孔中;高岭石吸附CH4与CO_2分子后体系的总能量和非成键能发生了变化,说明高岭石与CO_2的相互作用能要强于高岭石与CH4的相互作用能,高岭石对CH4的吸附为典型的物理吸附,而对CO_2的吸附以物理吸附为主,且伴随着微弱的氢键作用。研究结果为阐明CO_2和CH4在黏土矿物的赋存机理以及CO_2驱替CH4的研究提供了一定的理论依据。 相似文献
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本文提出以P_(507)为固定相,盐酸为流动相的萃取色谱法把铈从溶液中分离出来,以偶氮氯瞵-mN与铈的高灵敏显色反应进行比色。本法灵敏度ε=7.8×10~4。实验部分色谱柱:φ8×120m/m 硅烷化硅球100—120目(上试一厂出品) P_(507)(上海有机化学所实验工厂) 偶氮氯膦-mN0.05%水溶液杂质洗除液:5%NH_4Cl,2%磺基水杨酸,1%抗坏血酸,调至pH2—3 铈、镧、镨标准液:用光谱纯的氧化铈、氧化镧、氧 相似文献
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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
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Chemical composition and mode of occurrences of (Au, Ag)Te2 minerals such as calaverite (AuTe2), sylvanite (AuAgTe4) and krennerite ((Au, Ag)Te2) in epithermal gold telluride ores from Suzaki, Kawazu and Teine are examined. In the ores from Suzaki, (Au, Ag)Te2 minerals occur in microbands of tellurides and fine quartz. The minerals in telluride bands change from krennerite, via calaverite‐native tellurium, to sylvanite, in the order of crystallization. A sample from Kawazu contains sylvanite and native tellurium with stutzite, hessite and tetradymite in the coarser gray quartz part. The Teine sample also contains sylvanite and native tellurium with barite and quartz. The peak patterns of XRD of calaverite, krennerite and sylvanite from Suzaki are almost identical to that of JCPDS 43–1472, JCPDS 8–20 and JCPDS 9–477, respectively. The Te, Au, Cu, and Ag contents of calaverite from Suzaki range from 56.4 to 57.9 wt.%, from 41.6 to 42.6 wt.%, from 0.28 to 0.45 wt.% and from 0.14 to 0.31 wt.%, respectively, corresponding to the formula Au0.97Ag0.01Cu0.02Te2. The Te, Au, Ag, and Cu contents of krennerite from Suzaki range from 59.6 to 61.4 wt.%, from 31.3 to 33.6 wt.%, from 4.91 to 6.13 wt.% and from 0.66 to 0.80 wt.%, respectively, corresponding to the formula Au0.71Ag0.22Cu0.05Te2 with Au and Ag ranging from 0.68 to 0.74 and from 0.20 to 0.25, respectively. The Te, Au, Ag, and Cu contents of sylvanite from Suzaki range from 61.5 to 63.4 wt.%, from 24.1 to 27.4 wt.%, from 10.0 to 12.5 wt.% and from 0.00 to 0.12 wt.%, respectively. The Te, Au, Ag, and Cu contents of sylvanite from Kawazu range from 62.7 to 63.3 wt.%, from 23.5 to 24.1 wt.%, from 12.0 to 12.5 wt.% and from 0.09 to 0.16 wt.%, respectively. The Te, Au, Ag, Cu and Fe contents of sylvanite from Teine range from 61.8 to 63.5 wt.%, from 23.6 to 24.7 wt.%, from 11.9 to 13.3 wt.%, from 0.01 to 1.65 wt.% and from 0.00 to 0.02 wt.%, respectively. The average formulae of sylvanite from Suzaki, Kawazu, and Teine are expressed as Au1.06Ag0.94Cu0.02Te4, Au1.00Ag0.95Cu0.02Te4 and Au1.01Ag0.95Cu0.06Te4, respectively. Judging from the mineral assemblages of these ores and other localities, Au–Te mineralization in the Japanese Islands can be divided into four types: native gold–calaverite at Date and Agawa, krennerite(?native tellurium) at Osore‐zan and Mutsu, sylvanite–native tellurium–hessite at Teine, Kawazu, Kobetsuzawa, and Kato, and polyminerallic assemblages at Suzaki and Kushikino. The pH–Eh diagram of aqueous tellurium species and tellurium minerals at 250°C indicates that (Au, Ag)Te2 minerals in epithermal gold telluride mineralization would have been formed under middle to low Eh and acidic (to intermediate) pH conditions. It is possible that dilute tellurium‐containing fluid would scavenge dilute gold. 相似文献
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本文建立一个灵敏的测定钒的催化动力学分光光度法。它基于在热的稀H_2SO_4溶液中,有抗坏血酸存在时,依文思蓝与KBrO_3反应受钒的催化且吸光度降低与钒量相关。方法的检出限为2.23×10~(-13)g/ml(lg(A_0/A)=0.001,b=1cm时),测定范围为0—6ng V/25ml。方法已用于多类样品中痕量钒的分析,相对标准偏差在3.71—5.09％范围。 相似文献
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混合吸附剂分离富集-电感耦合等离子体质谱法测定地质样品中铂钯金 总被引：1，自引：1，他引：0
贵金属分析应用火试金法分离富集时,试金配料复杂、耗时较长,分析成本相对较高,空白较难控制.本文建立了采用过氧化氢-盐酸湿法分解样品,电感耦合等离子体质谱同时测定地质样品中Pt、Pd、Au的分析方法.在10％的盐酸介质中,以LSC-400巯基树脂和活性炭为混合吸附剂,采用动态吸附方式对样品中的Pt、Pd、Au分离富集,用Lu作内标元素,195 Pt、197 Au、108 Pd为待测同位素消除了非谱线干扰和谱线干扰,三元素的回收率均大于96.4％.方法检出限(3σ):Pt为0.06 ng/g,Pd为0.08 ng/g,Au为0.12 ng/g,优于火试金等其他分离富集方法的检出限.应用于测定国家标准物质,Pt、Pd、Au的测定结果与标准值相符,12次测定的相对标准偏差均小于16.1％,满足区域地球化学调查样品的分析要求.该方法操作简便、成本低廉,提高了分析速度,有效地降低了测试过程的空白值. 相似文献
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耦合等离子体质谱技术在地质调查中的应用研究 总被引：6，自引：1，他引：6
本文简要介绍近年来开展的ICP—MS在地质调查中的应用研究工作进展。新方法包括镍锍试金-ICPMS测定铂族元素；封闭酸溶-ICPMS测定地质样品中稀土等47个元素；封闭酸溶乙醇增强ICP—MS测定碲；半熔或稀氨水封闭溶样ICP—MS测定碘溴等非金属元素。 相似文献
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Valentina G. Tsimbalist Gennady N. Anoshin Valentin N. Mitkin Ljudmila I. Razvorotneva Nadezhda P. Golovanova 《Geostandards and Geoanalytical Research》2000,24(2):171-182
Some recent experiments on the determination of Au and the platinum-group elements (PGE) in geochemical samples are reviewed. Emphasis is given to the determination of ultra-low levels of PGE concentrations in resistant matrices, including chromites, molybdenites and ultrabasic ores. The problems and features of PGE determination in samples of various chemical composition are considered. For each sample type studied, a series of sample preparation techniques are proposed. These techniques included acid digestion, fusion with sodium peroxide, cold sintering with an oxidizing mixture of Na2 O2 + Na2 CO3 and also oxidizing fluorination with bromine trifluoride. A new approach for preparing geochemical material prior to digestion, based on mechano-chemical activation with simultaneous hyperfine grinding, is proposed and studied. The instrumental determination of PGE contents was carried out directly by AAS from extracted organic phases. It was found that a combination of digestion processes was required to achieve geochemical background levels of Au and PGE concentrations with the following detection limits: Pd, Rh - 1 ng g−1 , Pt, Ru - 10 ng g−1 , Au - 0.2 ng g−1 , Ag - 0.1 ng g−1. The uncertainty in PGE and Au determination in geochemical samples is dependent on metal concentration, and also on their distribution in samples. The total analytical uncertainty of the proposed method is between 15-30%. 相似文献
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以过氧化钠为熔剂,经高温熔融-热水提取-盐酸酸化前处理样品,选用金为内标元素,电感耦合等离子体发射光谱法测定铬矿石中的二氧化硅。试验了熔融试样时引入的基体元素钠对被测元素的干扰情况,结果表明,钠含量高于300 mg/L时,二氧化硅的回收率均低于92.5%。采用金内标法有效克服了基体效应及仪器波动产生的影响,改善和提高了准确度和精密度。二氧化硅的检出限为0.0075 mg/L,测定范围为0.025%～10.0%。对铬矿石标准物质进行测定,结果与标准值一致,方法精密度(RSD,n=9)小于2%。与常规化学分析法进行比对试验,二氧化硅的测定值吻合较好,但克服了常规化学分析方法步骤繁琐、耗时长、工作量大的不足,提高了工作效率。本方法也可用于同时测定铬矿石中铝、铁、钙、镁、磷等主次量成分。 相似文献
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雪峰山中段铲子坪和大坪等金矿区目前发现的岩金矿脉均赋存于剪切带中，说明剪切作用本身也就是成矿作用。通过剪切作用过程中的应力分析，发现剪切带中金矿脉走向与剪切带走向的交角遵循一定的数学关系，从而提出二者交角的数学表达式，该数学表达式推算出的理论值与实测值可以相互对照。 相似文献
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氢化物发生-电感耦合等离子体发射光谱法同时测定土壤中的痕量砷铜铅锌镍钒 总被引：1，自引：1，他引：0
土壤中砷的测定方法多采用氢化物发生-原子荧光光谱法(HG-AFS);电感耦合等离子体发射光谱法(ICP-OES)在多元素同时测定方面应用普遍,但测定砷的检出限稍高。氢化物发生技术与ICP-OES两者联用也多有研究,较大幅度降低了砷的检出限,已能实现砷锑铋汞等元素的同时测定。但联用技术只能应用于测定能够发生氢化反应的元素,无法实现易氢化元素和难氢化元素的同时测定。本文通过改进ICP-OES仪器的进样装置,采用氢化反应气与ICP-OES雾化气双管路同时进样的方法,实现了一次溶样、一台设备同步测定样品中的砷和多种金属元素。土壤样品经氢氟酸、硝酸、高氯酸、盐酸溶解后,用10%盐酸提取,用硫脲-抗坏血酸溶液将砷元素预还原为+3价后双流路同时进样测定。对于溶液中共存的离子,高于1.0mg/L的La和Dy对砷测定有干扰;低于50.0mg/L的K、Na、Ca、Mg、Fe,低于20.0mg/L的Pb、Mo、Zn、Cu、Ba、Ti、Mn、Ni、Sr、V、Cr,低于10.0mg/L的Co、Ag、U、Cd、Li、Au对砷测定无影响。本方法提高了砷的测定灵敏度,又充分利用多元素同测的优势,实现了同时测定易氢化的痕量砷和难氢化的铜、铅、锌、镍、钒等元素。方法精密度高(RSD5%),经土壤标准物质验证方法可靠,适合痕量砷与其他元素的同步测定。 相似文献