ICP-AES法测定铅精矿中的杂质元素

用HNO3-KClO3-H2SO4溶样,采用ICP-AES测定铅精矿中的杂质元素。并试验了酸度、共存元素对测定的影响,方法的精密度、检出限及回收率均能满足要求。     

ICP-AES法测定铝合金中钪元素的方法研究

本方法采用ICP-AES法进行铝合金中Sc元素的测定,系统研究了四十余种元素对Sc三条分析谱线的光谱干扰情况,进行了分析线的选择,分别用酸溶解法和碱溶解法溶解铝合金样品,测定了方法检出限,方法回收率98％-100.3％。该方法准确、可靠、简便、快速。     

ICP-AES测定铜合金中的磷

采用ICP-AES测定铜合金中的磷元素。通过实验探讨了铜合金中基体元素,共存元素对磷元素分析谱线的光谱干扰情况,确定了合适的分析谱线。对一系列不同牌号不同含量的铜合金中的磷进行测定,通过实验探讨了铜合金中基体元素铜对磷元素测定的干扰情况。方法的检出限为0.00084%,Z-15铍青铜和铅黄铜测定结果的相对标准偏差分别为2.06%和2.89%。加标回收率为85.3%—98.2%。     

ICP-AES测电解金属锰中的金属元素

采用电感耦合等离子体-原子发射光谱法(ICP-AES)同时测定电解金属锰中的Ca、Mg、Fe、Cu、Co、Ni、Zn、Cr、Sb、Pb金属元素。样品用HNO3+HCl经微波消解后,试液直接进样用ICP-AES同时测定上述元素。对分析谱线、基体效应和等离子体参数等进行了讨论,确定了实验的最佳测定条件。在选定的最佳测定条件下各元素的检出限为0.004—0.053μg/mL,相对标准偏差小于3.5%,回收率为93.7%—105.1%。     

微波消解-ICP—AES同时测定黄芪中10种微量元素

用硝酸和过氧化氢作为消解剂,微波消解技术处理黄芪样品,建立了微波消解-电感耦合等离子体发射光谱法（ICP-AES）同时测定黄芪中K、P、Ca、Mg、Fe、Sn、Mn、Cu、Zn和Cr等10种微量元素含量的方法。通过对样品微波消解条件和ICP-AES工作参数进行了优化,测定了各元素的分析线性、检出限、精密度和回收率等。各测试元素的校准曲线均具有良好的线性关系,检出限符合分析要求;以西红柿叶标准样品EPS-1验证,测得方法回收率为89.7%—112.8%,相对标准偏差（RSD）〈5.0%;黄芪样品的加标回收率为90.4%—107.0%,RSD〈5.0%。该方法具有良好的准确度和精密度,且具有快速、高效等特点。测定结果表明,黄芪中富含有K、P、Ca、Mg、Fe和Sn等元素,并据此对黄芪中富含的各元素与其特殊药理功效的关系做了初步讨论。     

ICP-AES测定钕铁硼永磁合金中主量元素

采用ICP-AES同时测定了钕铁硼永磁合金中的Nd、Fe、Co、B、Zr5种主量元素.选择了合适的分析线和样品测定浓度,确定了各元素的检出限为0.54-1.94μg/L,加标回收率为90.5%-119%.方法准确,快速、简便,用于生产实践中,结果令人满意.     

活性炭富集电感耦合等离子体原子发射光谱测定铋系超导粉中痕量铁

建立了电感耦合等离子体原子发射光谱(ICP-AES)测定超导粉中痕量铁的新方法。优化了仪器工作参数,对痕量铁测定时的基体干扰及消除干扰的方法进行了系统研究,结果表明:大量存在的基体元素产生一定基体效应,并使重现性变差,且由于铁含量甚微,仪器灵敏度不能满足测定的要求,需采用分离富集方法以提高测定结果的准确度和精密度。以三乙醇胺掩蔽基体元素铋和铜,在适宜的酸度条件下,铁与邻二氮菲生成配合物,以活性炭定量吸附,用1∶1硝酸解吸,并对分离富集条件进行了优化。对模拟标准样品进行测定,分析结果与理论值一致,相对标准偏差为2.4%,方法检出限为0.033μg.g-1。该方法已用于超导前驱粉样品中痕量铁的分析,结果令人满意,并进行了回收实验,回收率为95.6%～98.0%。     

ICP-AES测定工厂废酸液中的8种元素

工厂废酸液经过处理后,采用电感耦合等离子体-原子发射光谱法(ICP-AES)测定其中铝、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,选择各元素的分析线,测定各元素的检出限,样品的加标回收率在95.1％-101.5％之间,对2个工厂废酸液样品进行分析,8种元素测定的相对标准偏差RSD值(n=9)在0.087％-7.6％之间.     

ICP-AES测定粉末冶金材料中钨、钼等八种元素

用硝酸、高氯酸和氢氟酸溶解样品,在0.025 mol·L-1 EDTA介质中,采用一种标准溶液,用ICP-AES光谱法测定样品溶液中Ni,Cu,V,Mn,W,Mo,Co,Cr的含量。研究了基体和共存元素对分析元素光谱的影响,选择合适的波长,测定了分析结果的精密度,方法的检出限和回收率,结果表明,分析方法有很低的检出限,样品分析结果的相对标准偏差小于1%,加入回收率在98.2%～101.6%,方法准确、可靠、简便、快速,满足生产要求。     

ICP-AES法测定镍基高温合金中16个元素的方法研究

该方法采用ICP-AES法对镍基高温合金中16个元素进行了测定,系统研究了基体元素和共存元素对分析元素谱线的光谱干扰情况,进行了分析线的选择,测定了方法检出限,通过准确度试验和精密度试验,表明该方法准确、可靠、简便、快速。     

JP-303型极谱分析法测定痕量铅的研究

本文提出了在HCl-H3PO4底液中用极谱分析仪测定痕量的铅的方法,该方法检出限为0．02ug/mL,在0．02－10．00ug/mL范围内有很好的线性关系,峰电位在0．42V处波形清晰,重现性好,应用本方法测定酒中铅,回收率在99．9％－100．2％,此方法准确,简便,快速,选择性高。     

改进前处理方法测量土壤中痕量汞的重复性和重现性

为验证新的汞前处理方法,在本次实验中进行4次重现性验证,同一样品汞含量的平行值重复性较好,除第1次外,其他3次重现性均较好;4次实验中的校准曲线线性重现性非常好,斜率和截距变化不大,均在合理变化范围之内;初次实验中标准样品的汞含量测定值与理论值大部分不相符,经分析标准样品中汞元素不高,使得消解液中的汞的含量在检出限以下,导致仪器误差的增大,通过在验证实验中加大标准样品的取样量顺利地解决问题。     

荧光光谱法测定灵芝中多糖含量

以无水葡萄糖为标准品,对用荧光光谱法测定灵芝中多糖的含量进行了探讨,确定最佳实验条件为12.00mL浓硫酸,o.17mL 5%的苯酚溶液,室温下静置50min,荧光参数λex=478nm,λem=510nm.在此条件下对6种不同种灵芝的多糖含量进行了测定,多糖浓度与生成物的荧光强度呈良好的线性关系,线性方程为y=486...     

'Wrong-way-round ionization' and screening for doping substances in human urine by high-performance liquid chromatography/orbitrap mass spectrometry

To free analytical resources for new classes of doping substances, such as banned proteins, maximization of the number of compounds that can be determined with high sensitivity in a single run is highly urgent. This study demonstrates an application of 'wrong-way-round ionization' for the simultaneous detection of multiple classes of doping substances without the need to switch the polarity. A screening method for the detection of 137 compounds from various classes of prohibited substances (stimulants, diuretics, β(2)-agonists, β-blockers, antiestrogens, glucocorticosteroids and anabolic agents) has been developed. The method involves an enzymatic hydrolysis, liquid-liquid extraction and detection by liquid chromatography/orbitrap mass spectrometry with wrong-way-round ionization. Up to 64% of compounds had a 10-fold lower limit of detection (LOD) than the minimum required performance limit. To compare the efficiency of conventional ionization relative to wrong-way-round ionization of doping substances in?+?ESI, a fortified blank urine sample at the minimum required performance limit was analyzed using two ESI approaches. All compounds were detected with markedly better S/N in a high-pH mobile phase, with the exception of acetazolamide (minimal change in S/N, < 20%).The method was validated by spiking 10 different blank urine samples at five different concentrations. Validation parameters included the LOD, selectivity, ion suppression, extraction recovery and repeatability.     

红车轴草总异黄酮粉剂的质量标准

采用薄层色谱法建立其有效成分芒柄花素和鹰嘴豆芽素A定性方法,采用高效液相色谱法建立其有效成分芒柄花素和鹰嘴豆芽素A含量测定方法,以期建立红车轴草总异黄酮粉剂的质量标准。结果显示薄层斑点清晰、重现性好;测定芒柄花素和鹰嘴豆芽素A重现性好,平均加样回收率分别为101.10%及98.44%,RSD分别为2.19%和2.15%。本法简便、准确,可用于本品的质量控制。     

氢化物-原子荧光光谱法检测生活饮用水中的痕量铅

建立一种简便准确的氢化物-原子荧光光谱法检测生活饮用水中痕量铅的方法.在酸性介质中,以铁氰化钾为氧化剂,2%的盐酸为载流,样品中的铅与硼氢化钠(NaBH<,4>)或硼氢化钾(KBH<,4>)反应生成铅的挥发性氢化物(PbH<,4>),将氢化物导入原子化器中,检测其荧光强度.铅在0.00-30.0μg/L范围内,荧光强度...     

Repeatability characteristics of laser percussion drilling of stainless-steel sheets

An analysis on the repeatability of a laser percussion drilling process is conducted using a flash lamp pumped Nd:YAG laser on 2 mm thick stainless-steel sheets. Laser drilling process is finding increasingly widespread application in the industry and has continually attracted new interests to the industry in recent years. However, the inherent problem of hole geometry repeatability associated with laser percussion drilling is likely to limit the extent of industrial applications of the process. The characteristic of melt ejection is found to be dependent on the parameter setting and is shown to have a significant influence on entrance hole geometry and hence repeatability. The relationship between the percentage standard deviation of entrance hole diameter and the operating parameters is established, and varies between 1.8% and 5.6% in the operating range under this study.     

基体溶液改进-原子荧光法测定食品中的汞

探讨改进基体溶液双道原子荧光光谱法测定食品样品中的汞。样品消解后用6mol/L盐酸、硫脲+抗坏血酸(50g/L)作为基体溶液进行仪器测定。本方法检出限0.051μg/g,最低检出质量浓度0.10μg/L,相对标准偏差为7.45%、6.76%,回收率为88.6%—113.2%。方法具稳定性好、灵敏度高、检出限低等优点。     

A novel method for quantification of ethanol and methanol in distilled alcoholic beverages using Raman spectroscopy

In this study, direct quantification of ethanol and methanol in distilled alcoholic beverages using Raman spectroscopy was performed. Raman spectra of varying ethanol–methanol mixtures were obtained, baseline corrections were made, and the data were normalized using Raman scattering intensity of an internal standard (acetonitrile, 921 cm^–1). Then, calibration graphs were produced for ethanol and methanol concentrations in the ranges of 0–7 M and 0–10 M, respectively. Accurate R² values of the calibration graphs proved the notable linear correlations (0.998 for ethanol and 0.998 for methanol). The method was validated based on linearity, sensitivity, intraday and interday repeatability, and recovery tests. The limit of detection and limit of quantification values of the validated method were determined for ethanol concentration as 1.2 and 3.7 mM, and for methanol concentration as 3.4 and 10.3 mM, respectively. The ability of the developed method to detect ethanol and methanol concentrations in real samples was also investigated. The results of the developed method were compared with the experimental results from traditional method and high correlation value (R² = 0.926) was obtained. Besides being sensitive and cheap, the developed method is rapid with the analysis time of less than 30 s. Furthermore, it eliminates labor‐consuming operations, chromatographic separation, and measurement error due to the high number of experiment steps in the standard method. Copyright © 2012 John Wiley & Sons, Ltd.