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高效液相色谱法测定山生柳中酚苷类成分的含量 总被引:2,自引:0,他引:2
用高效液相色谱法测定山生柳中水杨苷、水杨酰水杨苷和木犀草素07-O-葡萄糖苷的含量,流动相为1.5%醋酸溶液-甲醇,Symmetry C18柱,柱温30℃,流速1.1mL/min,检测波长270nm,线性浓度范围分别为527.0-105.4um/mL,140-28.0ug/mL,81.0-16.2ug/mL,平均回收率是104.9%和103.6%,RSD分别为2.0%,0.3%和0.3%。 相似文献
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ICP-AES法测定氧化铝粉中硅、钙、铁、钛、钒和锌 总被引:1,自引:1,他引:1
采用高压盐酸消化,电感耦合等发射光谱法测定氧化铝中硅、钙、铁、钛、钒和锌等6元素,研究了铝基体对被测元素的影响,并选择了最佳工作条件,被测元素的检出限为0.34-52ng/mL,样品加标回收率为95.7%-108.6%。 相似文献
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离子色谱荧光检测法测定废水中痕量2-氨基联苯和4-氨基联苯 总被引:2,自引:0,他引:2
采用离子色谱荧光检测法测定废水中的2-氨基联苯(2-ADP)和4-氨基联苯(4-ADP),流动相为1.0mL/min的0.06mol/L NaCl,0.08mol/L HCl,40%(V/V)ACN,分离柱为Dinoex OmniPac PCX-500,该法具有良好的重现性和线性关系,2-ADP和4-ADP的回收率分别为98.5%-101.4%和102.2%-104.0%,检测限分别为0.006mg/L和0.10mg/L。 相似文献
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高效毛细管电泳电导法快速检测复方维生素B片中的VBl、VBl2、VB6和VC 总被引:1,自引:0,他引:1
采用高效毛细管电泳电导法同时分离、测定了复方维生素B片中的主要成分VB1,VB12,VB6和VC的含量。研究了运行缓冲溶液的酸度和浓度、电泳电压、进样时间等因素对电泳的影响。在优化的实验条件下:40mmol/L Tris-4mmol/L H3BO3(pH8.0)的缓冲溶液中加入0.30mmol/L CTAB(溴化十六烷基三甲基铵),分离电压为15kV,上述4组分在5min内得到良好的分离。维生素B1,B12,B6和VC的线性范围分别为5.5~1.0mg/mL;15~1.5mg/mL;1.0~0.40mg/mL和6.6~0.80mg/mL;检测限分别为0.80μg/mL,4.0μg/mL,0.50μg/mL,2.9μg/mL;5次测定峰高的相对标准偏差分别为2.2%,1.6%,3.9%,2.8%。5次测定的平均回收率分别为99%,94%,l00%,97%。 相似文献
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氢化物发生-冷阱捕获-色谱分离-原子吸收法测定天然水中砷的形态 总被引:4,自引:0,他引:4
研究建立了氢化物发生-冷阱捕获-色谱分离-原子吸收方法测定天然水中四种主要砷形态。测试系统自行组装,色谱住填料采用ChromosorbGAW-DMCS(粒径0.3~0.45mm),其上涂布3%OV-101。方法的检出限以砷计分别为:As(V)0.51ng,As(Ⅲ)0.43ng,MMA0.38ng,DMA067ng;12ng砷标准偏差As(Ⅴ)4.21%,As(Ⅲ)3.56%,MMA3.23%,DMA5.46%。在0~50ng砷量范围标准曲线线性关系良好。该法适用性广,已用于湖水、河水、海水和地下水等不同水样神形态测定,加标回收率93.5%~104.9%。给出了上述水样四种砷形态的分析结果。 相似文献
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塞曼石墨炉原子吸收法直接测定血清中的硒 总被引:12,自引:0,他引:12
采用硝酸钯为硒的基体改进剂,用塞曼效应扣除背景,对消化后的血样直接进行测定。该法的检出限为6.0ng/mL,线性范围10ng/mL-136ng/mL,回收率为94.8%-102.5%。 相似文献
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Linbo Xia Yingliang Wu Zucheng Jiang Shengqing Li Bin Hu 《International journal of environmental analytical chemistry》2013,93(11):953-962
The use of 1-phenyl-3-methyl-4-benzoylpyrazolone (PMBP) as extractant for separation of Fe(III) and Fe(II) and low-temperature vaporization of the Fe(III)–PMBP chelate into ICP-AES for their speciation analysis was investigated. The factors affecting the formation of Fe(PMBP)3 chelate and its vaporization behavior were investigated in detail. PMBP was used not only as the extractant for the separation of Fe(III) and Fe(II) but also as the chemical modifier for the low-temperature ETV-ICP-AES determination of iron. Under the optimized conditions, the detection limit for iron(III) and iron(II) are both 3.2?ng/mL, with relative standard deviations of 3.9 and 4.5%, respectively. The proposed method was applied to the determination of trace iron in biological standard reference materials and the species in East Lake water samples, and the results obtained were satisfactory. 相似文献
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Based on gaseous compound introduction as 1-phenyl-3-methyl-4-benzoylpyrazolone[5](PMBP) chelate of aluminum by electrothermal vaporization in ICP-AES, a method for determination of trace aluminum was developed. Trace aluminum was vaporized at temperature of 1000 degrees C, and the vaporization behavior of aluminum chelate was detailedly investigated. Under the optimum conditions, the detection limit of aluminum was 0.6 ng ml(-1), and the relative standard deviation for 0.1 mug ml(-1) aluminum was 4.7% (n=8). The proposed method was applied to the determination of trace aluminum in rice flour reference materials, and the results well agreed with the reference values. 相似文献
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A new method for the simultaneous determination of five transition metal ions in water and food by rapid high‐performance liquid chromatography was developed. The cobalt, nickel, copper, zinc and vanadium ions were pre‐column derivatized with 2‐(2‐quinolinylazo)‐4‐methyl‐1,3‐dihydroxidebenzene (QAMDHB) to form colored chelates, then the Co‐QAMDHB, Ni‐QAMDHB, Cu‐QAMDHB, Zn‐QAMDHB and V‐QAMDHB chelates were enriched by solid phase extraction with a C18 cartridge. The enrichment factor of 50 was achieved by eluting the retained chelates from the cartridge with tetrahydrofuran (THF). These chelates were separated on a ZORBAX Stable Bound rapid analysis column (4.6 × 50 mm, 1.8 um) with 68% methanol (containing 0.1% of acetic acid and 0.1% of CTMAB) as mobile phase at a flow rate of 2.0 mL/min and detected with a photodiode array detector from 450?600 nm. The Co‐QAMDHB, Ni‐QAMDHB, Cu‐QAMDHB, Zn‐QAMDHB and V‐QAMDHB chelates were separated completely within 2.0 min. The detection limits of cobalt, nickel, copper, zinc and vanadium are 2 ng/L, 1.5 ng/L, 2 ng/L, 3 ng/L, and 3 ng/L, respectively, in the original samples. This method was applied to the determination of the five transition metal ions in water and food samples with good results. 相似文献
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The possibility was investigated by using 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) as the chelating reagent for separation and preconcentration of manganese(II) by cloud point extraction (CPE) and subsequent determination by flame atomic absorption spectrometry (FAAS). The effects of experimental conditions such as pH, concentration of chelating agent and surfactant, equilibration temperature and time on cloud point extraction were studied. Under the optimum conditions, preconcentration of 10 ml of sample solution permitted the detection of 1.45 ng mL(-1) of manganese with an enrichment factor of 20. The proposed method was applied to the determination of trace manganese in water samples with satisfactory results. 相似文献
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A reversed phase ion-paired chromatographic method that can be used to determine trace amounts of iron (II,III), nickel (II) and copper (II) was developed and applied to the determination of iron (II) and iron (III) levels in natural water. The separation of these metal ions as their 4,7-diphenyl-1,10-phenanthroline (bathophenanthroline) chelates on an Inertsil ODS column was investigated by using acetonitrile-water (80/20, v/v) containing 0.06 M perchloric acid as mobile phase and diode array spectrophotometric detection at 250-650 nm. Chromatographic parameters such as composition of mobile phase and concentration of perchloric acid in mobile phase were optimized. The calibration graphs of iron (II), nickel (II) and copper (II) ions were linear (r > 0.991) in the concentration range 0-0.5, 0-2.0 and 0-4.0 mug ml(-1), respectively. The detection limit of iron (II), nickel (II) and copper (II) were 2.67, 5.42 and 18.2 ng ml(-1) with relative standard deviation (n = 5) of 3.11, 5.81 and 7.16% at a concentration level of 10 ng ml(-1) for iron (II) and nickel (II) and 25 ng ml(-1) for copper (II), respectively. The proposed method was applied to the determination of iron(II) and iron(III) in tap water and sea water samples without any interference from other common metal ions. 相似文献
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Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples 下载免费PDF全文
Mohammad Ali Taher Fatemeh Pourmohammad Hamid Fazelirad 《Journal of separation science》2015,38(23):4153-4158
In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra‐trace amounts of rhodium after adsorption of its 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015–0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. 相似文献
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Cloud point extraction (CPE) was applied as a preconcentration step prior to graphite furnace atomic absorption spectrometry (GFAAS) determination of manganese(II) and iron(III) in water samples. After complexation with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), the analytes could be quantitatively extracted to the phase rich in the surfactant p-octylpolyethyleneglycolphenylether (Triton X-100) and be concentrated, then determined by GFAAS. The parameters affecting the extraction efficiency, such as solution pH, concentration of PMBP and Triton X-100, equilibration temperature and time, were investigated in detail. Under the optimum conditions, preconcentration of 10 ml of sample solution permitted the detection of 0.02 ng ml(-1) of Mn(II) and 0.08 ng ml(-1) of Fe(III) with enrichment factors of 31 and 25 for Mn(II) and Fe(III), respectively. The proposed method was applied to determination of trace manganese(II) and iron(III) in water samples with satisfactory results. 相似文献
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对石墨炉原子吸收光谱法测定地球化学样品中痕量银进行了研究。样品经盐酸、硝酸、硫酸、高氯酸溶解,在盐酸(1.2mol/L)介质中用醋酸丁酯萃取银与二苯硫脲螯合物,用石墨炉原子吸收光谱法测定地球化学样品中痕量银,方法检出限为0.011ng/mL,相对标准偏差(RSD,n=11)为6.0%~12.2%,加标回收率为96.00%~105.00%。能满足地球化学样品中银含量为0.02~5μg/g范围内银测定的准确度和精密度的要求。 相似文献