JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
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2018
·Vol. 33
·期 11
·1910-1916
·
IF 3.608
Airui Zhang,Hai Wang,Pengfei Zha,Meiling Wang,Haifeng Wang,Bingqi Fan,Danhua Ren,Yanxiang Han,Sitian Gao
An analytical method of microwave induced combustion (MIC) combined with ICP-OES and TXRF is proposed to determine elemental impurities in graphene. Optimized MIC conditions (e.g. sample mass up to 30 mg, microwave irradiation 900 W for 10 min, and oxygen pressure 2 MPa) can achieve the rapid and complete digestion of graphene. Analytical results show that this method can accurately determine elemental impurities such as S, Fe, Cr, Mn and Ni in graphene, and that ICP-OES and TXRF data are comparable. The validity of this method is also verified using three different CRMs for cellulose nanocrystal powder and single-wall carbon nanotubes. The limits of detection (LODs) using MIC combined with ICP-OES are 5.4, 10.6, 7.3, 0.7 and 2.7 μg kg−1 for Fe, S, Cr, Mn and Ni, respectively. The LODs using MIC coupled with TXRF are 30.2, 215, 21.3, 9.5 and 15.8 μg kg−1 for Fe, S, Cr, Mn and Ni, respectively. The experimental results are also compared with those from three other pretreatment methods including dry ashing coupled with acid digestion (DA-AD), microwave-assisted digestion (MWAD) and DA-MWAD, which shows that MIC is superior to the other procedures due to the incomplete digestion and/or escape of volatile S of the latter. The MIC digestion combined with ICP-OES or TXRF could be one of the most promising procedures for the accurate determination of some elemental impurities in carbon nanomaterials with stable structures like graphene.
研究领域:
分析化学
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材料科学
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DOI
高影响因子
PLoS One
·
2017
·Vol. 12
·期 9
·e0185302
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IF 2.806
FuKai Li,AiJun Gong,LiNa Qiu,WeiWei Zhang,JingRui Li,Yu Liu,YuNing Liu,HuiTing Yuan
The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N′, N′-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL -1 (Nd) to 0.5038 ng mL -1 (Ho). The relative standard deviations (c = 100 ng mL -1 , n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4–1000 ng mL -1 (R 2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
ANALYTICA CHIMICA ACTA
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2020
·
IF 5.977
Xuelin Dong,Yuxiang Xiong,Nan Wang,Zhou Song,Jie Yang,Xiumei Qiu,Lihua Zhu
The analysis of siliceous matrix samples may adopt a two-step pretreatment , which includes melting with ammonium hydrogen fluoride and redissolving with nitric acid . However, the residual of substrate silicon unfavorable to the determination of trace elements in the samples due to serious matrix effects. Here, a new digestion method using simultaneously both ammonium bifluoride and nitric acid under normal pressure was developed for high-purity quartz sand sample. The digestion pretreatment is a two step process: melting/dissolving with both ammonium bifluoride and nitric acid at 200 °C for 2 h, and evaporating the solution at 250 °C to dryness. As confirmed by XRD analysis, silicates in the sample were converted to (NH 4 ) 3 SiF 6 NO 3 in the melting/dissolving step. TGA analysis shows that the generated (NH 4 ) 3 SiF 6 NO 3 could be decomposed and evaporated completely at 250 °C, which ensured a complete removal of silicon by the followed evaporation of the solution at 250 °C. As a result, the followed ICP-OES and ICP-MS analysis needed a solution dilution of only 100 times for the determination of Ca, Mg, Al, Rb, Ba, REE and other trace elements. The new method was applied to the analysis of three certified reference materials, and the results were well consistent with the standard value with RSD% values between 0.62% and 9.73%. Therefore, this method can be applied to the analysis of trace elements in high purity silica-based samples, with the advantages of time-saving, small dilution factor (only 100 times) and low detection limit.
研究领域:
分析化学
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材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
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2016
·
IF 4.035
Songqing Chen,Xingxiu Qin,Weixi Gu,Xiashi Zhu
Ionic liquids-β-cyclodextrin polymer (ILs-β-CDCP) was attached on Fe 3 O 4 nanoparticles to prepare magnetic solid phase extraction agent (Fe 3 O 4 @ILs-β-CDCP). The properties and morphology of Fe 3 O 4 @ILs-β-CDCP were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction(XRD), size distribution and magnetic analysis. A new method of magnetic solid phase extraction (MSPE) coupled to ICP-OES for the speciation of Mn(II)/Mn(VII) in water samples was established. The results showed that Mn(VII) and total manganese [Mn(II)+Mn(VII)] were quantitatively extracted after adjusting aqueous sample solution to pH 6.0 and 10.0, respectively. Mn(II) was calculated by subtraction of Mn(VII) from total manganese. Fe 3 O 4 @ILs-β-CDCP showed a higher adsorption capacity toward Mn(II) and Mn(VII). Several factors, such as the pH value, extraction temperature and sample volume, were optimized to achieve the best extraction efficiency. Moreover, the adsorption ability of Fe 3 O 4 @ILs-β-CDCP would not be significantly lower after reusing of 10 times. The accuracy of the developed method was confirmed by analyzing certified reference materials (GSB 07-1189-2000), and by spiking spring water, city water and lake water samples.
研究领域:
分析化学
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环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2020
·
IF 1.467
Weimin Ding,Xing Jin,Boyu Ma,Xiaobing Wang,Chenmei Lou,Jian Zheng,Zhiwei Hu,Lijia Jing,Yang Wang
A modified calibration curve method based on the combination of standard addition and traditional calibration curve methods was employed for the quantification of Prussian blue nanoparticles in rats in the presence of endogenous iron interferences. The assay was performed using inductively coupled plasma – optical emission spectrometry (ICP-OES) with yttrium as the internal standard, and validated in biomatrices including liver, heart, kidneys, lungs, spleen and whole blood. For the liver tissue, the intra-day and inter-day precision were 7.84% or less, and the accuracy was between 99.88% and 102.37%. For kidneys, lungs, heart, spleen, and blood, at each exo-additive level from 0.4 to 3.2 µg/mL, the intra-day accuracy was between 98.74% and 102.09%, and the intra-day precision was 6.17% or less. For the addition of no analyte, the intra-day accuracy was between 96.42% and 107.52%, and the intra-day precision was 15.67% or less. The stability was investigated at 25 °C for 24 h and 4 °C for 15 days in liver standard addition samples, and no significant degradation occurred under these conditions. This method was successfully applied to the preliminary pharmacokinetics and tissue distribution study of Prussian blue nanoparticles in rats. This approach may also be applied to the quantification of other ferruginous materials in the biological matrices with endogenous iron.
研究领域:
分析化学
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药代动力学
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生物医学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
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2025
·
IF 5.1
Yan Zhou,Xiaofang Yang,Leshou Zhang,Shaodui Ye,Ya Liu,Ning Lu,Yong Liu,Xiaodong Wen
Developing a fast, simple, and efficient sample pretreatment method is of great practical significance for the analysis of complex matrix samples. In this study, a novel multifunctional “four-in-one” effervescent tablet based on switchable hydrophobic deep eutectic solvent (SHDES) was prepared, which can simultaneously facilitate the in situ synthesis of SHDES and CO 2 generation, phase transition, and phase separation. The effervescent tablet based on the SHDES-assisted microextraction (ETA-SHDES-ME) technique was combined with inductively coupled plasma optical emission spectrometry (ICP-OES) for the determination of Pb 2+ in Pinellia ternata (Thunb.) Breit. The important parameters affecting the extraction efficiency of Pb 2+ were optimized using the Box-Behnken design (BBD). The enrichment factor (EF) and limit of detection (LOD) of the established method for Pb 2+ are 31 and 0.2 μg/L, respectively, offering a fast, simple, and eco-friendly approach, and has the application potential of field analysis.
研究领域:
分析化学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
TALANTA
·
2024
·
IF 5.6
Yukun Huang,Guangyu Chen,Biao Fu,Yingfu Si,Peng Li,Yijun Cao,Lingkun Rong,Chunjie Zhao
This study developed a rapid and efficient graphite furnace digestion combined with inductively coupled plasma emission spectrometry (ICP-OES) method, enabling precise quantification of germanium (Ge) in coal and various coal-derived metallurgical byproducts across a broad concentration level (∼ppm-n%). The graphite furnace digestion conditions were examined intensively as a function of the acid amounts of HNO 3 and HF (5–10 mL), temperature (80–180 °C), time (1–5 h), and acid drive methods (H 3 BO 3 neutralization versus heating). Coal references including SARM 19, SARM 20, NIST SRM 1632e, and fly ash standard NIST SRM 2689 were tested. The optimum recovery of germanium was obtained when the HNO 3 dosage, HF dosage, solid sample mass, temperature, and duration time were 10 mL, 5 mL, 0.1 g, 80 °C and 1 h. Agreement of 95.15–96.54 % between the measured and certified value was obtained under the optimum conditions. The spiked recovery was 103.23–103.54 %, indicating the matrix-analytes interactions were negligible. Boric acid neutralization reduced the recovery rates to 47.2–49.3 % and was not be appropriate for driving HF. The optimal spectral line for determining Ge is at a wavelength of 265.117 nm, at which the limit of detect and the limit of quantification were 0.46 μg L −1 and 1.53 μg L −1 , respectively. The applicability of the method was validated by quantifying Ge in Ge-rich lignite, fly ashes (FA), and chlorinated distillation residue (CR) samples. The concentration of Ge in coals was 44.75–225.41 μg g −1 , the content in FA was 0.68%–2.3 %, and the content in CR was 0.18 %, with the uncertainty of the method obtained being less than 0.5 %. X-ray fluorescence spectrometer (XRF) was used to verify the results. The difference between XRF data and ICP-OES data was less than 5 %, confirming the accuracy and reproductivity of the analytical method.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
Pigment & Resin Technology
·
2023
·Vol. 53
·期 5
·638-649
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IF 1.4
Shan Peng,Ranran Yang,Binglong Lei,Yun Gao,Renhua Chen,Xiaohong Xia,Kevin P. Homewood
PurposeThis paper aims to systematically demonstrate a methodology to determine the relative and absolute encapsulation efficiencies (αReandαAb) for thermally- and chemically-robust inorganic pigments, typically like ZrSiO4-based pigments, thereby enhancing their coloring performance.Design/methodology/approachThe authors designed a route, surplus alkali-decomposition and subsequently strong-acid dissolution (SAD2) to completely decompose three classic zircon pigments (Pr–ZrSiO4, Fe2O3@ZrSiO4and CdS@ZrSiO4) into clear solutions and preferably used inductively coupled plasma-optical emission spectrometry (ICP-OES) to determine the concentrations of host elements and chromophores, thereby deriving the numeric data and interrelation ofαReandαAb.FindingsZircon pigments can be thoroughly decomposed into some dissoluble zirconate–silicate resultants by SAD2 at a ratio of the fluxing agent to pigment over 6. ICP-OES is proved more suitable than some other quantification techniques in deriving the compositional concentrations, thereby the values ofαReandαAb, and their transformation coefficientKRA, which maintains stably within 0.8–0.9 in Fe2O3@ZrSiO4and CdS@ZrSiO4and is slightly reduced to 0.67–0.85 in Pr–ZrSiO4.Practical implicationsThe SAD2 method and encapsulation efficiencies are well applicable for both zircon pigments and the other pigmental or non-pigmental inhomogeneous systems in characterizing their accurate composition.Originality/valueThe authors herein first proposed strict definitions for the relative and absolute encapsulation efficiencies for inorganic pigments, developed a relatively stringent methodology to determine their accurate values and interrelation.
研究领域:
材料科学
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分析化学
✓ 已验证
DOI
高影响因子
ANALYTICAL LETTERS
·
2018
·
IF 1.206
Ziwei Li,Dongming Han,Mingchuan Wang,Yuexin Zhang,Yang Wang,Xiufeng Yan,Qiuying Pang
This study aimed to develop a precise and accurate method of sample preparation of Auricularia auricula for inductively coupled plasma-optical emission spectrometry-based trace element determination and to compare concentrations of seven trace elements (Mg, Fe, Mn, Zn, Ni, Cr, Sr) in six A. auricula samples belonging to three varieties with two cultivation substrates. Five sample preparation procedures, microwave-assisted digestion, nitric acid digestion with hot plate heating, nitric acid and perchloric acid digestion with hot plate heating, nitric acid digestion with ash content, and aqua regia digestion with ash content, were compared. The performance of the procedures was determined based on the precision and accuracy of the results and the limits of detection of the elements. The best results, with limits of detection of 0.60–6.60 ng · mL−1 and recoveries for spiked samples between 93.80 and 105.00%, were found using nitric acid digestion with ash content. Six A. auricula samples were analyzed using the proposed procedure. Among the tested elements, the concentration of Fe was highest in all six A. auricula samples up to a maximum concentration of 284.83 µg · g−1. The concentrations of Mn, Cu, and Ni increased in mixed stands (basswood, birch, and mongolica) compared with pine sawdust cultivation.
研究领域:
食品科学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2015
·Vol. 7
·期 19
·8235-8240
·
IF 1.821
Liping Wang,Haijun Li,Yaping Dong,Jiaoyu Peng,Haitao Feng,Wu Li
A magnesium hydroxide coprecipitation method for the determination of trace elements in high-salt samples from salt lake brines by inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. Some effects on the coprecipitation and analysis, such as the pH value and Na and Mg amounts in primary brines, have been thoroughly investigated and optimized. After adjusting the pH to 8.70, associated with sodium hydroxide, the complicated matrix was removed from high salt brines, and thus trace amounts of Al, Co, Cu, Fe, Mn, Ni, V, and Zn were simultaneously coprecipitated and precisely determined. Recoveries of all the determined trace elements in the samples of both synthesized and real salt lake brines were more than 90%. The detection limit in the range of 0.62–14.4 μg L−1 was obtained and the precision was less than 3% relative standard deviation. The optimized method has been successfully applied for the determination of trace elements in the intercrystal brine mined from Dachaidan salt lake located in the Qaidam Basin, China.
研究领域:
分析化学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
·
2026
·
IF 3.5
Zhiguang Xia,Mengting Zhang,Zihu Zhang,Xinyang Chen,Ying Gao,Jun Hu,Chunxia Yang,Thomas J. Algeo,Chao Li
An improved and robust method for determining carbonate-associated phosphate (CAP) is presented. • AG50W-X12 effectively purifies P from carbonate samples with high Mg Ca matrices. • The use of the P 177.495 nm emission line enables a low detection limit of <3 ppb. • CAP values for carbonate reference materials (GSR-13, GSR-23 and Jdo-1) agree well with published data and exhibit improved precision. • CAP values of five carbonate standards (GSR-26, GSR-27, GSR-28, GSR-29, and BCS-CRM 393) are reported for the first time. Carbonate-associated phosphate (CAP) serves as a direct proxy for reconstructing past oceanic phosphorus (P) concentrations and provides valuable insights into the co-evolution of marine P cycling, primary productivity, and atmospheric oxygen levels throughout Earth's history. However, current CAP analytical methods face challenges, including poor reproducibility, high detection limits, and a scarcity of geological reference material datasets for inter-laboratory comparison. In this study, we developed a method to purify P from carbonate samples with high Ca Mg matrices using AG50W-X12 cation-exchange resin, followed by quantitative determination by ICP-OES using the strongest P emission line at 177.495 nm, achieving a detection limit for CAP values of 0.002 mmol/mol. The methodological robustness with respect to variations in acid concentration, dissolution time, and the fraction of carbonate dissolved was evaluated through multiple independent experiments. The method was then applied to determine CAP values of eight carbonate geological reference materials (mmol/mol): CAP GSR-13 = 0.018 ± 0.002 (2σ, N = 3, RSD = 4.2%); CAP GSR-23 = 0.061 ± 0.008 (2σ, N = 8, RSD = 6.9%); CAP GSR-26 = 0.093 ± 0.014 (2σ, N = 3, RSD = 7.3%); CAP GSR-27 = 0.025 ± 0.006 (2σ, N = 3, RSD = 12.3%); CAP GSR-28 = 0.047 ± 0.008 (2σ, N = 3, RSD = 8.9%); CAP GSR-29 = 0.051 ± 0.010 (2σ, N = 3, RSD = 9.6%); CAP BCS-CRM 393 = 0.027 ± 0.005 (2σ, N = 3, RSD = 9.4%); CAP JDo-1 = 0.147 ± 0.008 (2σ, N = 3, RSD = 2.6%). Compared with previously published CAP values for three standards: CAP GSR-13 = 0.022 ± 0.004 (2σ, RSD = 9.1%), CAP GSR-23 = 0.075 ± 0.015 (2σ, RSD = 9.7%) or 0.070 ± 0.014 (2σ, RSD = 10.0%), and CAP JDo-1 = 0.135 ± 0.012 (2σ, RSD = 4.6%), our results exhibit comparable accuracy but improved analytical precision. Long-term reproducibility of the GSR-23 standards was better than 0.008 mmol/mol (2σ) over a three-month measurement period. The CAP values for GSR-26, GSR-27, GSR-28, GSR-29, and BCS-CRM 393 are reported here for the first time. This high-precision analytical method enables the identification of subtle variations in P concentrations during carbonate formation and significantly facilitates future investigations into the evolution of marine phosphorus cycling. Download: Download high-res image (133KB) Download: Download full-size image
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DOI
高影响因子
RESEARCH ON CHEMICAL INTERMEDIATES
·
2022
·Vol. 48
·期 6
·2557-2573
·
IF 3.134
Liu Yueyu,Yin Zhili,Wang Ziqing,Mou Ronglin,Wei Zhong
High surface area ZrO 2 –KOH sample was prepared and used the catalyst for the synthesis of glycerol carbonate (GC) from dimethyl carbonate (DMC) and glycerol. The structure properties of ZrO 2 –KOH were characterized by XRD, BET, CO 2 -TPD, XPS, and ICP-OES. It was found that the strong basicity of ZrO 2 –KOH might be attributed to the oxygen vacancies as well as the big surface area. Experiments were developed to evaluate the effects of catalysis loading, proportion of reactants, temperature and reaction time on the conversion of glycerol to GC. The consequences showed that ZrO 2 –KOH was a highly efficient basic catalyst for synthesis of GC from glycerol. The catalytic performance of ZrO 2 –KOH is much better than that of ZrO 2 –KOH–CP, ZrO 2 –NH 4 OH, and some reported heterogeneous catalysts. And the higher performance of ZrO 2 –KOH was ascribed to the strong basicity. 99.43% conversion was obtained in a particular situation of catalyst/glycerol weight ratio of 3 wt%, DMC/glycerol molar ratio of 3:1, reaction temperature of 80 °C, and reaction time of 2 h. The plausible reaction mechanism for the transesterification on the strong basic active sites was discussed.
研究领域:
催化
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化学工程
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材料科学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）