石墨炉原子光谱法测定工业废渣中痕量元素砷、铅、铬、钡、银

建立了石墨炉原子吸收光谱法测定检测工业废渣中痕量元素砷、铅、铬、钡、银的方法。采用悬浮进样,硝酸-硫酸混合酸溶解样品。10g/L Mg(NO3)2作基体改进剂,提高了砷的灰化温度,加入10g/L CaCO3防止钡在石墨炉中形成不易挥发的碳化钡,增加了钡的灵敏度。回收率为98%～112%,测定结果的相对标准偏差为2.22%～4.46%。As的线性范围2～80μg/L,Pb的线性范围1～60μg/L,Cr的线性范围0.5～20μg/L,Ba的线性范围5～150μg/L,Ag的线性范围1～100μg/L。     

微波消解-电感耦合等离子体质谱法同时测定垃圾渗滤液中8种生物毒性元素

建立了微波消解–电感耦合等离子体质谱法测定垃圾渗滤液中铜、锌、镍、铬、镉、砷、铅、汞等8种生物毒性元素的含量。以5 mL硝酸及1 mL过氧化氢为消解剂,对垃圾渗滤液样品进行微波消解处理,以45Sc,89Y,115In,209Bi为内标元素消除非质谱干扰,以氦气为碰撞反应气消除质谱干扰,用电感耦合等离子体质谱仪进行定量分析。在1～100μg/L的质量浓度范围内标准工作曲线线性关系良好,相关系数均大于0.999,方法检出限为0.02～0.13μg/L,测定结果的相对标准偏差为1.02%～3.78%(n=6),加标回收率为88.0%～98.8%。该方法检出限低、精密度高,能够满足垃圾渗滤液中上述8种元素的日常分析测定。     

KED-ICP-MS法测定电子级丙二醇甲醚中的银、镉和铅

建立了电感耦合等离子体质谱法(ICP-MS)测定电子级丙二醇甲醚中银(Ag)、镉(Cd)和铅(Pb)含量的方法。样品经超纯水稀释后直接进样,采用标准加入法作为定量方法,选择待测同位素为¹⁰⁷Ag,¹¹¹Cd, ²⁰⁸Pb,并通过选择检测模式和碰撞/反应池气体流量有效消除质谱干扰。结果表明,在碰撞模式下利用动能歧视技术(KED), He流量为4 mL/min时,质谱干扰消除效果最佳。该方法的线性范围为0.2～5μg/L,线性相关系数大于0.9995,各元素检出限(LODs)为0.002～0.009μg/L,加标回收率为93.8%～104.2%,相对标准偏差(RSDs)小于9.5%。使用KED-ICP-MS法可以准确测定电子级丙二醇甲醚中Ag,Cd和Pb的含量。     

ICP-MS法测定镍基单晶高温合金DD416中的镓、锡、锑、铅、铋

建立电感耦合等离子体质谱法测定镍基单晶高温合金DD416中镓、锡、锑、铅、铋元素的含量。以盐酸–硝酸(体积比3∶1)混合酸为消解剂,利用微波消解仪消解样品,以Rh(10μg/L)为内标元素。镓的线性范围为0～50μg/g,锡、锑、铅的线性范围为0～20μg/g,铋的线性范围为0～2μg/g,线性相关系数均大于0.999,检出限分别为0.01,0.2,0.1,0.07,0.006μg/g。用该方法对标准物质进行测定,测定结果与标准值之间的相对误差在7.7%～22.7%范围内。样品加标回收率为98.2%～108.0%,测定结果的相对标准偏差为0.1%～1.5%(n=5)。该方法可以快速、准确地对镍基单晶高温合金DD416中镓、锡、锑、铅、铋元素进行同时测定。     

基于微波消解/电感耦合等离子体质谱法测定土壤中全磷

建立了微波消解/电感耦合等离子体质谱仪(ICP-MS)碰撞池(CCT~(ked))测定土壤中全磷的方法,采用内标法定量。用土壤标准物质验证了方法的准确度与精密度。方法的线性范围为0～2 000μg/L,检出限为5μg/L,土壤样品的检出限为2.5μg/g。土壤基质溶液的加标回收率为94.0%～103%。该方法与钼锑抗分光光度法无显著性差异,具有灵敏度高、简便、快速的特点。     

比较液-质联用法与高效液相色谱法对水中苯胺和联苯胺的同步测定

比较了液-质联用法与高效液相色谱法两种方法同时测定水中苯胺和联苯胺。液-质联用法中,苯胺、联苯胺的检出限分别为0.11μg/L和0.03μg/L,回收率为93.5%～112.2%,相对标准偏差为1.2%～3.2%。高效液相色谱法中,采取直接进样,两种物质检出限为4.6μg/L和2.4μg/L,回收率为104.4%～112.8%;富集后进样,检出限为0.06μg/L和0.01μg/L,回收率为83.5%～94.0%,相对标准偏差均不超过6%。经比较,液-质联用法无需富集即可实现低检出限、高灵敏度,可以作为首选的检测方法。     

电感耦合等离子体质谱法测定包装材料中10种有毒元素

建立电感耦合等离子体质谱法测定包装材料中铬,镍,铜,锌、砷、硒、钼、镉、汞、铅10种有毒元素的方法。以硝酸和过氧化氢为消解试剂,采用微波消解法消解样品,在选定的仪器工作条件下进行测定。汞的质量浓度在1～10μg/L范围内,其它9种元素的质量浓度在1～100μg/L范围内与质谱响应值具有良好的线性关系,相关系数均不小于0.999 7,方法检出限为0.000 3～0.027 6 mg/kg。塑料和纸质包装材料样品中10种元素测定结果的相对标准偏差为1.10%～4.44%(n=7),样品加标回收率为85.17%～106.16%。该方法适用于包装材料中多种元素的同时测定。     

ICP–MS法同时测定儿童洗涤护肤产品中17种有毒有害元素

建立电感耦合等离子体质谱法同时测定儿童洗涤护肤产品中铝、锑、砷、钡、硼、镉、铬、钴、铜、铅、锰、汞、镍、硒、锶、锡和锌17种有毒有害元素的方法。样品采用微波消解法处理,通过在线内标及碰撞反应池技术校正基体效应,并优化了仪器的工作参数。测定锌的线性范围为5~1 000μg/L,砷、镉、铬、汞的线性范围为0.5~100μg/L,其它12种元素的线性范围为1~200μg/L,相关系数均在0.999以上,方法检出限为1.0~25.7μg/kg。加标平均回收率为88.6%~103.2%,测定结果的相对标准偏差均小于5%(n=6)。该方法快速、简便、准确,可应用于儿童洗涤护肤产品中有毒有害元素的测定。     

氢化物发生-原子荧光光谱法测定高纯阴极铜中硒、碲

本文报道了采用氢化物发生-原子荧光光谱法(HG-AFS)测定高纯阴极铜中硒、碲。实验考察了盐酸、三氯化铁的浓度对氢化物发生效率的影响,探讨了铜和其它共存元素的干扰情况。该法测定硒、碲的检出限分别为0.27μg/L、0.11μg/L,加标回收率分别为94.9%～114.0%、91.8%～105.3%,精密度为1.5%～7.8%。     

电感耦合等离子体质谱法同时测定食品包装用聚对苯二甲酸乙二醇酯材料中9种重金属

建立了聚对苯二甲酸乙二醇酯(PET)材料中Li、Mn、Fe、Co、Cu、Zn、Sb、Pa、Pb 9种重金属的电感耦合等离子体质谱(ICP-MS)检测方法。样品加入HNO_3和H_2O_2进行微波消解,内标法定量,各元素均呈现良好的线性关系(Sb:0.1～5.0μg/L;Pb、Co:1.0～50μg/L;Li、Mn、Cu、Zn、Ba:10～500μg/L;Fe:10～500 mg/L),相关系数(R~2)均大于0.9998。方法检出限在0.009～0.147μg/g范围内,样品加标回收率为86.2%～107.1%,精密度(RSD)在2.16%～6.84%之间。所建立的方法操作简便,灵敏度高,可用于食品包装用塑料材料中重金属快速检测。     

ICP-MS混合模式测定植物性农产品中的9种痕量元素

建立了ICP- MS混合模式测定蔬菜、水果、大米等植物性农产品中痕量元素的检测方法.样品经HNO3 + H2O2消解,以74Ge,115In、209Bi作为内标溶液消除基体干扰,动能歧视型碰撞/反应池技术消除质谱干扰的方式测定植物性农产品中As,Hg,Pb,Cd,Cr,Se,Cu,Ni,Zn 9种痕量元素.结果表明:该...     

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10 mL时有机强化剂称样量控制在0.20 g、无机强化剂称样量控制在0.10 g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。     

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.     

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.     

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。     

三重四极杆电感耦合等离子体质谱(ICP-MS)法测定氧化铕中13种稀土杂质元素

稀土杂质元素直接影响高纯单金属稀土材料的整体性能,是高科技领域许多材料的重要组成部分。通过考察最佳的消解酸量、温度、时间、氧气反应气流量、稀释气流量,建立了基于三重四极杆电感耦合等离子体质谱仪(ICP-MS/MS)直接测定氧化铕中13种稀土杂质元素分析方法。该方法采用0.1%基体直接进样,可以很大程度提高前处理分析效率。利用碰撞模式测定氧化铕稀土中的Y、La、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Yb、Lu元素,氧气质量转移模式测定氧化铕中的Tm,两种模式结合可以有效去除多原子干扰,实现氧化铕的稳定测试分析。通过对氧化铕标准物质（GBW02902）直接测定分析,结果表明,在碰撞和氧气质量转移模式下,各元素线性相关系数（r）均大于 0.9999,方法检出限为0.001~0.023 mg/kg,测试精密度优于1.99%,13种元素的测试值都在认定值的不确定度范围之内。该分析方法操作简单,测试稳定,效率高,为实验室进行氧化铕材料中REE杂质的准确测试分析提供思路和借鉴。     

鱼腥草中钛含量分析方法研究

The research of the effects of surfactants on coloring reaction between titanium and phenyl fluorone was developed.A survey of coexisting elements in the houttuynia cordata thunb was carried out by X-ray fluorescence spectrometry,and a series of interference tests and analyses were performed.The interference can be eliminated by processing through high temperature cineration and adding ascorbic acid.A new method of determination of titanium in houttuynia cordata thunb was established by phenyl fluorone spectrophotometry in the presence of Emulsifier OP.The results showed that Beer's law is obeyed within the range of 0～0.32 μg·mL-1 for titanium.The relative standard deviation(RSD) was 1.9%～2.0%,and the recovery was 96.8%～100.6%.The method was applied for determination of titanium in houttuynia cordata thunb with satisfactory results.     

分光光度法测定钨矿中微量钨

提出了一种测定钨矿中微量钨的分光光度法。该法摩尔吸光系数ε为9.6× 1 0 4 L· mol-1· cm-1,相对标准偏差 <2 % ,加标回收率为 95%～ 1 0 4 %。WO3 含量在 0～ 30 μg/50 m L 范围内满足比尔定律     

电感耦合等离子体质谱法检测氧化镓中杂质元素

建立了电感耦合等离子体质谱法(ICP-MS)测定氧化镓中杂质元素的检测方法,采用微波消解技术溶样,以5 ng/mL Rh为内标补偿校正镓基体的抑制效应,采用碰撞室技术(CCT)消除多元素分子离子的干扰.方法的检出限为0.10～1.0 ng/mL,加标回收率在85%～110%之间,RSD为0.6%～7.1%.该方法能满足99.95%～99.995%氧化镓中杂质元素的分析要求.     

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.