ICP-AES法同时测定化妆品中汞砷铅

采用高压溶样弹,将样品用于硝酸－过氧化氢或高氯酸－过氧化氢溶解后,用ＩＣＰ－ＡＥＳ法对汞砷铅连续测定。方法回收率分别为８６．０％、９６．２％、９９．８％,ＲＳＤ分别为３．１７％、２．５１％、２．０１％。与原子吸收汉比较,无显著差异。应用于市售化妆品检测,结果满意。     

比光谱导数-零交点法同时测定铜、锌、镍

在ｐＨ＝８的硼砂－ＨＣｌ缓冲溶液中，以乳化剂ＯＰ作增溶剂，Ｃｕ＾２＋，Ｚｎ６２＋，Ｎｉ＾２＋分别与５－Ｂｒ－ＰＡＤＡＰ形成稳定的配合物，用比光谱导数－零交点法同时测定铜，锌，镍，合成试样６次测定的相对标准偏差小于５％，铜，锌，镍的回收率分别为９７．０％－１０３．２％，９６．３５－１０４．８％和９５．２％－１０１．９％。     

动力学—两次标准加入法同时测定钼和钨

本文提出了动力学－两次标准加入法双组份同时测定的新方法，讨论了测定的基本原理；用停流ＦＩＡ光度法研究了钼和钨共同催化的Ｈ２Ｏ２－Ｉ＾－动力学反应体系，并建立了钼和钨同时测定的条件，用本法测定了钢样和模拟样品中的钼、钨含量，结果满意，钼和钨的回收率分别为９７％－１０２．６％和９８．２％－１０３％；相对标准偏差分别为２．８％－３．２％和２．１％－３．５％。     

一阶紫外导数光谱PLS法直接同时测定硝酸根和亚硝酸根

用偏最小二乘（ＰＬＳ）法解析了ＮＯ_３~－和ＮＯ_２~－混合体系的一阶紫外导数光谱，提出了直接同时测定环境水样中ＮＯ_３~－－Ｎ和ＮＯ_２~－－Ｎ的计算分析法。该法对ＮＯ_３~－和ＮＯ_２~－来说，最低检测浓度分别为９×１０~（－８）和２×１０~（－７）ｍｏｌ·Ｌ~（－１），精密度（ＲＳＤ）分别为２．０５％和２．１２％。用于测定合成水样，平均相对误差在４％以内；用于测定环境水样，结果与标准法相吻合。     

病人血样中痕量锗,锶的石墨炉原子吸收光谱法测定

本文运用石墨炉ＡＡＳ法加基体改进技术，测定了５０岁以上病人血清及环境水样中锗和锶的含量。用０．０１ｍｏｌ／ＬＨＮＯ３－０．１％ＴｒｉｔｏｎＸ－１００稀释血清，测定精度可与火焰法媲美。锗，锶的特征量分别为２８ｐｇ和１８ｐｇ；线性范围为０－２５０ｎｇ／ｍＬ和－３５．０ｎｇ／ｍＬ；相对标准偏差（ｎ＝１０）４．１０％和２．４９％；回收率分别为９２．２％－９９．０％和９２．０％１０２％。方法快速准确，结果满     

高效液相色谱法测定抗氧剂264和对甲酚

用反相高效液相色谱法分离和测定了抗氧剂２６４和对甲酚，其线性范围分别是１．２×１０－９～２．８×１０－８ｍｏｌ和１．８×１０－９～２．４×１０－６ｍｏｌ，相对标准偏差分别为１．７％和０．９８％。     

苯酚在Ln—ZrO2催化剂上直接氧化制取邻苯二酚地研究

以Ｌｎ－ＺｒＯ２作为苯酚选择氧化催化剂，用过氧化氢氧化，得到邻苯二酚选择性高达８５．７％的良好结果，添加稀土元素镧，钕的氧化锆催化剂的单纯的二氧化钛催化剂相比，邻苯二酚选择性分别提高了７３．５％和６７．８％。     

高压消解-火焰原子吸收光谱法测定大米中痕量铅铬镉镍和钴

采用高压溶样弹，将样品用硝酸－过氧化氢溶解后，用FAAS法对大米中铅、铬、镉、镍和钴测定，回收率为96％－103％，RSD分别为2.7%、3.1%、4.3%、3.9%和1.8%。应用于出口大米检测，取得满意的结果。     

半微分阴极溶出伏安法研究硫离子在银电极上的电化学行为

用半微分阴极溶出伏安法研究硫离子在银电极上的电化学行为。在ＮａＯＨ－ＥＤＴＡ－Ｎａ２ＳＯ３底液中，可消除溶解氧及部分重金属离子Ｃｕ２＋，Ｐｂ２＋，Ｚｎ２＋，Ｃｄ２＋和Ｎｉ２＋的干扰。一些阴离子Ｃｌ－，Ｉ－，ＮＯ－３和ＳＯ２－４不干扰。硫离子浓度在３．１９×１０－６ｍｏｌ／Ｌ至３．１３×１０－５ｍｏｌ／Ｌ范围内与溶出峰高成线性关系。对两种人发样品中硫含量测定的回收率分别为９３．９％和９７．８％。     

比值光谱导数法同时测定铝合金中铁,铜,锌

用比值光谱－导数分光光度法，在ｐＨ５．５缓冲溶液中，利用金属－２－（５－溴－２－吡啶偶氮）－５－二乙氨基酚（５－Ｂｒ－ＰＡＤＡＰ）－ＯＰ三元络合物显色体系，对混合物中铁，铜，锌三组分进行了同时测定。合成试样５次测定回收率在９７．３％－１０４．４％之间。应用于铝合金中铁，铜，锌的测定，各６次测定的ＲＳＤ分别为３．６６％，１．３８％，２．０３％。     

ICP-AES 法测定金属镝与氧化镝中 Mn、Ca、La 等15个元素

采用等离子光谱法测定了镝金属中的Mn、Ca、La等15个元素。利用正交试验L9（3^4）优化了仪器操作条件。方法回收率在93.6％－108％之间,相对标准偏差小于6.5%。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定无定形硼粉中的镁

提出了使用电感耦合等离子体原子发射光谱法(ICP-AES)测定Mg元素的方法。采用硝酸、盐酸溶解样品,用硝酸和盐酸的混合酸作为测定介质,在选定的仪器条件下直接测定Mg元素的检出限为0.0044μg/mL,相对标准偏差RSD(n=6)为0.49%～0.60%,样品加标回收率在94.0%～102.0%之间。经对比试验证明,电感耦合等离子体原子发射光谱法(ICP-AES)测定无定形硼粉中Mg的测定值与美国军用标准重量法测定值一致。     

Combined use of atomic spectrometric methods in the analysis of rocks

Standard reference materials of limestone, granite and argillite were analyzed by X-ray fluorescence spectrometry (XFS), flame and graphite furnace atomic absorption spectrometry (F-AAS and G-AAS), and inductively coupled plasma atomic emission spectrometry (ICP-AES). The major elements Al, Ca, Fe, Si and Ti were determined by XFS and ICP-AES. The relative standard deviations (RSD) of the concentrations of the corresponding oxides obtained by XFS and ICP-AES were (1.36±0.51)% (n=18) and (1.30±0.70)% (n=17), respectively, on the average. The relative deviations (RD) from the certified values were (1.29±3.01)% (n=18) and (–0.69±5.48)% (n=14), respectively, on the average. The numbers in parentheses are the numbers of the single RSD- and RD-values used for the calculation of the averages and the relative standard deviations. Some minor and trace elements of the standard reference materials were determined by G-AAS and ICP-AES. The precision (RSD) was markedly better in the case of ICP-AES. On the other hand, the accuracy (RD) of both methods was about the same (7%). Apparently, the precision and the accuracy are primarily determined by the measuring technique and the sample pretreatment procedure, respectively. The analytical power of the combined use of atomic spectrometric methods is also discussed.     

Determination of cadmium in polyethylene by analytical atomic spectrometry with gas-phase sample introduction technique

Cadmium in polyethylene was determined by both inductively coupled plasma atomic emission spectrometry (ICP-AES) and atomic absorption spectrometry (AAS) with continuous-flow gas-phase sample introduction in a reaction medium of ascorbic acid. In the presence of mixture of cobalt and thiourea in the ascorbic acid solution, the sensitivities by both ICP-AES and AAS for cadmium were greatly enhanced. The gaseous cadmium species was phase-separated in a gas–liquid separator and directed via a stream of argon carrier gas to an inductively coupled plasma and an electrically heated quartz tube atomizer (QTA) for atomic spectrometry. Under the optimized experimental conditions, the best attainable detection limits at Cd I 228.802 nm line were 1.3 and 0.017 ng/ml with linear dynamic ranges of 10–500 ng/ml and 0.1–1 ng/ml in concentrations by ICP-AES and QTA-AAS, respectively. The instrumental precisions expressed as the relative standard deviation (R.S.D.) from ten replicate measurements of 50 and 1 ng/ml cadmium by ICP-AES and QTA-AAS were 5.6% and 3.2%, respectively. With the use of ICP-AES and QTA-AAS with gas-phase sample introduction method, six- and 200-fold improvements in detection limits for cadmium were obtained in comparison with their conventional solution nebulization methods, respectively. After the effects of several diverse elements on the determination of cadmium by ICP-AES and QTA-AAS with the present gas-phase sample introduction systems were examined, these methods were applied to the determination of low concentrations of cadmium in polyethylene. The results obtained by the present method were in good agreement with the certified values.     

电感耦合等离子体发射光谱法测定锌精矿中的铟

应用电感耦合等离子体发射光谱法测定锌精矿中的铟,确定了最佳工作条件,选择了最佳分析谱线,并利用标准加入法和基体匹配法验证了方法的准确性。样品用氟化氢铵、盐酸、硝酸、高氯酸溶样,用盐酸定容。结果表明,电感耦合等离子体发射光谱法与萃取分离盐酸羟胺示波极谱法测定的铟含量结果一致。方法准确,快速,加标回收率为99.6%～101.7%,相对标准偏差为0.97%～2.1%。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷的含量

通过样品处理、干扰实验、方法检出限、准确度和精密度实验,确定了最佳实验条件,建立了电感耦合等离子体-原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷含量的方法。试料经盐酸、硝酸、氢氟酸、高氯酸分解,用盐酸溶解盐类,过滤,采用电感耦合等离子体原子发射光谱法同时测定滤液中铜、锰、铝、钙、镁、钛和磷的含量。方法检出限为锰、钛和磷小于0.00085%,其它元素小于0.0054%,分析结果与分光光度法、X射线荧光光谱法(XRF)和原子吸收光谱法(AAS)分析结果一致,8个实验室对5个水平样品进行协同实验给出了方法的精密度。     

Spectrophotometric and inductively coupled plasma atomic emission spectrometric determination of titanium in ilmenites after rapid dissolution with phosphoric acid

The use of 85% phosphoric acid in borosilicate conical flasks for the dissolution of ilmenites at 230 +/- 10 degrees C is reported. The samples were quantitatively dissolved in less than 13 min. Titanium was determined by both spectrophotometry and inductively coupled plasma atomic emission spectrometry ICP-AES. Vanadium and iron were determined by ICP-AES. In several samples of ilmenites analyzed, the TiO(2) concentration was in the range 10.6-57.5% and those of FeO and V(2)O(5) were in the ranges 31.6-51.4% and 0.39-1.32%, respectively. In the spectrophotometric method, vanadium interference occurs only when the Ti V concentration ratio is <4. In all samples analyzed this ratio was around 12, resulting in no interferences due to vanadium. Hence the ilmenite dissolution procedure using phosphoric acid was compatible with titanium quantification by both spectrophotometry and ICP-AES.     

K金饰品中金含量的检测方法比对

目前实验室对金首饰金含量的主要检测方法为火试金法、X射线荧光光谱（XRF）法和电感耦合等离子体-原子发射光谱（ICP-AES）法.当测试结果出现争议时,国家标准GB 11887-2012中以火试金法作为仲裁方法.采用上述3种不同的金含量测试方法分别对14K、18K和22K饰品的金含量进行测定,并对3种方法检测结果进行比对.结果发现,在3种方法均可满足样品分析对准确度的要求时,以火试金法为基准,XRF法与ICP-AES法对同纯度的金首饰检测结果的相对误差差异较大,XRF法的结果可满足检测要求,而ICP-AES法的结果无法满足检测要求.其中,XRF法的相对误差为0.05%~0.77%,ICP-AES法的相对误差为1.24%~3.89%.从结果来看,低纯度的K金饰品使用XRF法的检测结果要更接近于火试金法.     

电感耦合等离子体原子发射光谱法间接测定盐酸苯海索

研究了等离子发射光谱法间接测定片剂中盐酸苯海索含量的方法。详细讨论了ICP AES测定硼的“记忆效应”及最佳测定条件。实验表明在pH 2 .0～ 6 .0范围内 ,当四苯硼钠过量时可完全沉淀盐酸苯海索 ,硝酸铝可以使沉淀迅速絮凝而易于过滤 ,测定滤液中的四苯硼钠可以计算得到盐酸苯海索的含量。该法简单快速 ,相对标准偏差为 2 1%。实验测得盐酸苯海索 四苯硼沉淀的溶度积Ksp在 2 0℃时为8 84× 10 -12     

Speciation of Se,Fe and Zn in Human Milk Whey: The use of Instrumental Neutron Activation Analysis (INAA) to corroborate element profiles measured with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

In human milk trace elements normally exist in a form which can easily be absorbed by the newborn infant. For investigations of the bioavailability of trace elements it is necessary to carry out a speciation analysis of the elements of interest. An independent analytical method has been used for the quality control of the shape of the element profiles obtained from the speciation analysis of Se, Fe and Zn in individual samples of human milk whey after chromatographic separation. For the element detection in the untreated milk fractions Instrumental Neutron Activation Analysis (INAA) was chosen as the reference method. Element distribution patterns have been obtained with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) using on-line digestion of the fraction, reduction and hydride formation of Se ("T"-mode). Prior results are compared with those obtained by means of element detection in the untreated fractions ("U"-mode) with ICP-AES. The elution profiles of Se, Fe and Zn in human milk whey obtained by means of ICP-AES detection using the "T"-mode show good agreement with the distribution patterns obtained with INAA. Recoveries of 103% for Fe, 86% for Zn and 87% for Se were obtained. The element distribution patterns of Fe and Zn obtained with ICP-AES speciation using the "T"-mode also show good agreement with those obtained by means of ICP-AES using the "U"-mode.