电感耦合等离子体质谱法(ICP-MS)测定地下水中十五项稀土元素

采用电感耦合等离子体质谱法(ICP-MS)测定地下水中十五项稀土元素具有干扰少、谱线相对简单、检出限低、动态线性范围宽和能够进行"多元素同时分析"与快速同位素分析等特点。测定各个稀土元素方法加标回收率在86.0%~108%之间,检出限低于0.008μg/L,相对标准偏差小于4.7%,适用于地下水中微量稀土元素的测定。     

微波消解-电感耦合等离子体质谱法测定面制食品中铝的含量

本文以Li6为内标,采用微波消解-电感耦合等离子体质谱法(ICP—MS)对面制食品中铝的含量进行测定,通过对三种面制食品的加标回收试验,建立了面制食品中铝含量的ICP—MS分析方法,仪器检出限为在0.12ng/mL、测定的相对标准偏差均小于5.2%,加标回收率在90.4%97.6%。实验表明该法操作简单、快速,灵敏度高,重现性好,能够满足实际样品检测的要求。     

ICP-MS法同时测定金属包装材料中8种可溶性有害元素

建立了电感耦合等离子体质谱(ICP-MS)法同时测定金属包装材料中砷、钡、镉、铬、铅、锑、硒、汞等8种可溶性有害元素的分析方法,全面考察了消解剂种类及其用量、内标元素的选择及方法的干扰等影响其测量的各种因素,确定了最佳的实验测定条件。方法的检出限为0.03~0.18μg/L,相对标准偏差(RSD)小于5%,加标回收率为87.4%~118.1%。采用该法对金属包装材料实际样品进行了分析,结果表明,此方法简单、准确、重现性好。     

ICP-MS测定土壤和水系沉积物中的微量银

样品经三酸(HF+HNO3+H2SO4)完全分解后采用ICP-MS测定银时,锆会产生强烈干扰。为消除这种干扰,提高结果准确度,建立离线干扰校正方法。通过测试4件水系沉积物及9件土壤国家标准物质,选择最适测定条件:溶液酸度为1.0%,内标为10 ng/m L Rh、In,采用94Zn消除锆对107Ag干扰。实测结果表明该方法检出限为5.8 ng/g,精密度为5.80%,测试值与推荐值吻合,误差在标准物质允许范围内。该方法具有简便、快捷、准确的优点,还能实现多元素同时测定。     

微波消解-电感耦合等离子体质谱(ICP-MS) 同时测定塑料包装材料中有毒有害元素

采用硝酸-过氧化氢消解体系,及高压密闭微波技术处理塑料包装材料,建立了电感耦合等离子体质谱法同时测定塑料包装材料中铅、镉、砷、铬、锑、汞、硒、钡、镍、锡、锶、铊多种有毒有害元素的方法。方法的检出限为0.02~0.20μg/L,相对标准偏差(RSD)小于10%,加标回收率为88.0%~117.0%。该方法简单、快速、灵敏、准确度好。     

电感耦合等离子体质谱法(ICP-MS)测定北京地区常见野菜重金属含量

为科学评价北京地区常见几种野菜的重金属含量,选取苜蓿、苦菜、蒲公英、车前草、荠菜五种野菜为研究对象。采集北京多个区县高速公路两旁、山林、居民区、公园等区域内的野菜样品,采用微波消解+电感耦合等离子体质谱仪(ICP-MS)测定铅、镉、铜、铬、砷5种重金属在野菜中的含量。根据测定数据发现北京地区野外野菜重金属含量普遍超过GB 2762-2017《食品安全国家标准食品中污染物限量》的要求,公园和山林的铅、镉等重金属含量不低于甚至超过道路两侧野菜。食用非人工种植的北京地区野菜,会导致人体出现健康风险。应广泛宣传教育,提倡减少食用重金属含量超标的野菜产品,未雨绸缪预防长期累积性食品安全问题的发生。     

微波消解-电感耦合等离子体质谱法同时测定土壤样品中八种重金属元素

本文以Ge、In、Re内标校正体系,采用微波消解-电感耦合等离子体质谱（ICP—MS）对土壤样品中砷、铅、铜、锌、镉、铬、汞、镍八种重金属元素进行同时测定,通过加标回收试验,建立了土壤样品中砷、铅、铜、锌、镉、铬、汞、镍八种重金属元素ICP—MS分析方法,各元素检出限均小于1．0ng／mL,测定8种元素的相对标准偏差均小于10％,各元素的加标回收率在86．3％～101．0％。实验表明：该法操作简单、快速,灵敏度高,重现性好,而且能够对八种重金属元素进行同时测定,大大提高了检测效率。     

ICP-MS测定海水中的铅镉汞锌

通过对海水中微量元素的检出限、加标回收及对标准样品的测定，证明该法具有前处理简单、干扰少、检出限低、测定快速、能同时测定多种元素等优点。     

ICP-MS法在测定痕量贵金属中的应用探析

ICP-MS技术测量手法是对元素的含量进行分析的一种技术手段,主要的测定的范围是痕量与超痕量元素。随着时代的进步与科技的发展,这种技术也得到了革新与完善。文中主要针对ICP-MS技术分析性能在贵金属中的应用进行了简要分析,仅供专业人士的参考与借鉴。     

ICP-MS法测定保鲜薄膜中微量溶出铅镉的研究

采用电感耦合等离子体质谱(ICP-MS)法,用4％乙酸溶液萃取分离Pb,Cd,对保鲜薄膜表面微量溶出元素Pb和Cd进行了分析.对影响其测量的各种因素进行了较为详细的研究,确定了实验的最佳测定条件.结果表明,方法的检出限为:0.03(Pb)和0.02μg/L(Cd),回收率为94.4％～104.2％,RSD小于2.02％.该法准确、快速、简便,应用于保鲜薄膜中的微量溶出铅镉的测定,结果满意.     

ICP-MS测工业原材料氯化钕中的As含量

ICP-MS测工业原材料氯化钕中的As含量,发现存在基体干扰后通过内标校正得到一个测试值,样品用XRF扫描结果为ND,用ICP测试虽然谱线存在一定的干扰,但测试结果同ICP-MS的比较相差2个数量级,通过查找相关文献发现Nd有一个同位素150,双电荷的干扰是ICP-MS固有的,虽然可通过适当选择仪器操作条件降低其干扰,但目前无法从根本上消除,最后采用反应模式用AsO代替As避免双电荷的干扰从而得到正确的测试结果。     

食品原料超微粉碎后性能的变化

对食品原料超微粉碎后营养成分、功能性成分、自身理化性能、功能活性及加工性能等方面的改变进行综述。提出食品原料超微粉碎能提升食用和加工性能,利用率提高,加工性能改善,提升产品品质,应用前景最广阔,将为食品资源的开发的重要手段和主流发展方向;对食品原料进行深度加工和广度加工,能获得更理想的符合感官需求的成品,获得更多的可利用食品资源。     

电感耦合等离子体质谱法测定土壤中痕量铊

在使用王水-HClO4-HF消解法对土壤进行消解后,采用ICP-MS法测定土壤中痕量的铊。对王水-HClO4-HF消解法中王水冷浸时间、HClO4和HF的用量进行优化,发现在土壤取样量为0.500 0 g,王水冷浸时间为4 h,HF用量为4 m L,并且在保证测定值准确的情况下不需要加入HClO4,是测量土壤中痕量的铊的最佳条件。通过一系列的实验建立一种更加准确,经济,灵敏检测土壤中痕量铊的ICP-MS方法。     

应用AFS—930型双道原子荧光光度计联合测定水中的砷和硒

本文采用原子荧光光谱法,研究了联合测定水样中砷和硒的技术。用10%盐酸和1%硫脲-1%抗坏血酸混合试剂处理样品,并以2.0%硼氢化钾和0.5%氢氧化钠为还原剂,在5%的盐酸介质测定砷和硒。砷和硒的检出限分别为:0.20μg/L和0.13μg/L,本方法具有操作简便、快速、基体干扰少、灵敏度高等优点,可用于水样中砷和硒的联合测定。     

Evaluation of various digestion procedures for trace element contents of some food materials

The levels of trace elements in different types of food material consumed in Turkey were determined by flame and graphite furnace atomic absorption spectrometry. Food samples were digested with dry ashing, wet ashing and microwave digestion procedures in this study. The microwave digestion procedure was chosen for the digestion of all the food samples because it required shorter time and made higher recovery (specially for Se). Fe, Cu, Mn, Zn, Al and Se were determined by flame and graphite furnace atomic absorption spectrometry, respectively. Relative standard deviations (RSD) were found below 10%. The accuracy of the procedure was confirmed by certified reference materials. Moreover, this procedure was easier to use when compared with dry and wet digestions.     

ICP-MS法同时测定卷烟主流烟气中的7种痕量元素

建立卷烟主流烟气中7种有害痕量元素的测定方法。采用剑桥滤片和吸收瓶分别捕集卷烟主流烟气中粒相物和气相物中的As、Cd、Cr、Pb、Ni、Se、Hg元素,硝酸-过氧化氢混合溶液微波消解后,用电感耦合等离子体质谱(ICPMS)法同时测定捕集到的7种元素。方法相对标准偏差15%(n=6),检出限为0.12~2.3 ng/支,回收率为82%~110%。     

Evaluation of metal migration and determination of trace metals after microwave digestion for lithographic materials

The radioactive tracer technique was applied to investigate the migration of cesium and zinc impurities from bottom antireflective coating (BARC) and photoresist (PR) into underlying substrate. The effects of normal baking temperatures and substrate types were studied. Our results indicated that BARC has higher migration ratios than PR, irrespective of the substrate types and normal baking temperatures. The substrate type did not appear to strongly affect the metal migration ratios. However, water and/or solvent evaporation due to temperature change was found to have a significant effect on metal migration. The diffusion profiles of BARC and PR were depicted based on diffusion equations and the migration ratios. Both the UV/visible spectrometric and the gravimetric methods were successfully implemented to evaluate the feasibility of closed-vessel microwave digestion efficiency for BARC and PR samples. By following the established microwave digestion method and the inductively coupled plasma mass spectrometer (ICPMS) determination, the detection limits obtained for multielements were in the ppb and sub-ppb levels. Except for calcium, the spike recoveries of metals ranged from 91 to 132% and 87 to 125% for BARC and PR, respectively. The analytical results were found to be in reasonably good agreement with the literature values.     

Detection of trace melamine in raw materials used for protein pharmaceutical manufacturing using surface-enhanced Raman spectroscopy (SERS) with gold nanoparticles

Melamine, a nitrogen-rich molecule, was found as an adulterant in pet foods in 2007 in North America and in milk products in 2008 in China. These scandalous abuses of melamine have alarmed the biopharmaceutical industry and the FDA and alerted them to potential adulteration and contamination of melamine in raw materials used to make protein therapeutics. Highly sensitive analytical methods are needed to screen melamine adulteration and contamination in raw materials. We conducted surface-enhanced Raman spectroscopy (SERS) experiments to test trace melamine spiked in three raw materials commonly used for protein pharmaceutical formulation and purification, including sucrose, urea, and arginine, with a portable Raman device and gold nanoparticles. The detection limit of 10 ppb in raw material dissolved in 30:70% water/acetonitrile is equivalent to 0.5 ppm in solid raw material. It has excellent linearity in the concentration range measured. The cross-validation regression coefficient R(2) and the standard error of prediction (SEP) are 0.960 and 7.18 ppb, respectively, in sucrose. The R(2) and SEP are 0.958 and 9.15 ppb in urea. It has a relatively lower R(2) = 0.630 and a SEP of 35.0 ppb in arginine, which could be due to the competitive adsorption of arginine molecules to the surfaces of gold nanoparticles. The detection of melamine using the SERS technique is rapid (within 3 minutes), convenient, and requires no extraction procedure, offering an alternative method for screening melamine in raw materials at biopharmaceutical manufacture sites.