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1.
A method for direct determination of trace arsenic in high purity neodymium oxide by ICP-MS/MS was established. The interference of 150Nd++ on the determination of 75As+ was eliminated by oxygen reaction mode. Neodymium oxide was reacted in oxygen mode to generate 166(NdO) + and 166(NdO) ++ interfering ions, which did not affect the detection of 75As+. When the matrix concentration was 500 mg/L and the internal standard element was Ge, the recoveries of arsenic were between 96.2% and 102.2%, the relative standard deviations (RSDs) were between 5.2% and 8.6%, and the detection limit was 0.037 µg/g. The determination results of the actual samples were consistent with that of the glow discharge mass spectrometry. © 2023, Youke Publishing Co.,Ltd. All rights reserved.  相似文献   

2.
郭鹏 《分析试验室》2008,27(3):106-109
建立了用电感耦合等离子体质谱仪(ICP-MS)测定高纯氧化钽中28种痕量杂质元素的方法。讨论了质谱干扰及接口效应,采用标准加入法消除基体效应。各元素的方法检出限为0.001~0.1μg/g,回收率为90%~115%,方法适用于纯度为99.999%的高纯氧化钽中痕量杂质元素的测定。  相似文献   

3.
采用自行设计的固相微萃取(solid phase microextraction,SPME)与电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)联用的双气路热解析接口单元,建立了SPME-ICP-MS测定金属有机化合物的新方法.双气路热解析接口单元可实现样品在线热解析并与气动雾化的内标溶液气溶胶同步进入等离子体电离.方法线性范围为0.05~100 ng/mL,相对标准偏差1.3%~6.6%(n=5),检出限2pg/mL.所建立的方法用于合成水样中四乙基铅的测定,加标回收率93%~105%.  相似文献   

4.
5.
采用自制四氧化三锰纳米粒子固相萃取-电感耦合等离子体质谱法测定蔬菜中铅和铜的含量。优化的固相萃取条件如下:(1)样品溶液的pH为4.0;(2)样品溶液的流量为1.0mL·min^(-1);(3)四氧化三锰纳米粒子的用量为50mg;(4)洗脱剂为3mol·L^(-1)盐酸溶液,用量为2mL;(5)样品溶液的体积为20mL。铅和铜的线性范围依次为0.01~5.0,0.02~1.0μg·L^(-1),检出限(3s/k)依次为4,8ng·L^(-1)。加标回收率为80.0%~108%,测定值的相对标准偏差(n=7)为0.94%~3.2%。  相似文献   

6.
采用多孔聚偏氟乙烯膜包裹多壁碳纳米管制备成多孔膜保护固相微萃取装置,该装置经水洗涤、甲醇活化、干燥后,放入1 L样品中,包膜以500 r·min^(-1)的速率搅拌30 min,吸附富集痕量苯系物。取出包膜,在1 mL甲醇中解吸5 min后获得浓缩的苯系物样品,经气相色谱-质谱法分析,比对NIST 14谱库并结合标准品的气相色谱保留时间对其中的10种痕量苯系物进行定性,采用外标法定量。结果表明,应用自制的固相微萃取装置,可有效去除体系的基质干扰,提高萃取效率,与NIST 14谱库比对定性,富集的10种苯系物的匹配度均不小于90%,说明方法定性准确。定量分析时,10种苯系物的质量浓度在1.000~1 000 ng·L^(-1)内与对应的峰面积呈线性关系,检出限为0.010~0.013 ng·L^(-1)。按照标准加入法进行回收试验,回收率为97.5%~100%,测定值的相对标准偏差(n=5)为0.89%~1.5%。方法用于测定12份实际水样,其中1份样品中氯苯检出量为179.0 ng·L^(-1),1份样品中对二甲苯检出量为151.0 ng·L^(-1)。  相似文献   

7.
钡以及轻稀土元素氧化物对中、重稀土元素的干扰一直是质谱测试中存在的问题。建立了石墨粉垫底碳酸钠-硼酸混合熔剂熔融前处理样品,以103Rh为内标校正,一体化碰撞反应-电感耦合等离子体质谱仪法测定地质样品中稀土元素含量的方法。探讨了碳酸钠-硼酸混合熔剂熔融前处理样品注意事项、碰撞模式下碰撞气流量和离子透镜的参数的优化、干扰校正试验等问题,采用国家标准物质GBW07403、GBW07405、GBW07427、GBW07429验证,实验结果表明,各元素线性关系良好,相关系数均大于0.999,方法检出限在0.01~0.03mg/kg之间,相对误差为0.13%~7.1%,相对标准偏差为0.79%~6.59%,测试结果与标准值相吻合。对实际样品分析,得到平滑的球粒陨石归一化的稀土元素配分曲线,证明测定结果是合理可信的。该方法熔剂用量少,过程空白低,对器皿的侵蚀小,直接加热浸取,简化了操作过程,适用于大批量地质样品中稀土元素的测定。  相似文献   

8.
取磨碎的软木塞样品0.500 0g,用水超声提取30min,取提取液9mL置于萃取瓶中,加入1.8g Na2SO4,于55℃进行固相微萃取35min后,于气相色谱仪进样口解吸7min,采用气相色谱-质谱法测定其中愈创木酚的含量。结果表明:愈创木酚在25.00~2 000μg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.022μg·L-1,按标准加入法进行回收试验,回收率为69.8%~115%,测定值的相对标准偏差(n=6)为6.3%~13%。  相似文献   

9.
分别将N-(β氨乙基)-?-氨丙基三甲氧基硅烷(AEAPTMS)、3-巯丙基三甲氧基硅烷(MPTMS)与四乙氧基硅烷(TEOS)水解共聚,制备氨基巯基键合的硅胶材料。将此材料作为固相萃取(SPE)小柱的填充材料,建立了固相萃取快速分离富集海产品样品中五价砷As(Ⅴ)和三价砷As(Ⅲ)电感耦合等离子体质谱法(ICP-MS)测定海产品中无机砷的方法。研究了固相萃取小柱对无机砷的吸附原理、性能和洗脱条件,在pH3~4范围内固相萃取小柱材料有良好的选择吸附性,利用2%硝酸可将As(Ⅴ)洗脱,利用2%硝酸+0.1mol/L KIO3可将As(Ⅲ)洗脱。实际样品检测的加标回收率在72~103%之间,方法实现了海产品样品中无机砷形态快速、方便、准确的检测。  相似文献   

10.
采用王水溶样,活性炭动态吸附富集,电感耦合等离子体质谱法测定化探样品中痕量金,优化了样品分解、吸附条件、干扰消除等条件。结果表明,检出限0.13ng/mL,RSD〈4.7%,回收率97.63%~103.35%。该法准确可靠、简便快速,能满足化探样品检测要求。  相似文献   

11.
    
Graphene oxide based molecularly imprinted polymers modified with β‐cyclodextrin were prepared as solid‐phase extraction column sorbents for specific recognition and sensitive detection of di(2‐ethylhexyl) phthalate in water samples. The morphology and composition of synthesized sorbents were characterized by scanning electron microscopy, thermo‐gravimetric analysis, Raman spectroscopy, and Fourier‐transform infrared spectroscopy. The conditions affecting the performance of extraction procedures such as desorption solvent types and volume, sample pH and volume were investigated. The loading capacity (8.2 μg/mg) of the prepared sorbents increased eight times after modification with β‐cyclodextrin. The developed extraction procedures coupled to high‐performance liquid chromatography exhibited good linearity (0.2–500 μg/L), low limit of detection (0.052 μg/L), and good precision (relative standard deviation?5.7%) under optimized conditions. The developed solid‐phase extraction technique with prepared sorbents has been successfully applied in extracting trace di(2‐ethylhexyl) phthalate from real natural waters with high efficiency, good selectivity, and desirable recoveries.  相似文献   

12.
    
The application of graphene‐based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene‐based material, their properties, synthesis routes, and the most important applications in both off‐line and on‐line sample preparation techniques. The discussion of the off‐line approaches includes methods derived from conventional solid‐phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on‐line approaches focus on the use of graphene‐based material mainly in on‐line solid phase extraction, its variation called in‐tube solid‐phase microextraction, and on‐line microdialysis systems.  相似文献   

13.
    
A new three‐dimensional graphene oxide‐wrapped melamine foam was prepared and used as a solid‐phase extraction substrate. β‐Cyclodextrin was fabricated onto the surface of three‐dimensional graphene oxide‐wrapped melamine foam by a chemical covalent interaction. In view of a specific surface area and a large delocalized π electron system of graphene oxide, in combination with a hydrophobic interior cavity and a hydrophilic peripheral face of β‐cyclodextrin, the prepared extraction material was proposed for the determination of flavonoids. In order to demonstrate the extraction properties of the as‐prepared material, the adsorption energies were theoretically calculated based on periodic density functional theory. Static‐state and dynamic‐state binding experiments were also investigated, which revealed the monolayer coverage of flavonoids onto the β‐cyclodextrin/graphene oxide‐wrapped melamine foams through the chemical adsorption. 1H NMR spectroscopy indicated the formation of flavonoids–β‐cyclodextrin inclusion complexes. Under the optimum conditions, the proposed method exhibited acceptable linear ranges (2–200 μg/L for rutin and quercetin‐3‐O‐rhamnoside; 5–200 μg/L for quercetin) with correlation coefficients ranging from 0.9979 to 0.9994. The batch‐to‐batch reproducibility (= 5) was 3.5–6.8%. Finally, the as‐established method was satisfactorily applied for the determination of flavonoids in Lycium barbarum (Goji) samples with relative recoveries in the range of 77.9–102.6%.  相似文献   

14.
    
Determination of methamphetamine is of great importance in clinical and forensic laboratories because there are low dosages of drugs in the biological media and social problems created due to the methamphetamine consumption. Polymeric carbon based‐nano composites are reasonable candidates for dispersive solid phase extraction method due to facial and affordable synthesis process and high selectivity and sensitivity. Nano graphene oxide polypyrolle composite was synthesized and employed as dispersive solid‐phase extraction adsorbent for methamphetamine extraction from complex urine matrix. Full characterization of the prepared nano graphene oxide polypyrolle composite was completed and the influential extraction parameters were investigated through one‐parameter‐at‐a‐time method. High‐performance liquid chromatography detectors were applied as detection and quantification instrument. The optimized extraction parameters included 300 µL of methanol, 10 min of extraction and desorption time, 6000 stirring rate, urine pH value of 10, 60 mg of adsorbent, and 6 mL of urine volume. After outlining the calibration curve, the linear range of the method was considered as 30–800 ng/mL. The detection limit for the suggested method was 9 ng/mL. The analysis of addicted subjects with the proposed method confirmed the utility of the method in different analytical and clinical laboratories.  相似文献   

15.
    
Magnetic dispersive solid‐phase extraction followed by dispersive liquid?liquid microextraction coupled with gas chromatography/mass spectrometry was applied for the quantitative analysis of phenazopyridine in urinary samples. Magnetic dispersive solid‐phase extraction was carried out using magnetic graphene oxide nanoparticles modified by poly(thiophene‐pyrrole) copolymer. The eluting solvent of this step was used as the disperser solvent for the dispersive liquid?liquid microextraction procedure. To reach the maximum efficiency of the method, effective parameters including sorbent amount, adsorption time, type and volume of disperser and extraction solvents, pH of the sample solution, and ionic strength as well as desorption time, and approach were optimized, separately. Characterization of the synthesized sorbent was studied by utilizing infrared spectroscopy, scanning electron microscopy, and energy‐dispersive X‐ray analysis. Calibration curve was linear in the range of 0.5?250 ng/mL (R2 = 0.9988) with limits of detection and quantification of 0.1 and 0.5 ng/mL, respectively. Intra‐ and interday precisions (RSD%, n = 3) of the method were in the range of 4.6?5.4% and 4.0?5.5%, respectively, at three different concentration levels. Under the optimal condition, this method was successfully applied for the determination of phenazopyridine in human urine samples. The relative recoveries were obtained in the range of 85.0?89.0%.  相似文献   

16.
    
We present a simple method for the fabrication of a magnetic amino‐functionalized zinc metal‐organic framework based on a magnetic graphene oxide composite. The resultant framework exhibited a porous 3D structure, high surface area and good adsorption properties for nitrogen‐containing heterocyclic fungicides. The adsorption process and capacity indicated that the primary adsorption mechanism might be hydrogen bonding and π‐π conjugation. In addition, an optimized protocol for magnetic solid phase extraction was developed (such as adsorbent content, pH, and desorption solvent), and utilized for the extraction of nitrogen‐containing heterocyclic fungicides from vegetable samples. Quantitation by high performance liquid chromatography coupled with tandem mass spectrometry offered a detection limit of 0.21–1.0 μg/L (S/N = 3) with correlation coefficients larger than 0.9975. These results demonstrate that magnetic amino‐functionalized zinc metal‐organic framewor is a promising adsorbent for the extraction and quantitation of nitrogen‐containing heterocyclic fungicides.  相似文献   

17.
    
Packed cartridges have been widely used in solid‐phase extraction. However, there are still some drawbacks, such as they are blocked easily and the method is time‐consuming. In view of the advantages of monoliths, a monolithic extraction material has been directly synthesized in a glass syringe without any gap between the monolith and syringe inner wall. The monolithic syringe was modified with graphene oxide by loading graphene oxide dispersion onto it. The content of graphene oxide and the surface topography of the monolith have been evaluated by elemental analysis and scanning electron microscopy, respectively, which confirmed the successful modification. This prepared graphene oxide‐modified monolithic syringe was directly used as a traditional solid‐phase extraction cartridge. As expected, it shows good permeability and excellent capability for the extraction of quaternary ammonium alkaloids. The sample loading velocity (1–6 mL/min) does not affect the recovery. Under the optimal conditions, good linearities (= 0.9992–0.9998) were obtained for five quaternary ammonium alkaloids, and the limits of detection and quantification were 0.5‐1 and 1–2 μg/L, respectively. The proposed method was successfully applied for the analysis of quaternary ammonium alkaloids in Chinese patent medicine.  相似文献   

18.
    
A novel method was developed to simultaneously determine the ciprofloxacin and levofloxacin levels in human urine using an ionic‐liquid‐based, dual‐molecularly imprinted polymer‐coated graphene oxide solid‐phase extraction monolithic column coupled with high‐performance liquid chromatography. The molecularly imprinted monolithic column was prepared using ciprofloxacin and levofloxacin as templates, 1‐vinyl‐3‐ethylimidazolium bromide as the functional monomer, and graphene oxide as the core material. The resulting imprinted monoliths were characterized by scanning electron microscopy and fourier transform‐infrared spectroscopy. The efficiency and capacity of the ionic‐liquid‐based imprinted monolithic column were investigated by varying the synthesis conditions (ciprofloxacin/levofloxacin ratio and template/functional monomer/cross‐linker ratio). The solid‐phase extraction process was optimized by changing the washing and eluting conditions. The results suggested that the proposed ionic‐liquid‐based molecularly imprinted solid‐phase extraction monolithic‐high‐performance liquid chromatography method could separate ciprofloxacin and levofloxacin efficiently and simultaneously from human urine. The mean recoveries of ciprofloxacin and levofloxacin ranged from 89.2 to 93.8 and 86.7 to 94.6%, respectively. The intra‐ and interday relative standard deviation ranged from 0.9 to 3.2 and 0.8 to 2.9%, respectively. Under the optimized conditions, the recoveries of ciprofloxacin and levofloxacin were more than 93.8%.  相似文献   

19.
    
Magnetic zeolitic imidazolate framework 67/graphene oxide composites were synthesized by one‐pot method at room temperature for the first time. Electrostatic interactions between positively charged metal ions and both negatively charged graphene oxide and Fe3O4 nanoparticles were expected to chemically stabilize magnetic composites to generate homogeneous magnetic products. The additional amount of graphene oxide and stirring time of graphene oxide, Co2+, and Fe3O4 solution were investigated. The zeolitic imidazolate framework 67 and Fe3O4 nanoparticles were uniformly attached on the surface of graphene oxide. The composites were applied to magnetic solid‐phase extraction of five neonicotinoid insecticides in environmental water samples. The main experimental parameters such as amount of added magnetic composites, extraction pH, ionic strength, and desorption solvent were optimized to increase the capacity of adsorbing neonicotinoid insecticides. The results show limits of detection at signal‐to‐noise ratio of 3 were 0.06–1.0 ng/mL under optimal conditions. All analytes exhibited good linearity with correlation coefficients of higher than 0.9915. The relative standard deviations for five neonicotinoid insecticides in environmental samples ranged from 1.8 to 16.5%, and good recoveries from 83.5 to 117.0% were obtained, indicating that magnetic zeolitic imidazolate framework 67/graphene oxide composites were feasible for analysis of trace analytes in environmental water samples.  相似文献   

20.
    
Novel molecularly imprinted chitosan microspheres were prepared on the surface of magnetic graphene oxide, with deep eutectic solvents both as a functional monomer and template. The prepared molecularly imprinted chitosan microspheres‐magnetic graphene oxide was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X‐ray diffraction, Brunauer‐Emmett‐Teller surface area, thermogravimetric analysis were subsequently combined with solid‐phase micro‐extraction for simultaneous separation and enrichment of the extraction of chlorophenols from environmental water. Factors affecting the extraction efficiency of chlorophenols were optimized using response surface methodology. The actual extraction capacities under the optimal conditions (liquid to solid ratio = 3, cycles of adsorption/desorption = 5, 40°C extraction temperature, and extraction time for 35 min) were 86.90 mg/g. Compared to the traditional materials, the molecularly imprinted chitosan microspheres‐magnetic graphene oxide produced higher selectivity and extraction capacity.  相似文献   

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