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离子色谱-电感耦合等离子体质谱联用法测定水中痕量BrO-3及Br- 总被引:14,自引:0,他引:14
建立了离子色谱-电感耦合等离子体质谱联用技术(IC-ICP-MS)用于饮用水中的痕量BrO-3及Br-的测量.使用DIONEX Carbopac PA-100(4 mm×250 mm i.d.)在流速1 mL/min及5 mmol/L NH4NO3(pH 5.7)淋洗液下进行BrO-3和Br-的分离.该方法以100 μL进样量对BrO-3的检出限为0.0027 μmol/L(0.22 μg/L);对Br-的检出限为0.0067 μmol/L (0.54 μg/L).对水样的分析结果表明,所测矿泉水中的BrO-3浓度大大超出了世界卫生组织最新<饮用水水质准则>中所规定的溴酸盐的指导值,而所测量的青岛崂山区生活用水则未检出BrO-3. 相似文献
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建立草酸沉淀分离氧化钕,用校正方程消除残余钕离子产生的双电荷离子干扰,电感耦合等离子体质谱法测定砷含量的方法。选择了溶解样品条件,硝酸溶解样品即能满足检测要求;优化了仪器条件,功率1500W,雾化器流量0.86L/min;进行了内标元素的选择,确定Rh为最佳校正内标元素;确定用草酸分离基体并结合干扰校正方程消除钕的双电荷离子干扰;方法检出限为0.029 ng/mL,定量限为0.097 ng/mL。采用方法对实际样品进行测定,回收率(n=11)为94%~104%,相对标准偏差(RSD,n=11)为0.56%~5.82%。 相似文献
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高效液相色谱-电感耦合等离子体质谱联用技术测定水产类膳食中5种砷形态的方法研究 总被引:8,自引:0,他引:8
采用高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用技术建立了三价砷As(Ⅲ)、砷甜菜碱(AsB)、二甲基砷酸(DMA)、一甲基砷酸(MMA)、五价砷As(Ⅴ)5种砷形态的分析方法。采用超声溶剂提取法对水产类膳食样品和带鱼等水产品进行前处理后,对砷形态进行分析。实验表明,5种砷化合物的线性范围为2.5~500μg/L,相关系数(r)均大于0.999 0,检出限为0.6~0.9μg/L,RSD均小于5%。采用加标回收考察方法的准确性,加标回收率为87%~124%。样品的测定结果显示,水产品及水产类膳食中砷形态的主要存在形式为砷甜菜碱。 相似文献
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An inductively coupled plasma mass spectrometer (ICP‐MS) was used as a liquid chromatographic detector for the speciation analysis of thallium in environmental samples. In this study, ionic thallium species, namely Tl(I) and Tl(III) were well separated by reversed‐phase high performance liquid chromatography (RP‐HPLC) with a C8‐HPLC column as the stationary phase and 1 mmol L?1 tetrabutylammonium phosphate (TBAP), 2 mmol L?1 diethylenetriamine pentaacetic acid (DTPA) in 1% v/v methanol solution (pH 6) as the mobile phase. Effluent from the HPLC column was delivered to the nebulizer of the ICP‐MS for the determination of thallium. The separation was complete in less than 3 min. Detection limit was 0.002 μg L?1 for both Tl(I) and Tl(III) compounds based on peak height. The relative standard deviation of the peak areas for five injections of a mixture containing 1 μg Tl L?1 was better than 3.4%. The concentrations of Tl compounds were determined in standard reference materials, including NIST SRM 1643e Trace Elements in Water and NRCC NASS‐5 Open Ocean Seawater and water samples collected in Kaohsiung area, Taiwan. The HPLC‐ICP‐MS results of the reference samples agreed with the reference values. This method has also been applied to determine Tl(I) and Tl(III) compounds in custard apple (Annona squamosa) leaves collected from Chai‐shan Mountain, Kaohsiung and Taitung City, Taiwan. The thallium species were quantitatively leached from the leaves with a 5 mmol L?1 DTPA in 100 mmol L?1 ammonium acetate solution in an ultrasonic bath during a period of 30 min. The HPLC‐ICP‐MS result that was obtained after the analysis of leaves sample showed a satisfactory agreement with the total thallium concentration obtained by ICP‐MS analysis of completely dissolved sample. 相似文献
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An ion chromatography‐inductively coupled plasma mass spectrometric (IC‐ICP‐MS) method for the speciation of sulfur compounds, namely sulfite [SO32?], sulfate [SO42?] and thiosulfate [S2O32?], was described. Ionic sulfur compounds were well separated in about 3 min by ion chromatography with a Hamilton PRP‐X100 column as the stationary phase and 60 mmol L?1 NH4NO3 and 0.1% v/v formaldehyde (HCHO) solution (pH = 7) as the mobile phase. The analyses were carried out using dynamic reaction cell (DRC) ICP‐MS. The sulfur‐selective chromatogram was determined at m/z 48 as 32S16O+ by using its reaction with O2 in the reaction cell. The method avoided the effect of polyatomic isobaric interferences at m/z 32 caused by 16O16O+ and 14N18O+ on 32S+ by detecting 32S+ as the oxide ion 32S16O+ at m/z 48, which is less interfered. The detection limit of various species studied was in the range of 3.6–4.6 ng S mL?1. The accuracy of the method has been verified by comparing the sum of the concentrations of individual sulfur compounds obtained by the present procedure with the total concentration of sulfur in several natural water samples. The recovery was in the range of 97–102% for various compounds studied. 相似文献
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分别将N-(β氨乙基)-γ-氨丙基三甲氧基硅烷(AEAPTMS)、3-巯丙基三甲氧基硅烷(MPTMS)与四乙氧基硅烷(TEOS)水解共聚,制备氨基\巯基键合的硅胶材料.将此材料作为固相萃取(SPE)小柱的填充材料,建立了固相萃取快速分离富集海产品样品中五价砷As(Ⅴ)和三价砷As(Ⅲ),电感耦合等离子体质谱(ICP-M... 相似文献
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电感耦合等离子体光谱/质谱联机同时测定多金属结核中常量、微量、痕量元素 总被引:9,自引:0,他引:9
采用电感耦合等离子体质谱(ICP-MS)与等离子体光谱(ICP-OES)联机同时测定多金属结核样品中常量、微量、痕量元素。样品经高压密封溶样弹消解后,一次气动雾化进样,ICP-OES测定常量和微量元素,ICP-MS测定微量和痕量元素。详细探讨了不同浓度范围元素的测定方式、元素分析信号的采集模式、多原子离子干扰的校正因子。采用ICP-MS与ICP-OES二种方式同时测定Co、Cu、Ni、Zn、V、Ba、Sr,分析结果表明具有较好的一致性。所建立的ICP-MS与ICP-OES联机检测技术用于多金属结核标准样品的分析(Nod-A-1,GSPN-1,GSPN-2,GSPN-3),分析结果与推荐值符合,相对标准偏差小于10%。 相似文献
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电感耦合等离子体质谱法测定黄沙土壤中铅同位素比 总被引:4,自引:0,他引:4
用电感耦合等离子体质谱法(ICP—MS)测定了5个黄沙原土样品中铅同位素比207Pb/206Pb、208Pb/206Pb,样品来自被认为是黄沙气溶胶源地区,为了使铅同位素测量中质量偏差和漂移减至最少,在样品中加入了铊标准溶液,测量205Tl/203Tl比,校正质量数差别选择的影响.同时,采用ICP—MS和电感耦合等离子体原子发射光谱法(ICP一AlS)测定了随粒径变化样品中12种元素浓度的变化. 相似文献
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等离子体质谱法测定珊瑚锶和钙 总被引:9,自引:0,他引:9
研究了珊瑚中Sr(~8000ug/g)、Ca(~400mg/g)在同一份溶液中的等离子体质谱的同时测定。所有样品均加入Sc和Y作内标元素分别控制测定Ca和Sr时的仪器波动。本方法Sr、Ca测量精度(RSD%)分别~0.3%、~1%。90个珊瑚样品Sr分析结果中,仅有7个样品Sr数据与同位素稀释热电离质谱法数据相比,相对偏差较大(~1%),其它数据相互吻合。本方法适合珊瑚样中Sr的快速测定,并可以此 相似文献
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电感耦合等离子体质谱的微量进样系统分析性能评价及其应用 总被引:1,自引:0,他引:1
用2种微量雾化器组装成微量进样系统与常规气动雾化方式的ICP-MS的分析性能作了详细比较。FM02雾化器在22μL/min低提升率下,20μg/L的Be、Co、In和Bi进行10次平行测定的RSD分别为7.6%、3.0%、2.7%和1.8%;检出限分别为0.14、0.10、002和0.01μg/L;^115In的信号强度达到常规气动雾化器1.3mL/min提升速率下的60%,显示了良好的分析性能。对20μL Wistar鼠的羊水样品中La、Ce、Pr和Nd4种元素的测定结果与常规进样系统的结果完全吻合。 相似文献
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逆流色谱分离感应耦合等离子质谱在线测量超痕量钚 总被引:3,自引:0,他引:3
将逆流色谱(CCC)与感应耦合等离子质谱(ICP-MS)相联,研究了几种两相体系在CCC中的固定相保留率,从中选择1%TNOA-正庚烷作固定相,通过CCC富集分离钚并去除基体及干扰元素,通过研究在线分离条件及定量方法等,建成了CCC分离ICP—MS在线测量超痕量钚的方法。采用该方法分析得到实际土壤样品中^239Pu的含量与由传统的分离方法给出的结果相吻合。 相似文献
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高效液相色谱-电感耦合等离子体质谱技术测定海水中锡化学形态 总被引:3,自引:1,他引:3
建立了反相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS),用于测定海水中一丁基锡(MBT)、二丁基锡(DBT)、三丁基锡(TBT)和三苯基锡(TPhT)。分别使用两种不同色谱柱C18ACE和TC-C18,缓冲溶液V(acetonitrile)∶V(water)∶V(acetic acid)∶V(TEA)=65∶23∶12∶0.005%,在分别在流速0.2和0.4 mL/min下对4种不同形态的锡进行分离。所建立的方法在20μL进样量下,对DBT、MBT、TBT及TPhT的检出限分别为30、50、80及10 ng/L。对青岛沿岸海水分析的结果表明海水中DBT、TPT含量分别为35和20 ng/L,而MBT及TBT的含量则低于本方法的检出限。 相似文献