发射光谱法测定化探样品中的Cu、Pb、Zn、Co、Ag、Sn、Mo和B

以Al2O3、K2S2O7、NaF、C作为缓冲剂与样品混匀,装入石墨电极中,以平头石墨电极为上电极,样品电极为下电极进行摄谱,由光电译谱仪测定谱线的黑度值,以锗为内标用内标法测定样品中Cu、Pb、Zn、Co、Ag、Sn、Mo和B的质量分数。     

双电极发射光谱法测定水系沉积物中硼锡银

本方法采用双电极摄谱,以K2S2O7,NaF,Al2O3和GeO2为缓冲剂与样品混匀,Ge为内标,电弧发射光谱法测定样品中的硼锡银。测定国家一级标准物质,结果与标准值相符。     

发射光谱法定量测定岩矿、土壤中的Ag、B、Sn、Mo

样品以焦硫酸钾、氟化钠、三氧化二铝和碳粉为缓冲剂,改善各元素的蒸发行为,采用较短的摄谱时间,大大降低光谱背景,以两根装样电极两次重叠摄谱,分别对长波、短波相板采用不同显影时间,以锗作为内标元素,实现了试样中银、硼、锡、钼的同时定量测定.方法应用于岩石、土壤等地质样品测试中取得了满意的结果。     

深孔电极发射光谱法测定地质样品中Be、B、Pb、Mo、Sn、Cu、Ag、Zn

本法是在样品中加入适量的缓冲剂,使难发挥元素Be形成易挥发的氟化物,与B、Pb、Mo、Sn、Cu、Ag、Zn等元素在同一时间内蒸发,利用深电孔极的分馏效应,有效地降低光谱背景以及被测元素的检出限。加入内标元素,提高了方法的准确度和精密度。采用深孔电极,取样量大,代表性好。一次摄谱,同时检测多个元素,大大提高了工作效率,又减少了测试费用。方法操作简便,适合于大批量样品的测试。检出限ω(B)/10-6分别达到:Be:0.50、B:0.91、Sn:0.50、Ag:0.02等,均满足《覆盖区多目标地球化学调查样品测试及质量监控暂行规定》规定。     

深孔电极载体蒸馏光谱法测定化探样品中八个易挥发元素

以碘化铵、硫酸钠、硫粉、碳粉、氧化钙、二氧化硅混合物为缓冲剂，深孔电极，截取曝光，以谱带背景作内标，一次摄谱同时测定化探样品中As、Sb、Bi、Ag、Pb、Cd、Tl、Sn等微量元素。方法精密度（RSD，n=10）为1．2％-5．0％，检出限为0．013—1．0μg／g。方法经国家一级标准物质验证，测定结果与标准值基本相符。     

碳酸岩样品中银、锡、硼的光谱测定

碳酸岩样品中由于CaO的辐射背景深而影响了许多元素的测定。本法针对碳酸岩样品的组份,在缓冲剂中加入大量的SiO_2(石英粉)稀释样品,从而消除了CaO对测定Ag、Sn、B等的影响。 实验部分 一、CaO对谱线强度的影响 据资料介绍,样品中CaO的含量或CaO/SiO-2的比值和谱线强度的减弱有线性关系。在本体系中,CaO的影响如图所示。当样品与缓冲剂的混合物中CaO含量低于10％时,Ag、Sn和B的谱线强度无明显减弱,而当混合物中CaO含量超过10％时,Ag、Sn的谱线强度急剧减弱,且光谱背景逐     

发射光谱法定量测定岩矿、土壤中的Ag,B,Sn

对土壤中的银、硼、锡测定通常用光谱法,以焦硫酸钾、氟化钠、三氧化二铝和碳粉为缓冲剂,改善各元素的蒸发行为,采用较短的摄谱时间,大大降低光谱背景,以锗作为内标元素,实现了试样中银、硼、锡的同时定量测定,方法应用于岩石、土壤等地质样品测试中并取得了满意的结果。     

简便快速富集测定微量金的方法研究

本法采用特制碳电极对含金试液加以富集后,在常规光谱分析条件下进行摄谱分析。经对电极性状及转速、富集液用量、电流强度和摄谱时间等主要影响因素进行试验选择,初步确定出富集测定金的最佳折衷工作条件。在尚未采用内标的情况下,标准曲线仍有较好的线性关系。尤本法检测限较低(C_L<0.1g/T),整个富集测定操作简便快速。这为常规电弧光谱分析迅速有效地富集测定样品中的微量金探索出一可取新途径。     

化学光谱法测定微量金的摄谱电极之改进

化学光谱法测定微量金已实用多年。一般使用杯形下电极、锥形上电极，本实验在前人基础上将上电极改为凹形电极，与锥形上电极摄谱相比较的优点是：（）使用凹形上电极避免了炽热的锥形电极头像进入光栏孔。样品含量低于μ时摄谱11g曝光时间控制为。上下电极有效对齐，避免了摄谱激发因瞬时电势差极大而引起的溅弧现8 s象，所以光谱背景浅。×110－3μ的金在线处也能看到清晰谱线。g2 675.95 （）凹形对电极摄谱，增大工作电流，延长曝光时间，从而提高弧焰的温度，使蒸发出2来的金得以充分激发。另外，上下电极都存在一个气室，对金的…     

高灵敏度化学光谱法测定钯的研究

拟定三正辛胺负载泡塑富集地质样品中痕量钯的化学光谱测定方法。一次摄谱的测定范围为 0 .1× 10 - 9～ 2 0 0× 10 - 9     

电感耦合等离子体发射光谱法测定煤及煤灰样品中21个主次微量元素

对化学物相法分析矿石中红柱石的含量作了初步探讨。试样经氢氟酸冷浸12 h,过滤后残渣用过氧化钠熔融,热水提取,用乙酸锌标准溶液滴定三氧化二铝含量,最后以三氧化二铝的含量换算成红柱石的含量。结合青海乐都矿区红柱石与其伴生矿物的组成特点,试验了排除其他含铝矿物的工作条件与红柱石的溶解特性,并用人工模拟样品中的红柱石溶解率求得校正系数,确定了铝量法作为矿区红柱石化学物相分析方法。     

电感耦合等离子体质谱法测定岩石样品中的锆铌铪钽两种预处理方法的比较

研究了微波消解酸溶和过氧化钠碱熔两种测定岩石样品中锆、铌、铪、钽前处理方法,利用电感耦合等离子体质谱法进行测定。对所选用不同种类的岩石国家标准物质样品进行了条件实验,结果表明:采用过氧化钠碱熔法处理岩石样品后,锆、铌、铪、钽的测量值准确度高,且相对标准偏差(RSD,n=10)小于6%,该方法更适用于岩石样品中锆、铌、铪、钽的测定。     

X射线荧光光谱法同时测定石灰石中主次痕量组分

采用熔融玻璃片和粉末压片法制样,选用标准样品,以经验α系数和散射线内标法校正元素谱线重叠干扰和基体效应,用ZSX PrimusⅡX射线荧光光谱仪对石灰石样品中CaO、Na2O、MgO、Al2O3、SiO2、K2O、TFe2O3、P2O5、TiO2、MnO和S等主次痕量组分进行测定,分析结果与标准值和化学值相符,12次测定的相对标准偏差小于10%。     

发射光谱法同时测定地球化学样品中微量银铍硼锡铋钼

采用垂直电极装样,二米平面光栅交流电弧摄谱测定地质样品中的微量元素银、铍、硼、锡、铋、钼,以三氧化二铝、焦硫酸钾、氟化钠、碳粉和硫粉作缓冲剂,锑、锗作内标。方法检出限为:银0.019μg/g、铍0.11μg/g、硼0.85μg/g、锡0.26μg/g、铋0.031μg/g、钼0.12μg/g。各元素12次测定的相对标准偏差(RSD)均小于10%。用水系沉积物、土壤、岩石国家一级标准物质进行验证,测定值与标准值基本一致,符合多目标地球化学填图的质量要求。     

化探样品中金、铋、钼化学光谱法联测

介绍了一种应用化学光谱法对化探样品中痕量金、铋、钼进行联测的方法。该方法是先将试样焙烧后，用王水溶解样品，在盐酸介质中用活性炭静态吸附痕量金、铋、钼，并与其它元素发生分离，再将吸附了待测元素的活性炭灰化后装入电极板，进行光谱测定。生产实践表明，该方法快速、准确，能够进行三元素联测，进一步改进测试工艺，还可进行多元素联测。     

电感耦合等离子体发射光谱法同时测定玻璃中铝钙铁钾镁钠钛硫

通过选择分析谱线、处理样品方法和消除干扰因素等实验,建立了电感耦合等离子体发射光谱法同时测定玻璃中的Al2O3、CaO、Fe2O3、K2O、MgO、Na2O、TiO2和SO3的方法,克服了利用常规化学法测定玻璃中各氧化物步骤繁琐、耗时长、工作量大的不足。方法的回收率为95.0%~103.0%,精密度(RSD,n=10)为0.20%~1.72%。方法具有快速、简便、线性范围宽等优点,分析误差满足常规化学分析法的要求。用于钠钙硅玻璃及其制品的分析,结果令人满意。     

The microdetermination of H2O,CO2, and SO2 in glass using a 1280°C microscope vacuum heating stage,cryopumping, and vapor pressure measurements from 77 to 273 K

A new microscope vacuum heating stage and gas analyzer has been developed for measurement of H₂O, CO₂, SO₂, and noncondensable gas (H₂, CO, N₂, Ar, CH₄, etc.) evolved from samples, particularly natural glass, at temperatures up to 1280°C. The gas evolved upon heating to 1280δC is collected in a liquid nitrogen cold trap. Gas components are identified by the characteristic vapor pressure and temperature ranges over which solid and vapor are in equilibrium during sublimation of individual components. The masses of CO₂, SO₂, and H₂O derived from samples and blanks are calculated using the ideal gas law, the molecular weights of the components, and the gauge constant (i.e. the ratio of the number of moles of a gas to its partial pressure in the constant volume). Results obtained by repeated determinations of H₂O, CO₂, and SO₂ evolved from a submarine basaltic glass from Kilauea volcano, Hawaii, (average sample mass = 3 × 10^?3 g) gave probable errors for the determinations of H₂O (0.23%), CO₂ (0.025%), and S (0.071%) equal to 4, 10, and 8% respectively, of the concentrations. Determinations of H₂O in smaller samples of H₂O-poor basaltic pumice show a linear proportionality (0.063%) between the measured H₂O and the sample mass over the range 0.1 × 10^?6 to 1.7 × 10^?6 g H₂O. Comparisons of H₂O determinations by this technique with those obtained by Penfield, gas chromatic, microcoulometric, and vacuum fusion techniques used elsewhere show reasonably good agreement. Determinations of SO₂ by this technique agree reasonably well X-ray fluorescence and electron microprobe determinations of sulfur. Determinations of CO₂ by the present technique are reproducible but cannot be compared directly to measurements made in other labs because of differences in samples analyzed. The principle advantages of this analytical technique are the very small sample required, the simultaneous determination of H₂O, CO₂, SO₂ and noncondensable gas, the avoidance of calibration procedures dependent on chemical standards, and the visual observations that can be made during sample outgassing.     

X射线荧光光谱法测定土壤和水系沉积物中碳和氮等36个主次痕量元素

采用低压聚乙烯镶边垫底的粉末样品压片制样，用ARL ADVANT’XP＋型X射线荧光光谱仪对土壤和水系沉积物样品中C、N、Na2O、MgO、Al2O3、SiO2、P、S、Cl、K2O、CaO、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、Nb、Zr、Y、Sr、Rb、Pb、Th、Ba、As、Br、Hf、La、Ce和Nd等36个组分进行测定。重点研究了C、N等元素的测定务件和痕量元素的背景选择和谱线重叠校正问题。使用经验系数法和康普敦散射作内标校正基体效应。经标准物质校验，结果与标准值吻合。方法的检出限、精密度和准确度能满足多目标地球化学调查样品的分析要求。用GBW 07404土壤国家标准物质进行测试，12次重复测定的精密度（RSD），除N和Cl〈11．0％，其余各组分均〈6．0％。     

Volatiles in amphiboles from xenoliths,Vulcan's Throne,Grand Canyon,Arizona, USA

Analyses of major element and volatile components of amphiboles from Vulcan's Throne, a Recent volcano on the north rim of the Grand Canyon, Arizona, USA, have been performed by using the electron microprobe and high temperature mass spectrometry. The amphiboles occur as megacrysts, as oikocrysts in peridotite and pyroxenite xenoliths, in amphibole-rich selvages on lherzolite xenoliths, and as grains in hornblendite xenoliths. Total volatiles range from 1.27 to 1.75 wt.%. In all samples, H₂O is the principal volatile species. Lesser amounts of structurally bound fluorine, chlorine, and oxygen were also released. The amphiboles studied are hydroxyl-deficient. The O(3) site is probably partially occupied by O^2?, which was detected as O₂ during degassing of the amphibole. Ti shows a strong positive correlation with the amount of hydroxyl deficiency in the amphiboles except for one oxidized sample. Thus, Ti probably is significant in charge balancing the substitution of O^2? for OH^? and the substitution probably occurred during crystallization rather than by dehydrogenation. Small amounts of both oxidized and reduced carbon and sulfur-bearing volatile species (e.g., CO₂, CO, CH₄, SO₂, H₂S) were detected in all samples. The observation of reduced carbon species supports the hypothesis that the oxygen fugacity of at least portions of the upper mantle is probably less than the quartz-fayalite-magnetite buffer.