碰撞池反应-电感耦合等离子体质谱(ICP-MS)法测定出口食品营养强化剂中的26种元素

采用碰撞池反应-电感耦合等离子体质谱(ICP-MS)法建立了11种营养强化剂中26种元素的He碰撞反应池模式下的全定量检测方法。考察了不同的样品处理方式及样品称样量对分析过程的影响,比较了普通模式和He碰撞反应池模式的优缺点。实验结果表明,对于易溶性营养强化剂可以采用直接酸溶液溶解进样方式,且定容体积为10mL时有机强化剂称样量控制在0.20g、无机强化剂称样量控制在0.10g以下时基体干扰较小,可得到满意的测定结果。各元素加标回收率在81.0%～110%,相对标准偏差(RSD)为2.1%～5.4%,可实现对26种元素一次性测定,为河北辖区出口营养强化剂提供分析方法和风险监控分析依据。     

六极杆碰撞反应池-等离子体质谱测定生物样品中痕量铬和钒

采用带六极杆碰撞反应池的电感耦合等离子体质谱直接测定了生物样品中痕量铬和钒。在碰撞反应池中引入He/NH3(93∶7)混合气,有效地消除了分子离子(ArC 、NCl 、Cl O 、Cl OH 等)对超痕量铬、钒测定的干扰,降低了方法的检出限。比较了干法灰化和湿法消解两种样品处理方法,两种消解方式获得的结果基本一致。方法的检出限(3σ):钒为0.005 0μg.g-1,铬为0.001 8μg.g-1。相对标准偏差:钒为3.25%~14.08%;铬为4.20%~8.24%。经国家一级生物标准物质验证,测定值与标准值吻合。     

石墨消解-动态反应池模式-电感耦合等离子体质谱法测定烟用香精和料液中5种元素的含量北大核心CSCD

将烟用香精和料液样品0.3 g(精确至0.001 g)置于全自动石墨消解仪消解罐中,分3次加入消解液(共计10 mL硝酸、1 mL高氯酸),在170℃的最高消解温度下,样品消解完全.所得溶液用水定容至50 mL,采用电感耦合等离子体质谱法(ICP-MS)测定其中砷、铅、镉、铬、镍等元素的含量.以铟为内标,铬、镉、镍、铅、砷元素的测量同位素分别为^(52)Cr、^(111)Cd、^(60)Ni、^(208)Pb、^(75)As,使用动态反应池(DRC)模式消除了铬、砷元素的质谱干扰,铬、镉、镍、铅等元素的测定选择氦气碰撞模式,砷元素的测定选择氢气反应模式.结果表明,5种元素的质量浓度在一定范围内与各元素与内标计数值的比值呈线性关系,检出限(3s)为0.016~0.035 mg·kg^(-1).按标准加入法进行回收试验,各元素回收率为91.5%~111%,相对标准偏差(n=6)为0.28%~3.1%.方法用于10个烟用香精和料液样品的分析,铬、砷、镍的检出量分别为0.019~0.061 mg·kg^(-1),0.039~0.061 mg·kg^(-1)和0.022~0.031 mg·kg^(-1),镉和铅未检出.     

微波消解-电感耦合等离子体质谱(ICP-MS)法测定硅石中五种杂质元素

采用微波消解溶解样品,建立ICP-MS法测定硅石中锰、铜、钒、钛、铬5种杂质元素的方法。探讨了溶解样品及消除干扰的最佳方式,选用Sc(10μg/L)为内标,动态反应池(DRC)模式进行测定。方法检出限为0.1mg/kg(51V)~1.66 mg/kg(47Ti),加标回收率在88.6%~109%,相对标准偏差均小于3%。方法快速准确,精密度好,检出限低,适合硅石中5种杂质元素的测定。     

高效液相色谱-电感耦合等离子体质谱联用技术测定皮革中Cr(Ⅵ)

本文建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)法测定皮革中Cr(Ⅵ)含量。采用Dionex AS19色谱柱,以NH4NO3(pH=7.4)为流动相,在流速为1.0mL/min的条件下,可以很好地分离Cr(Ⅲ)与Cr(Ⅵ)。在色谱进样量为100μL,质谱采用He碰撞池模式下,对Cr(Ⅵ)的检出限达到了0.02μg/L;2.0、20.0μg/L两个加标水平的回收率分别为93.5%~97.0%和97.8%~102.3%,方法精密度优于4.1%,可以满足测定要求。应用该方法测定了各类皮革产品中的Cr(Ⅵ)。     

硝酸-过氧化氢敞口消解/ICP-MS测定植物样品砷含量

选取了玉米秸秆与籽粒、小麦秸秆与籽粒、烟草等5种不同的植物样品,加入硝酸-过氧化氢,进行敞口消解,消解液中As(⁷⁵As)采用电感耦合等离子体质谱仪He碰撞模式测定,以⁷²Ge为内标元素。结果表明：2个国家生物成分分析标准物质GBW10011(GSB-2,小麦)和GBW10020(GSB-11,柑橘叶)砷的测定值在标准确认值范围内;在植物样品中加入砷标准溶液,加标回收率在87%~104%之间;方法检出限为0.0055 μg/g,灵敏度较高;对4个植物样品分别重复测定5次,相对标准偏差均小于10%。本文结论认为电感耦合等离子体质谱仪He碰撞模式可以用于测定硝酸-过氧化氢敞口消解植物样品中砷含量,该方法测定结果准确可靠,重现性好,灵敏度高。     

湿法消解ICP-MS法测定紫菜和海带中15种元素

以HNO3-HClO4作为消解液,采用电热板湿法消解样品,ICP-MS法建立了同时测定紫菜和海带等高盐样品中As,Pb,Cd,Cr,Hg,Mn,Fe,Co,Ni,Cu,Zn,Se,Ag,Sr和Ba等15种元素的分析方法。通过优化仪器条件,选择带碰撞池的He模式和耐高盐(HMI)模式,避免了样品中盐分带来的双电荷干扰和基体效应等常见干扰。被测元素的检出限为4.0×10-3~0.283 ng/g,相对标准偏差(n=11)低于10%。方法经国家标准物质GBW10023(紫菜)验证,与标准值一致。方法适用于紫菜和海带等高盐样品的质量控制和安全风险评估。     

电感耦合等离子体质谱法测定玩具材料中17种有毒有害元素

玩具材料样品经微波消解处理,采用电感耦合等离子体质谱法测定所得样品溶液中铝、锑、砷、钡、硼、镉、铬、钴、铜、铅、锰、汞、镍、硒、锶、锡、锌等17种有毒有害元素的含量。使用碰撞反应池技术消除了多原子离子对部分被测元素的干扰。方法的检出限为0.003~0.09μg.L-1。方法用于彩色布样品中17种元素的测定,加标回收率在84.5%~106.0%之间,相对标准偏差(n=7)在1.00%~5.79%之间,该方法完全达到了即将出台的欧盟玩具安全新指令的检测要求。     

电感耦合等离子体质谱法同时测定植物类新食品原料中14种无机元素北大核心CSCD

0.500 0g样品经硝酸3mL、过氧化氢2mL消解后,采用电感耦合等离子体质谱法同时测定样品溶液中Na、Mg、Ca、Al、Cu、Zn、Fe、Mn、Se、Pb、Cd、As、Hg和Cr的含量。采用0.5%(体积分数)硝酸的基体酸度增强分析元素的信号强度;在两次测试之间用100μg·L-1 Au-5%(体积分数)硝酸溶液清洗仪器,降低Hg的吸附效应;利用甲烷碰撞动态反应池技术消除了分析过程中的质谱干扰,选择Sc、Y、In、Bi为内标元素校正基体效应。14种元素的质量浓度在一定范围内与信号强度呈线性关系,检出限(3s)在0.003~0.039μg·L^(-1)之间。方法用于分析国家标准物质GBW 10027,各元素测定值与认定值相符,测定值的相对标准偏差(n=6)在1.6%~14%之间。     

有机溶剂溶样-电感耦合等离子体质谱法直接测定六氟磷酸锂中26种杂质元素

建立了电感耦合等离子体质谱(ICP-MS)法直接测定六氟磷酸锂中26种杂质元素(Be,Na,Mg,Al,K,Ca,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,Sr,Zr,Mo,Pd,Ag,Cd,Sn,Sb,Ba,Pb)的分析方法。样品用无水乙醇溶解后直接用ICP-MS测定。通过在等离子体中引入氧气,避免样品溶液中高浓度碳冷凝沉积在质谱锥接口和离子透镜上导致分析元素灵敏度的降低的现象,采用碰撞/反应池(CRC)技术校正了多原子离子质谱干扰,选择基体匹配法校正了基本效应。结果表明,26种杂质元素定量标准曲线的线性相关系数不小于0.9995,检出限在0.6~31.9 ng/L之间,RSD为2.5%~7.3%,加标回收率在90.6%~108.6%之间。本方法能满足六氟磷酸锂中杂质元素的分析要求。     

电感耦合等离子体质谱法测定手机壳套中14种可迁移元素

建立电感耦合等离子体质谱法测定手机壳套中14种可迁移元素含量的方法。样品经人工模拟汗液溶液振荡处理,使14种特定元素迁移至模拟溶液中,然后进行微波消解,采用电感耦合等离子体质谱法对消解液进行测定。14种元素在各自的质量浓度范围内具有良好的线性关系,相关系数均大于0.999,方法检出限为0.004~0.400μg/L。样品加标回收率为88.2%~99.5%,测定结果的相对标准偏差为2.5%~9.3%(n=5)。该方法操作简便,灵敏度高,线性范围广,定量准确,适用于手机壳套中14种可迁移元素含量的测定。     

电感耦合等离子体质谱法测定花生中34种元素

建立了微波消解-碰撞/反应池(ORS)电感耦合等离子体质谱仪(ICP-MS)同时测定花生中的Na、Mg、Ca、Fe、Se、Mo和稀土元素等34种元素的分析方法。样品经微波消解后,在线加入内标元素45Sc、72Ge、103Rh、115In和209Bi消除基体效应,应用碰撞反应池技术,以4.5 mL/min流速的氦气作为碰撞反应气,有效消除多原子离子产生的质谱干扰。各元素的检出限为0.0003～17.37ng/mL,相对标准偏差(RSD)低于2.9%;标准物质的测定值均在标准值范围内,结果令人满意。该方法可用于花生中多种元素的同时测定。     

火焰原子吸收光谱法测定铜冶炼渣中镍

通过对铜冶炼渣化学组成和性质的研究,确定了测定镍的实验方法。铜冶炼渣中二氧化硅含量在20%~40%,硫含量10%~20%,样品的分解具有一定的难度,必然影响镍的测定结果,因此需在样品分解过程中加入一定量的氟化氢铵、溴使二氧化硅生成四氟化硅、硫生成硫化氢挥发除去,溶液中其余共存元素主要有铜、银、铁、锌等元素不干扰测定结果,在硝酸(5%)介质中,用火焰原子吸收光谱法测定镍的含量,测定范围为0.01%~1%,加标回收率在99.5%~100.4%,测定结果的相对标准偏差(n=7)在0.61%~1.18%,检出限为0.004μg/mL,方法快速,简捷,能够满足日常生产检测需要。     

废弃线路板化学分析采样、制样及检测方法

介绍废弃线路板中有回收价值元素和有害物质分析的采样、制样及检测技术。样品经过分类采样、剪切破碎和高温灰化制样,采用样品全分析或副批混合样分析。通过提高称样量、多次测定求平均值的办法,火试金富集-重量法测定贵金属金、银。湿法王水溶解样品,碘量法测定主体元素铜。电感耦合等离子体发射光谱(ICP-AES)法测定其它杂质元素,被测元素质量浓度在0~10μg/mL范围内与光谱强度呈良好线性关系,相关系数均大于0.9998。测定结果的相对标准偏差小于10%(n=5),加标回收率为97.0%~102.5%。该方法简单、快速,有效地解决了线路板样品不均匀而难采样,以及硬度、韧性强制样难,金属易包裹难分解的技术瓶颈,测定结果准确,具有代表性。该方法适用于废弃线路板化学成分分析,其它废弃电子产品检测可参考此方法。     

有机进样–电感耦合等离子体质谱法测定汽油中锰、铁、铅

建立有机进样-电感耦合等离子体质谱法(ICP-MS)测定汽油中锰、铁、铅含量的分析方法。以乙醇为稀释剂,选择水性无机元素标准溶液为标准物质,采用标准加入法并加入内标校正、补偿基体干扰效应后直接稀释进样分析,用碰撞模式消除多原子离子质谱干扰。锰、铁、铅的含量在0.00~20.00 μg/kg范围内具有良好的线性关系,相关系数均大于0.999,检出限分别为0.20,0.50,0.05 μg/kg。按标准加入法进行回收试验,加标回收率分别为81.9%~95.5%,85.4%~103.1%,97.4%~101.4%,测定结果的相对标准偏差均小于6%(n=6)。该方法快速、准确,灵敏度高,操作简便,试剂用量小,能满足实际汽油样品中微量锰、铁、铅含量的分析要求。     

Determination of trace levels of iron in a seawater sample using isotope dilution/inductively coupled plasma mass spectrometry.

An analytical method for trace levels of iron in a seawater sample using isotope dilution ICP-MS was developed. Preconcentration of iron and the removal of major elements in seawater such as alkali and alkaline-earth elements can be carried out quickly using a chelating resin disk by adjusting the sample pH to 3. The collision cell option of the ICP-MS instrument method was used to improve the performance of the instrument for iron measurements since ArO and ArN interferences could be reduced using this analytical method. About 4 ml min(-1) helium, as the collision gas, were introduced into the cell. 40Ar14N and 40Ar16O which interfere with 54Fe and 56Fe in water had their amounts decreased by 5 orders of magnitude. Then, the isotope dilution method was used for iron determination below ng g(-1) level of trace iron in four environmental reference materials (river water standard sample JAC-0031 (Japan Soc. for Analytical Chemistry), estuarine standard sample SLEW-2 (NRC Canada) and seawater standard samples CASS-3 and NASS-5 (NRC Canada)) were measured. Good agreement between analytical results and certified values of reference materials was obtained, which confirmed the effectiveness of this method.     

Vanadium determination in chloride matrices using ICP-MS: finding the optimum collision/reaction cell parameters for suppressing polyatomic interferences

Efficiencies of He/NH₃ and He/H₂ collision gases were compared in a conventional type of hexapole cell of an inductively coupled plasma mass spectrometer (ICP-MS). The optimum conditions [hexapole and quadrupole bias voltage (V_H and V_Q) and collision/reaction gas flow rates] were tested for vanadium determination (⁵¹V) in chloride matrices. When the He/H₂ mixture was used, the optimum values of V_H and V_Q were −10.0 and −8.0 V, respectively. This set-up corresponds to the kinetic energy discrimination effect. When the He/NH₃ mixture was used, the optimum values of V_H and V_Q were +10.0 and −7.0 V, respectively. Positive V_H values correspond to the ion kinetic energy effect, which allows the reactivity of the ions entering the collision/reaction cell with the reaction gas to be controlled. The obtained results showed that the He/H₂ mixture is not optimal for V determination in samples containing chlorides due to the insufficient suppression of the polyatomic interference of ³⁵Cl¹⁶O⁺. Data obtained from vanadium determination using the He/NH₃ mixture were consistent for all selected Cl⁻ concentrations, and the results were acceptable. The detection limit was comparable with detection limits obtained from ICP-MS equipped with a dynamic reaction cell. Analyses of elements forming interfering molecules, e.g., iron (⁵⁶Fe), arsenic (⁷⁵As) and selenium (⁸⁰Se), were in good agreement with the certified values for both studied collision/reaction gas mixtures.     

蒸馏分离–电感耦合等离子体质谱法测定铜铅锌矿石中微量锗

建立蒸馏分离-电感耦合等离子体质谱法测定铜铅锌矿石中微量锗的方法。采用硝酸-磷酸混合酸消解铜铅锌矿石样品,在盐酸介质中蒸馏分离微量锗,在氦气碰撞池模式下,以103Rh为在线内标进行质谱法测定。锗的质量浓度在0~50 μg/L 范围内线性良好,相关系数为0.9995,方法检出限为0.019 μg/g。用所建方法对3个铜铅锌矿石成分国家一级标准物质进行测定,测定结果的相对标准偏差为4.58%~5.55%(n=7),样品加标回收率为93.0%~102.0%。该方法操作简便,灵敏度高,适用铜铅锌矿石中微量锗含量的测定。     

Elimination of chloride interference on arsenic speciation in ion chromatography inductively coupled mass spectrometry using an octopole collision/reaction system

Anion-exchange chromatography with inductively coupled plasma mass spectrometry (ICP-MS) is often used for the speciation of arsenic (As). In this work, either He or H₂ was introduced to the octopole collision/reaction cell to eliminate chloride (Cl⁻) interferences during As speciation by ICP-MS. Polyatomic species, ⁴⁰Ar³⁵Cl and ³⁸Ar³⁷Cl, which are formed in high chloride matrices interfere with the ICP-MS detection of ⁷⁵As. These interferences were reduced or eliminated by introducing He or H₂ to the collision/reaction cell, with some loss in sensitivity when compared to the standard mode (no gas). For example, the sensitivity of As(V) was 30.4 and 17.7% of that observed in standard mode when introducing He and H₂, respectively. Chloride interference was completely eliminated using a flow rate of 3.0 mL min^− 1 with H₂ as a reaction gas with detection limits in the range of 0.3-0.6 μg L^− 1. The developed method was applied to determination of arsenic species in waters containing high concentrations of chloride by following a simple procedure and without modification of the ICP-MS instrument.     

Arsenic determination by ICP-QMS with octopole collision/reaction cell. Overcome of matrix effects under vented and pressurized cell conditions

The determination of arsenic by inductively coupled plasma mass spectrometry (ICP-MS) in natural waters with high sodium and chloride content has been investigated. The instrument used is equipped with an octopole collision/reaction cell to overcome spectroscopic interferences. Thus, the optimization of collision/reaction gas flow rates is required when using a pressurized cell. A mixture of 2.9 mL min⁻¹ of H₂ and 0.5 mL min⁻¹ of He has been found to be suitable for the removal of ⁴⁰Ar³⁵Cl⁺ interference.The effect of the introduction of small amounts of alcohol has also been studied in this work under both vented and pressurized cell conditions. It has been observed that the presence of 4% (v/v) of ethanol or methanol results in an increase in arsenic sensitivity. Moreover, under vented cell conditions the addition of alcohol also decreases the formation of polyatomic interference. However, this decrease is not observed under pressurized cell conditions.Different elements have been studied as possible internal standards for arsenic determination in presence of high amounts of sodium. Good results have been obtained for rhodium and yttrium under both vented and pressurized cell conditions. Although the presence of alcohol in the sample matrix also affects their behaviour, rhodium and yttrium are still the most suitable elements to correct for these matrix effects.Different experimental conditions have been compared for arsenic determination in spiked, certified and natural waters with high sodium and chloride content. The best results have been obtained under pressurized cell conditions, in the presence of ethanol and using rhodium as internal standard.