电感耦合等离子体原子发射光谱法和电感耦合等离子体质谱法测定不同肥料产品中铊含量比对

铊是一种高毒性的微量元素,具有较强的富集能力,已被列为肥料的强制性检验项目。选择了水溶性肥料、复混肥料、有机肥料3种代表性的肥料样品,通过比对微波消解和电热板敞口消解前处理方式;分析电感耦合等离子体原子发射光谱(ICP-AES)法和电感耦合等离子体质谱(ICP-MS)法主要干扰来源;通过建立各自的标准工作曲线、比对方法检出限、精密度、加标回收率,探讨研究肥料产品中铊含量测定方法。研究结果表明：微波消解法和电热板敞口消解法各有优点,可以根据样品实际情况灵活选择。ICP-AES法主要干扰为光谱干扰,需要在前处理过程中除去Mn元素,而ICP-MS法主要干扰为基体效应,可以使用内标物加以校正。ICP-MS法的检出限低于ICP-AES法。由于微波消解-ICP-AES法无法除去消解液中的Mn元素带来的光谱干扰,因此不适合测定铊含量。而微波消解-ICP-MS法、电热板敞口消解-ICP-AES法和电热板敞口消解-ICP-MS法这三种方法测定结果无明显差异,测定标准化肥质控样品均在指定值范围内,加标回收率为86%-110%。实验室可以根据肥料样品的数量、组成、性质合理选择搭配前处理方式和测定方法。     

标准溶液配制用碳酸锂纯物质中杂质含量的测定

从高纯碳酸锂中杂质含量测定出发,研讨了标准溶液配制用原料的杂质测定方法,首先利用电感耦合等离子体质谱(ICP-MS)法对高纯碳酸锂进行半定量分析,再依据半定量分析结果选择ICP-MS、电感耦合等离子体原子发射光谱(ICP-AES)法、原子吸收光谱(AAS)法等方法对相应元素(杂质含量0.001%)进行定量分析,通过扣除杂质含量得出高纯碳酸锂纯度大于99.991%。从而建立了一个准确、高效,覆盖元素种类多的高纯物质中杂质含量的分析方法     

微波等离子体炬原子发射全谱仪测定粮食中微量金属元素

大米和面粉主要成分为碳水化合物，同时还含有Ca、Cu、Fe、Mg及Mn等人体必需的微量元素。大米和小麦中微量元素的测定主要有原子吸收法、ICP-AES及ICP-MS等方法。原子吸收法虽然灵敏度高，但一次只能测一种元素。ICP-AES及ICP-MS法均可同时测定多种元素，灵敏度高，线性范围宽，但仪器设备昂贵，运转费用高。本实验采用流动注射-微波等离子体炬原子发射(FI-MPT-AES)在线标准加入法同时测定粮食中的Ca、Cu、Fe、Mg及Mn等金属元素。该法操作简单方便，成本及运转费用低，快速并可同时得到检测波长范围内的全部光谱信息。     

电感耦合等离子体原子发射光谱法及电感耦合等离子体质谱法在二次资源分析中的应用进展

综述了2005-2012年间国内利用电感耦合等离子体原子发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)测定二次资源中有关元素、特别是重金属元素的分析的最新进展,从样品前处理方法、仪器测定条件优化、技术联用等方面阐述了上述两种方法在二次资源重金属分析中的应用(引用文献40篇)。     

电感耦合等离子体原子发射光谱法测定自来水中的8种元素

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了化学实验室自来水中铝、钾、锶、钡、锰、钴、钼、硒8种元素的含量;对仪器的工作条件进行了优化,确定了各元素的分析波长和检出限.结果表明,所述方法可以方便地用于测定化学实验室自来水样品中的8种元素,相对标准偏差为0.08%～6.90%.     

401螯合树脂富集-ICP-AES法测定近岸海水中微量金属元素

海水中微量元素含量甚低,电感耦合等离子体原子发射光谱(ICP-AES)法不能直接测定,通常需进行预分离和富集。富集方法有螯合溶剂萃取法、共沉淀法、离子交换法。近年来螯合树脂是分离碱金属、富集重金属元素的有效手段之一,广泛用于测定海水中重金属离子。ICP-AES法在多元素的联合测定方面具有比较突出的优点——检出限很低,测定范围可跨越3—4个数量级,同时测定试样中的主、次成分和痕量元素;具有良好的准确度和精密度。本工作采用D401型螯合树脂富集-ICP-AES法测定近岸海水中Co、Cu、Fe、Ni、Zn和Pb。     

ICP-AES法测定太阳能级硅中磷等12种痕量杂质元素

用电感耦合等离子体原子发射光谱仪(ICP-AES)测定太阳能级硅(SOG-Si)中磷等12种杂质元素。实验发现,在150℃时,用HF和HNO3的混合溶液,试样在PFA烧杯中能较快溶解。在1000级洁净室中,用金属氧化物半导体(MOS)级试剂溶解电子级硅(EG-Si,纯度大于9N)可控制样品空白中各元素的含量均小于1μg/L,并能较好的补偿基体效应。在选定仪器工作条件下,被测元素检出限为5~50 ng/mL,回收率在93%~105%,相对标准偏差RSD≤9.8%(n=11)。测定结果与电感耦合等离子体原子发射质谱(ICP-MS)法及辉光放电质谱(GDMS)法进行了比对,结果吻合。     

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。     

电感耦合等离子体原子发射光谱(ICP-AES)法和电感耦合等离子体质谱(ICP-MS)法测定大气降尘中的铅、镉、铬、锌、锰、镍、铜、铊

大气中Pb、Cd、Cr、Mn、Ni、Tl等重金属污染物是目前国内外城市大气污染的主要因子之一,研究大气降尘中重金属元素含量具有重大意义。本文采用盐酸-硝酸混合酸为消解体系,在105℃条件下用电热板消解回流大气降尘样品2小时后定容测定,通过电感耦合等离子发射光谱法仪(ICP-AES)和电感耦合等离子体质谱仪(ICP-MS)测定大气降尘中铅、镉、铬、锌、锰、镍、铜和铊等8种重金属元素。测定结果表明： ICP-AES(铅、镉、铬、锌、锰、镍、铜)和ICP-MS(铊)两种方法的曲线线性好,准确度高,测定范围宽,检出限在0.024mg/kg-0.548mg/kg之间,精密度在0.15%-2.38%之间,能准确测定大气降尘中的重金属元素含量。     

高温消解-电感耦合等离子体质谱法测定铜精矿中铅、砷、汞、镉、铬的含量

<正>中国自产铜精矿不能满足冶炼的需求,每年需要进口大量铜精矿^[1]。为保护环境和保障人民健康安全,我国对进口铜精矿中有害元素铅、砷、汞、镉、铬的含量进行了严格限定^[2]。如何快速、高效测定铜精矿中的有害元素含量已引起越来越多学者的关注^[3-7]。目前,测定铜精矿中铅、砷、汞、镉、铬含量的方法包括冷原子吸收光谱法、原子荧光光谱法、电感耦合等离子体原子发射光谱法(ICP-AES)、电感耦合等离子体质谱法(ICP-MS)等^[8-11]。其中,ICP-MS因具有检出限低、线性范围宽、可以同时测定多种元素等特点而被广泛应用于食品^[12]、矿产品^[13]、环境监测^[14]等领域。铜精矿样品的常用溶解方法有微波消解、电热板加热消解、石墨消解、高温消解等。本工作采用高温环绕式加热消解铜精矿,以ICP-MS同时测定铜精矿中铅、砷、汞、镉、铬的含量,并采用有证标准物质和加标回收的方法验证方法的准确度。     

White analytical chemistry-driven stability-indicating concomitant chromatographic estimation of thiocolchicoside and aceclofenac using response surface analysis and red,green, and blue model

White analytical chemistry is a novel concept for the assessment of analytical methods on basis of its validation efficiency, greenness power, and economical efficiency. White analytical chemistry-driven stability indicating chromatographic method has been developed for the concomitant analysis of thiocolchicoside and aceclofenac. The proposed chromatographic method has been developed using a safe and environmental-friendly organic solvents for the concomitant stability study of thiocolchicoside and aceclofenac. The analytical risk assessment was carried out for the identification of high-risk analytical risk factors and analytical method performance attributes. The mixture design was applied for the design of experiments-based response surface modeling of high-risk analytical risk factors and analytical method performance attributes. The degradation products were isolated and characterized using infrared, nuclear magnetic resonance, and mass spectral data. The proposed method was compared for its validation efficiency, greenness power, and cost-efficiency with published chromatographic methods using the red, green, and blue models. The white score of the proposed and reported method was calculated by averaging the red, green, and blue scores of the methods. The proposed method was found to be robust, green, and economical for the concomitant stability study of thiocolchicoside and aceclofenac.     

X射线荧光光谱法快速测定FeSiB非晶薄带中Si,B,Fe的含量合金薄带中硅硼铁

提出了以自制的标准样品,采用单点法绘制校准曲线,利用X射线荧光光谱仪测定FeSiB非晶薄带样品中硅、硼和铁的含量。对于4个FeSiB非晶合金薄带样品中硅、硼和铁进行了10次测定,其分析结果的相对标准偏差分别为0.4~0.5%,1.3~4.2%和0.2~0.4%。本方法的分析结果与火花源原子发射光谱法、化学重量法和ICP-AES的测定值吻合较好。本方法快速、简便,薄带样品无需制样,适用于FeSiB非晶合金薄带的快速成分分析。     

Stability-indicating capillary electrophoresis method for the simultaneous determination of metformin hydrochloride,saxagliptin hydrochloride,and dapagliflozin in pharmaceutical tablets

A capillary electrophoretic method coupled to a diode array detector (CE-DAD) was developed and validated for the simultaneous determination of metformin hydrochloride (MET), the dipeptidyl peptidase-4 (DPP-4) inhibitor saxagliptin hydrochloride (SAX), and the sodium glucose co-transporter (SGLT 2) inhibitor dapagliflozin (DAP). The proposed method was used for the determination of these drugs in binary antidiabetic combinations namely, SAX/MET, combination I, DAP/MET, combination II, and SAX/DAP, combination III. CE separation was performed on a fused silica capillary with background electrolyte consisting of 30?mM phosphate buffer (pH 6.0) with a high voltage of 30?kV, a pressure of 20 mbar, and an injection time of 40?s. The compounds were detected at 203?nm for SAX/DAP and 250?nm for MET. The method was linear in the concentration range of 10–200?µ?g/mL (SAX), 1.25–50?µ?g/mL (DAP), and 7.5–1000?µ?g/mL (MET). Full validation of the proposed method was performed as per the ICH guidelines. The obtained errors and deviation values did not exceed 2% assessing good accuracy and precision, respectively. The stability-indicating potential of the proposed method was proved under different stress-degradation conditions. The proposed method was successfully applied to the analysis of the three binary combinations in their tablets.     

电感耦合等离子体发射光谱法测定REACH法规涉及产品中铅、铬、钴、砷、锡、铝、锆、钼和硼

采用电感耦合等离子体原子发射光谱法对REACH法规涉及产品中铅、铬、钴、砷、锡、铝、锆、钼和硼的含量进行测定。0.2g样品经微波消解处理,聚合物材质试样以8mL硝酸和2mL过氧化氢为消解试剂;无机非金属材质试样以6mL硝酸、2mL过氧化氢和2mL氢氟酸为消解试剂。各元素的方法检出限均低于15mg·kg-1。方法的加标回收率在82.4%～108%之间,测定值的相对标准偏差(n=7)在3%～6%之间。     

Synthesis of 2, 4, 6-trialkyl-3-hydroxypyridines

Summary A new method was proposed for the synthesis of 2,4,6-trialky1-3-hydroxypyridines by the reactions of 3,5-dialkyl-2-acylfurans with ammonia.     

Preparation,infrared and Raman spectra,force field and thermodynamic functions for Trifluoromethylsulfenyl Bromide,CF3SBr

Trifluoromethylsulfenyl bromide was obtained by a new preparative method. Its IR (vapour and pure solid) and Raman (liquid) spectra are fully characterized and an assignment is proposed for the observed bands. A normal coordinate analysis was made by means of a stewise-coupling method. Thermodynamic properties in the temperatur range between 200—1000 K are tabulated.     

Validated and optimized high-performance liquid chromatographic determination of tizoxanide, the main active metabolite of nitazoxanide in human urine, plasma and breast milk

A high-performance liquid chromatographic method was optimized and validated for the determination of desacetyl nitazoxanide (tizoxanide), the main active metabolite of nitazoxanide in human plasma, urine and breast milk. The proposed method used a CN column with mobile phase consisting of acetonitrile-12mM ammonium acetate-diethylamine in the ratio of 30:70:0.1 (v/v/v) and buffered at pH 4.0 with acetic acid, with a flow rate of 1.5 mL/min. Quantitation was achieved with UV detection at 260 nm using nifuroxazide as internal standard. A simplified direct injection of urine samples without extraction in addition to the urinary excretion pattern were calculated using the proposed method. Also, the effectiveness of protein precipitation and a clean-up procedure were investigated for biological plasma and human breast milk samples. The validation study of the proposed method was successfully carried out in an assay range between 0.2 and 20 μg/mL.     

改进的GM（1,1）模型及其在色谱保留值研究中的应用

由于常规ＧＭ（１，１）模型对批相ＨＰＬＣ中化合物容量因子与流动相组成间非线性关系的线性近似以及常规ＧＭ（１，１）模型建模方法所固的缺点，使得常规ＧＭ（１，１）模型的预测精度难以提高。本文用近代非线性回归分析法对建模方法作了改进，建立了具有更高精度的ＧＭ（１，１）模型，并将其用于多环芳烃容量因子随流动相组成变化关系的建模，获得了满意的结果。     

Spectrophotometric Determination of Ampicillin, Amoxycillin, and Carbenicillin Using Folin-Ciocalteu Phenol Reagent

A spectrophotometric method for the determination of penicillins (ampicillin, amoxycillin and carbenicillin) using Folin-Ciocalteu reagent (FC reagent) is described. The reaction mixture of penicillin and FC reagent (pH 2.25) was heated in a thermostated water bath (95 ± 2°C) and the resulting blue color due to the formation of heteropoly blues was detected spectrophotometrically at the corresponding _max for these penicillins. The experimental conditions were optimized and Beer's law was obeyed over the applicable concentration ranges. The precision of the proposed method was checked using 10 replicate determinations of a specified amount of these penicillins. The proposed method was applied successfully for the analysis of these drugs in pure form and pharmaceutical preparations. The results obtained from the proposed and reference methods were compared statistically using the Student's t and F-variance ratio tests. A statistical analysis of the results is reported.     

Determination of hexabromocyclododecane enantiomers in chicken whole blood by a modified quick,easy, cheap,effective, rugged,and safe method with liquid chromatography and tandem mass spectrometry

A rapid and simple analytical method has been developed for the determination of hexabromocyclododecane enantiomers in chicken whole blood, based on a modified quick, easy, cheap, effective, rugged, and safe approach before liquid chromatography coupled with tandem mass spectrometry. The factors influencing performance of method were investigated by single factor experiment, and further optimized by the response surface methodology based on Box–Behnken design. The matrix effects were also evaluated by the isotopic dilution method. Under the optimal conditions, the proposed method showed good linearity within the range of 1–500 μg/L and good repeatability with relative standard deviation less than 9.5% (n = 5). The limits of detection (S/N = 3) were 0.03–0.19 μg/L. The developed method was successfully applied for the analysis of hexabromocyclododecane enantiomers in real chicken blood samples. The satisfactory recoveries ranging of 83.6–115.0% were obtained (at spiked levels of 5, 20, and 100 μg/L). The results demonstrated that the proposed method would be a practical value method for the determination of hexabromocyclododecane enantiomers in animal blood. It would be further developed with confidence to analyze other lipophilic organic pollutants in blood sample.