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1.
杨剑  万飞  王佳丽  杨婷 《吉林地质》2009,28(2):116-119
采用硼酸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Na、Mg、Al、Si、P、S、Cl等31个组分进行测定。重点研究了Cl和S等元素的测定条件、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。  相似文献   

2.
采用粉末样品压片制样,水系沉积物及土壤国家一级标准物质作为标准,使用经验系数法和散射线内标法校正元素间的吸收增强效应,用X射线光谱仪对土壤样品中的Fe_2O_3、Cao、Cl、S、As、Ba、Br、Ce、Co、Cr、Ni、Cu、Zn等34种主次痕量元素进行测定,用国家一级标准物质GBW07452(GSS-23),GBW07405(GSS-5)和GBW07404(GSS-4)分析检验准确度和精密度,分析结果与标样标准值吻合,除Cl、S、As、Br、Ce、Co、Ni、Th、Sc、Hf、Nb、Nd的精密度小于10.00%以外,其他各元素精密度均在5.00%以内,各元素检出限均满足化探要求。  相似文献   

3.
X射线荧光光谱法测定多种铁矿和硅酸盐中主次量组分   总被引:3,自引:15,他引:3  
欧阳伦熬 《岩矿测试》2005,24(4):303-306
采用熔融玻璃法,用Axios型X射线荧光光谱仪测定铁矿和硅酸盐中Fe2O3、SiO2、A l2O3、TiO2、CaO、MgO、SO3、MnO、V2O5、K2O、P2O5、Na2O、Co和N i等组分含量。使用理论α系数和经验系数法校正基体效应,经标准物质检验,分析结果与标准值基本吻合。用钒钛磁铁矿GBW 07225国家一级标准物质进行精密度试验,统计结果除K2O、P2O5、N i的RSD<15%,其余大多数组分的RSD<4.0%(n=12)。  相似文献   

4.
X射线荧光光谱法测定土壤样品中碳氮硫氯等31种组分   总被引:3,自引:3,他引:3  
利用新型的ZSX Primus Ⅱ型X射线荧光光谱仪采用粉末压片法直接测定土壤样品中的C、N、S、Cl等31种元素。各元素分析晶体为N采用RX45,C采用RX61,Na、Mg采用RX25,C1、S、P采用Ge,Si、Al采用PET,其余元素均采用LiF200。结果表明,方法的检出限、精密度和准确度对绝大多数元素而言,均可满足多目标地球化学调查样品分析的质量要求:  相似文献   

5.
朱晓贤 《地下水》2014,(4):197-198
利用电感耦合等离子体质谱法测定土壤、水系沉积物及岩石样品中的痕量银时,Zr 、Nb与氧的复合离子对银的测定结果产生干扰,经过反复试验计算出91 Zr16 O+对107 Ag+的干扰系数,利用系数进行在线干扰校正,用115 In内标校正仪器漂移和基体效应。经过对4个岩石标准物质,6个土壤标准物质和8个水系沉积物标准物质进行验证,测定结果与推荐值相吻合,能够满足岩土样品分析精密度和准确度的要求,同时也可进行钨、钼等元素的测量。  相似文献   

6.
发射光谱法快速测定银锡铜铅锌钼铍   总被引:4,自引:9,他引:4  
叶晨亮 《岩矿测试》2004,23(3):238-240
使用两台摄谱仪同时接收光谱,以K2S2O7、NaF、Al2O3为缓冲剂,Ge、Sb为内标,测定化探样品中7项元素,检出限(μg/g)分别是:Ag0.02,Sn0.5,Cu 1,Pb 2,Zn 10,Mo 0.2,Be 0.5;精密度(RSD,n=20)在2.9%~16.8%。采用国家一级标准物质验证方法可靠性,测定结果与标准值一致。  相似文献   

7.
徐婷婷  夏宁  张波 《岩矿测试》2008,27(1):74-76
采用混合熔剂熔融制备样片,用Axios X射线荧光光谱仪测定海洋沉积物样品中SiO2、Al2O3、Fe2O3、MgO、CaO、Na2O、K2O、P2O5、TiO2、MnO、BaO、Ni、Cu、V、Cr和Zn等16种组分,用理论α系数校正基体效应,分析方法的精密度(RSD,n=12)为Cu和Cr小于6%,其余大多数主次量组分小于2%。方法用海洋沉积物国家一级标准物质验证,测定值与标准值相符。  相似文献   

8.
采用压片制样波长色散X射线荧光光谱法对古陶瓷胎釉样品的Na2O、MgO、Al2O3、SiO2、P2O5、K2O、CaO、Sc、TiO2、V2O5、Cr2O3、MnO、Fe2O3、CoO、NiO、CuO、ZnO、Ga、As、Br、Rb、Sr、Y、Zr、Nb、Sn、Sb、Cs、BaO、La、Ce、Nd、Sm、Hf、PbO、Bi和Th等37个主、次、痕量组分进行测定。使用经验系数法和康普顿散射、背景作内标校正基体效应。方法经土壤和水系沉积物国家标准物质验证,测定值与标准值吻合;除个别组分,大多数元素11次测定的相对标准偏差(RSD)小于10%。方法的检出限、精密度和准确度能满足古陶瓷样品的分析要求,应用于7个古陶瓷样品的分析检测,分析结果与其他分析方法对比具有很好的一致性。  相似文献   

9.
采用粉末压片法制样,使用经验系数和散射线内标法校正元素间的吸收-增强效应,用3080E2X射线荧光光谱仪对试样中的Cl,Br,S三元素进行直接测定,其分析结果的精密度和准确度能满足区域化探样品的分析质量要求.  相似文献   

10.
采用熔融制样,以四硼酸锂-偏硼酸锂(质量比为67∶33)作熔剂,溴化铵作脱模剂,硝酸铵作氧化剂制备玻璃熔片。选用土壤、岩石、水系沉积物等国家标准物质拟合校准曲线,用经验系数法校正元素间的基体效应,各组分的线性相关系数均达到了0.999以上。使用日本理学ZSX PrimusⅡ型光谱仪对样品中SiO_2、Al_2O_3、TFe_2O_3、TiO_2、K_2O、Na_2O、CaO、MgO、MnO、P_2O_5等10种组分进行同时测定,分析结果与标准物质认定值或化学方法结果相符,相对标准偏差(RSD,n=12)小于5%,准确度和精密度均已达到地质矿产行业标准规范要求。方法简便、快速、准确、高效且绿色环保,满足了硅酸盐样品中主量元素快速分析测试的需求。实验表明,利用X射线荧光光谱法对硅酸盐主要成分含量进行同时分析是可行的。  相似文献   

11.
X射线荧光光谱法同时测定土壤样品中碳氮等多元素   总被引:14,自引:13,他引:14  
报道了采用粉末压片制样-X射线荧光光谱法测定土壤样品中C、N、S、Cl、Br、Hf、Mo、Sn、Se、Na、Mg、Al、Si、P、K、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Rb、Sr、Y、Zr、Nb、Ba、La、Ce、U、Th、Pb等38种元素的分析方法。着重研究了C和N的分析条件、存在问题和注意事项。所拟方法的检出限,精密度和准确度大多数满足覆盖区多目标地球化学调查样品分析质量的要求。  相似文献   

12.
The freshwater marshes in northern China are heavily impacted by anthropogenic disturbances such as cultivation and fertilization and increased levels of nutrients (especially N and P) through atmospheric deposition and agricultural surface runoff. These disturbances have affected the emission of N2O from these systems. This laboratory study was conducted to determine the effects of increased inputs of inorganic N and P on N2O emission from marsh soil in response to different soil moisture conditions. The results showed that the emission of N2O increased with the enhancement of N inputs when the soil was submerged, but that the highest N treatment suppressed the emission of N2O when the soil was at 60% water holding capacity (WHC), which may have occurred due to an inadequate amount of available C. Furthermore, the results of this study indicated that a small amount of N fertilizer induced much more N2O evolution from freshwater wetland soil, while P fertilizer inputs appeared to stimulate the emission of N2O only during the first few days of the experiment. Additionally, soil that was treated with P appeared to absorb N2O when it was at 60% WHC after around 6 weeks of the incubation, which indicates that the input of P fertilizer might serve as a shift of source or N2O sink in wetland soils under non-flooded conditions. When compared to soil at 60% WHC, submerged soil had significantly higher N2O emissions, except when subjected to the medial N treatment. These findings indicate that the soil moisture condition had a significant effect on N2O emissions when the same amount of N or P was applied. Therefore, the effects of N and P fertilization in the northern temperate wetlands cannot be neglected from regional or national emissions of N2O.  相似文献   

13.
Soils (n=250) were collected from ten salt and brackish-water marshes of North Carolina and analyzed for organic matter content by loss on ignition (LOI) and Kjeldahl nitrogen (KN). Total organic carbon and total nitrogen were determined on the same samples using an elemental CHN analyzer. Regression analyses indicated that LOI and KN were excellent estimators of organic C (R2=0.990) and total N(R2=0.986), respectively, in low clay content (0–11%) marsh soils containing a wide range of soil organic C (0.1–28%) and total N (0–1.6%). A quadratic equation best described the relationship between organic C and organic matter (Organic C=0.40 [LOI] +0.0025 [LOI]2) while a linear model accurately described the relationship between total N and Kjeldahl N (Total N=1.048 [KN]?0.010). The proportion of organic C in organic matter (C/OM) increased with increasing soil organic matter content, probably as a result of aging. Young marshes, which are characterized by low soil organic content contain C/OM ratios similar to emergent vegetation (40–45%). In old organic soils (70–80% organic matter), C/OM increased to 57–60% due to accumulation of reduced organic materials.  相似文献   

14.
The lack of analytical techniques for halogens in geological materials is mainly due to the loss of analytes during sample preparation. This study describes a rapid bulk rock digestion method (NH4F digestion) for determination of the abundances of Cl, Br and I in geological materials by SF-ICP-MS. During high temperature (200–240 °C) digestion, NH3 released from the decomposition of molten NH4F can effectively prevent the loss of halogens released from geological samples. Chlorine, Br and I were not lost during NH4F digestion at 220 °C for 0.25–6 h. The limits of quantitation for NH4F digestion were 2.8, 0.018 and 0.003 μg g-1 Cl, Br and I, respectively. Most results for halogens in geological reference materials by NH4F digestion were in agreement with their certified values, confirming that the high-performance rapid bulk rock NH4F digestion has sufficient digestion capability to extract Cl, Br and I from rocks, sediments and soils. In comparison, results obtained following acid digestion showed that HNO3 + HF digestion could effectively extract Br and I from soil and sediment samples, and that HNO3 acid digestion is only suitable to use for the determination of Br and I in soil samples.  相似文献   

15.
应用高频燃烧-红外碳硫分析仪测定农用地土壤质量调查样品中碳、硫的含量,解决了土壤样品中碳、硫测定过程中存在的基体影响和低电磁感应等问题。对样品称样量、助熔剂的加入量、氧气流量等测定条件进行优化试验,用国家一级标准物质验证了方法准确度和精密度,相对误差(RE)小于10%,相对标准偏差(RSD,n=8)总碳小于2%,硫小于9%。方法能够满足农用地土壤质量调查样品的分析质量要求。  相似文献   

16.
建立了二氯甲烷溶剂辅助微波消解-电感耦合等离子体质谱法测定原油中V、Cr、Fe、Ni、Cu、Zn、Mo、Co、Pb等16种微量金属元素。研究表明,用CH2Cl2分散原油样品,以浓HNO3-H2O2为消解体系,采用CEM微波消解系统消解样品,各元素线性关系良好,相关系数≥0.9995;检出限可达ng/L;方法精密度较高,相对标准偏差(RSD,n=3)<5.0%;回收率为92%~110%。以w(Ni)/w(V)与w(Fe)/w(V)比值为变量参数对不同原油样品进行聚类分析,表明国内与国外不同地区原油样品中各金属元素含量差异较大。  相似文献   

17.
采用Luminol-H。O。Air(巨)化学发光反应体系作为分析检测方法,建立了一个测定地质样品中痕量锑的化学发光分析法。方法的原理是用AgNO。吸收由样品发生的氢化锑气体,使吸收液中生成Sb(巨)与过量的K。Cr。O,反应生成Cr(1),方法的检出限为0.6us/mlSb,工作曲线的线性范围是2~1000ng/mlSb,测定的相对标准偏差小于5%。本方法已用于地质样品中痕量佛的测定。  相似文献   

18.
土壤样品中有机磷农药的加速溶剂萃取-气相色谱测定   总被引:7,自引:4,他引:3  
饶竹  何淼  陈巍  李松  刘艳 《岩矿测试》2010,29(5):503-507
建立加速溶剂萃取提取土壤样品中13种有机磷农药残留,经Carb柱净化、Rtx-OPP2大口径毛细管柱分离、气相色谱-火焰光度检测器检测。方法仪器检出限在0.67~1.50ng/mL,线性范围在0.67~600ng/mL,相关系数在0.9994~0.9999。模拟土壤样品和实际土壤样品基体加标回收率分别在54.3%~106%和60.7%~133%,方法精密度(RSD,n=5)在2.2%~9.9%。方法简便、灵敏,适用于土壤样品中有机磷农药残留的分析。  相似文献   

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