微波消解-ICP-AES法测定化妆品中8种有毒元素

采用微波消解-电感耦合等离子体发射光谱法(ICP-AES)对化妆品中Ba、Pb、Cd、Sb、Se、Cr、Hg、As8种有毒元素进行同时测定,通过试验确定了仪器参数和各元素的分析线。8种元素的浓度在0～10mg/L均与响应值呈线性关系,相关系数大于0.9995。8种元素测定结果的相对标准偏差均小于10%(n=3),方法检测限小于0.04mg/kg。样品中各元素的加标回收率为82.1%～108.7%。该方法适用于大批量的化妆品检测。     

ICP-AES法测定进口氧化铝中杂质元素含量

氧化铝样0．2000g在微波助溶下溶于4mL磷酸,定容于100mL,校准用标准溶液中准确加磷酸匹配。用ICP—AES法测定氧化铝中杂质钠、钛、铁、硅、钙、钒、锌,回收率在98．6%～105．0%间。方法满足进口氧化铝的检验要求,7项元素分析结果的RSD（n=11）均小于1.5%。     

微波消解-ICP-AES测定镁合金中10种杂质元素

采用微波消解技术对样品进行处理,确定了试剂的配比,微波消解功率、时间、压力、冷动温度等关键参数,建立了微波消解～电感耦合等离子体原子发射光谱法测定镁合金中10种杂质元素（AI,Mn,Zn,Zr,Nd,Si,Cu,Ni,Fe,Be）的方法。通过试验优化了仪器的工作条件,确定了各元素分析线,对镁基体、共存元素的干扰及消除进行了研究,各元素测定结果的相对标准偏差为0．04％－3．35％（n=8）,加标回收率为95．0％～105．0％。     

微波消解-ICP-AES法测定蒙药通拉嘎-5中的多元素

采用微波消解-ICP-AES法测定了蒙药通拉嘎-5中的Fe、Cu、Cd、Ca、Mg、Mn、Zn、Sr、Co、Ni、Cr 11种金属元素的含量。结果表明,微波消解法具有快速、高效、节约试剂的优点,由于样品在高压密封系统中进行消解,避免了污染,过程易于控制,消解效率高。测定方法的回收率为98.0%~105.5%,RSD为0.6%~2.4%。蒙药通拉嘎-5中含多种金属元素,尤其Ca、Mg、Sr、Fe、Zn的含量较高。     

微波消解-ICP-AES法测定塑料中Pb和Cd

采用微波消解法进行溶样,以ICP-AES法测定塑料中Pb和Cd的含量。Pb、Cd的回收率分别为96.0%~102.0、93.3%~105.0%。Pb、Cd测定结果的相对标准偏差分别为0.567%、1.19%(n=10)。Pb和Cd的检出限分别为0.02、0.005 mg/L。该方法适用于多种塑料中Pb和Cd含量的快速分析。     

微波消解-ICP-AES法测定茶叶中微量元素

在微波消解器中,以ＨＮＯ３－ＨＣｌＯ４分解茶叶,然后用ＩＣＰ－ＡＥＳ法测定样品溶液中的Ｂａ,Ｃａ,Ｃｕ,Ｆｅ,Ｍｎ,Ｐｂ,Ｚｎ,本法简便快速,污染少,回收率为９０．２％￣１０６．３％,相对标准偏差为１．７％￣６．２％。     

微波消解-ICP-AES法同时测定绞股蓝中4种微量元素

采用微波消解法,以HNO3-H2O2对样品进行处理,用电感耦合等离子体发射光谱法(ICP-AES)同时测定了绞股蓝中的铁、锰、铜、锌4种微量元素。结果表明,所测样品中的元素含量按铁、锰、锌、铜顺序递减,各元素测定结果的相对标准偏差在1.0%~3.8%之间,回收率在88%~97%之间。方法简单,有实用意义。     

微波辅助消解ICP-AES法测定小茴香中20种元素

采用微波消解法处理小茴香样品,电感耦合等离子体发射光谱(ICP-AES)测定其中Na、K、Sr、Ca、Mg、P、As、Zn、Pb、Co、Cd、Ni、Ba、Fe、Mn、Cr、Cu、Al、Ti和B 20种常量和微量元素的含量。20种元素的检出限为0.00002~0.00468μg·mL-1,回收率为89.50%~107.89%,相对标准偏差(RSD)均小6%。结果显示,小茴香果实及其嫩叶中除含有人体必需的常量元素K,Na,Ca,Mg,P外,还含有Fe、Zn、Mn、Cr、Co等必需的微量元素和其他元素Ti、B、Ni、Al、Sr、Ba等。     

微波消解-ICP-AES法测定回汉族人群血清中的微量元素

本文测定了宁夏农村地区回汉族人群血清中Li、Co、Cd、Ga、Ba、Sr、Cu、Zn、Fe、Al、Se、Sn、B、Mn、Cr、Ni、Pb、Ca、K、Mg、Na、P、S的含量。采用微波消解对样品进行了前处理,使用电感耦合等离子体原子发射光谱法(ICP-AES)进行测定。该方法的RSD≤3.5%,样品加标回收率为90%~117%。该法简便、快速、灵敏、准确,可用于血清中多种元素含量的同时测定。研究结果表明,K、Fe、Cu、Mn、Ni、Ga、Al、Se、Pb、S、Cd、Cr、Sr、Ca这14种元素含量在回族和汉族之间存在着显著性差异(P0.05),探讨了产生上述差异的原因。     

微波消解ICP-AES法测定玩具塑料中镉

采用微波加压消解溶样，ICP-AES法测定玩具塑料中镉含量，选择最佳工作条件，方法简便、快速、可靠。适用于各类玩具塑料中镉含量的分析。     

电感耦合等离子体原子发射光谱（ICP-AES）法测定铁矿石中钒

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定铁矿石中钒含量的分析方法。采用盐酸、硝酸、氢氟酸、高氯酸分解试样,不溶物残渣碱熔融回收,稀盐酸溶解盐类的方式对样品进行分解。对仪器的主要工作参数和分析谱线进行了选择,讨论了基体和共存元素的干扰,以及溶解酸和熔剂等条件实验,确立了最佳分析条件。按实验方法对铁矿石标准样品和试样中钒量进行测定,测定值与标准值或其它方法的认定值基本一致,相对标准偏差RSD<6.5%。     

微波消解—电感耦合等离子体原子发射光谱法测定天然微晶石墨中铝铁钙镁钠钛钾

针对传统微波消解法存在的消解温度过高、样品消解不完全等问题,实验在常规微波消解温度下,从提高体系的氧化性入手,对消解方法进行改进。探讨了消解体系、消解温度、升温时间,并对消解机理进行了分析。结果表明,以2mL硝酸—5mL硫酸—1 mL高氯酸—1 mL氢氟酸为消解体系、升温时间为25 min、消解温度为200 ℃时,能实现样品的完全消解。消解后的溶液经赶酸处理,盐类析出,为了使盐类复溶,比较了硝酸、盐酸、王水的复溶效果,选定盐酸为复溶酸。对分析谱线进行了优化,确定的各成分分析谱线为铝308.2 nm、铁259.9{129} nm、钙317.933 nm、镁280.2 nm、钠589.5 nm、钛336.1 nm、钾766.4 nm。基于以上研究,建立了微波消解—电感耦合等离子体发射光谱法测定微晶石墨中铝铁钙镁钠钛钾的分析方法。结果表明,标准曲线的线性良好,相关系数不小于0.9994,方法检出限在0.00003%～0.0007%之间。用标准物质GBW03120验证了方法的正确度,结果满意。将方法应用于实际样品分析,测定结果的相对标准偏差（n=8）为0.72%～3.5%,加标回收率在98.2%～104.1%之间,均满足GB/T 27417—2017的要求。建立的方法能在常规微波消解温度下完全消解样品,适用于微晶石墨中主量金属元素的测定。     

电感耦合等离子体原子发射光谱测定钒钛高炉渣中钪镓铬镍钴

建立电感耦合等离子体原子发射光谱法(ICP-AES)同时测定钒钛高炉渣中0005%～0.3%的贵金属元素钪、镓、钴和0.0005%～0.6%铬、镍的检测方法。样品前处理方法采用氢氟酸、盐酸、硝酸和硫酸消解钒钛高炉渣,高温加热至硫酸分解产生三氧化硫浓白烟为此,直接以水稀释定容制备样品溶液,不仅快速完全消解高钛基样品,而且通过挥发除去高含量二氧化硅基体和反应残余的氢氟酸,减少溶液共存组分有效降低基体效应影响以及避免腐蚀检测仪器;而且依靠残余硫酸根与高钛基体络合生成硫酸氧钛离子,解决了高浓度钛基体在低酸度介质中易水解问题,无需补充加入大剂量酸以限制钛水解,直接以水稀释制备样品溶液,从而降低溶液酸度减少酸度效应影响。方法重点试验考察了钒钛高炉渣中钒钛铁钙镁铝等共存介质下基体效应、光谱干扰等干扰影响因素,优选了元素的分析谱线、背景校正区域以及光谱仪工作参数等检测条件,采用基体匹配和同步背景校正法消除基体效应影响。验证表明方法的技术性能指标：校准曲线相关系数>0.999,背景等效浓度0.0001%～0.0002%,元素检出限0.0001%～0.0002%,检测范围内RSD＜15%,回收率90%～114%     

微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定含铜污泥中多种重金属

为了填补现有方法的技术空白,本方法采用微波消解和电感耦合等离子体原子发射光谱法（ ICP-AES）相结合,实现对含铜污泥中铅、锌、铬、镉、砷、镁、铝、锑量的同时测定。首先采用盐酸-硝酸-氢氟酸微波消解进行样品的前处理,消解后加入高氯酸置于电热板进行除碳并赶酸,溶样效果理想,且有效避免了高温溶样对易挥发元素砷、锑的损失,整个过程安全、高效、无损。溶样后以电感耦合等离子体发射光谱法（ ICP-AES）进行测定。对含铜污泥的分解方法进行了合理选择,并对测定时的元素分析谱线及各测定元素间干扰情况等进行了讨论。该方法的加标回收率在95.31%~107.28%%,相对标准偏差（RSD）在0.31%~2.05%之间（n=7),结果表明,该方法准确度高,操作简单快捷,可同时测定多种元素,能满足批量的测定含铜污泥中铅、锌、镍、铁、镉、铬、砷、锑含量的测定要求。     

电感耦合等离子体发射光谱法测定高效复合孕育剂中铝、钙、钡

通过硝酸、氢氟酸和盐酸分解试料,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,应用电感耦合等离子体发射光谱(ICP-AES)法对高效复合孕育剂中铝、钙、钡进行测定,此方法能准确、快速地测定其含量,回收率在98%～103%之间,精密度、标准样品分析对照均取得了满意的结果。     

Determination of titanium and vanadium in Ziegler-Natta catalysts by inductively coupled plasma atomic emission spectrometry.

A method for the determination of Ti and V using inductively coupled plasma atomic emission spectrometry (ICP OES) in Ziegler-Natta polymerization catalysts is proposed. The concentrations of both Ti and V are efficiently determined after catalyst acid digestion with a mixture of HNO3 + HCl + HF and heating (160 degrees C for 6 h) or with 10% (v/v) H2SO4 and heating (160 degrees C for 6 h) or with 10% (v/v) H2SO4 and sonication (during 2 min). The V and Ti detection limits are 0.002% and 0.08%, respectively, using 0.20 g of catalyst sample in 50 ml. The method is validated by a comparison with the Rutherford backscattering spectrometry (RBS) technique. In this case, catalyst samples are only pressed as pellets before analyte determination. Despite the fact that both the V and Ti concentrations cannot be determined individually by means of RBS, because the atomic numbers of Ti and V are very close, the sum of the V and Ti contents is in accordance with that attained by means of ICP OES. According to scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX) it is observed that the Ti distribution on the catalyst grain is not homogenous.     

Determination of iron, copper and zinc in tinned mussels by inductively coupled plasma atomic emission spectrometry (ICP-AES)

Summary An optimisation of the ICP-AES determination of Fe, Cu and Zn in tinned mussels has been carried out. The optimum conditions for the radio frequency power, peristaltic pump flow, plasma gas flow, nebuliser gas pressure, auxiliary gas flow and observation height above load coil were determined manually for each element, since the Simplex method was less adequate. Scans were carried out with the aim of finding the most sensitive spectral lines, whose intensity did not always coincide with literature data. Limits of detection, linearity, precision, and accuracy were also investigated. The possible spectral interferences due to Na, K, Ca, Mg, P, I and nitric acid were studied from three different points of view and the results did not agree. The influence of the matrix on the determination of the above elements in tinned food from the Galician Rias (in the south coast of Galicia) was also studied. The results obtained were comparable to those obtained by AAS.     

微波消解-ICP-AES 法测定乌梅中铁、锰、铜、锌

四川野生乌梅是药食兼优食物,在中医药方面已广泛应用,但作为保健食品的资源利用还有待进一步开发。乌梅中的微量元系含量与其药效及营养保健作用有关。本文应用微波消解-ICP-AES法同时测定了乌梅中Fe、Mn、Cu、Zn,选择了最佳测定条件,并探讨了乌梅中所含4种人体必需微量元素的药理功能。     

Determination of calcium, copper, iron, magnesium, manganese, potassium, phosphorus, sodium, and zinc in fortified food products by microwave digestion and inductively coupled plasma-optical emission spectrometry: single-laboratory validation and ring trial

A single-laboratory validation (SLV) and a ring trial (RT) were undertaken to determine nine nutritional elements in food products by inductively coupled plasma-optical emission spectrometry in order to modernize AOAC Official Method 984.27. The improvements involved extension of the scope to all food matrixes (including infant formula), optimized microwave digestion, selected analytical lines, internal standardization, and ion buffering. Simultaneous determination of nine elements (calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc) was made in food products. Sample digestion was performed through wet digestion of food samples by microwave technology with either closed- or open-vessel systems. Validation was performed to characterize the method for selectivity, sensitivity, linearity, accuracy, precision, recovery, ruggedness, and uncertainty. The robustness and efficiency of this method was proven through a successful RT using experienced independent food industry laboratories. Performance characteristics are reported for 13 certified and in-house reference materials, populating the AOAC triangle food sectors, which fulfilled AOAC criteria and recommendations for accuracy (trueness, recovery, and z-scores) and precision (repeatability and reproducibility RSD, and HorRat values) regarding SLVs and RTs. This multielemental method is cost-efficient, time-saving, accurate, and fit-for-purpose according to ISO 17025 Norm and AOAC acceptability criteria, and is proposed as an extended updated version of AOAC Official Method 984.27 for fortified food products, including infant formula.     

电感耦合等离子体发射光谱法测定铜阳极泥中的金含量

实验采用某铜冶炼生产企业的铜阳极泥样品,对其中的金含量进行测试。用王水溶解样品,在3%王水酸度下,定容至100mL容量瓶,用电感耦合等离子体发射光谱法测定。经试验研究,选择242.795nm为分析谱线,方法检出限为(n=11)0.09μg/mL,测定下限为0.27μg/mL,加标回收率在97%-107%之间,线性相关系数为：0.999928,分析结果满足要求。