ANALYTICA CHIMICA ACTA
·
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
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产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2025
·
IF 6
Xue-lin Dong,Jun-han Liu,Zheng-xun Jia,Shao-zhan Tang,Shuo-yun Tong,Yu-xiang Xiong,Lei Ouyang
Background The quantification of rare earth elements (REEs) in barite-associated geological samples is complicated by persistent matrix effects from coexisting elements and overlapping mass spectral interferences. These analytical challenges are particularly pronounced in samples containing high concentrations of light REEs (LREEs), which induce spectral overlaps on heavy REEs (HREEs) during inductively coupled plasma mass spectrometry (ICP-MS) measurements. Results A two-stage precipitation protocol achieved separation efficiencies exceeding 93.0 % for nine matrix elements (Ba, Na, Sr, etc.), while subsequent 717-type anionic resin chromatography enabled group separation of REEs. Sequential elution with methanol-nitric acid (3.40 mol/L, 7:3 v/v) and 0.20 mol/L nitric acid solutions yielded distinct recovery profiles: HREEs (Eu–Lu) showed >90.0 % recovery in the first elution phase, followed by quantitative isolation of LREEs (La, Ce, Pr) in the second phase. The method was verified by using certified reference materials (GBW07892, GBW07893), and the determination results were consistent with the certified values. The application to three natural barite-associated REE ores was also realized. Significance This methodology resolves critical limitations in REE analysis through matrix element elimination and controlled LREE/HREE fractionation. The demonstrated 90.2–106.9 % recovery range across all REEs confirms operational robustness, while successful implementation in certified materials and field samples establishes reliability for geochemical characterization. The elution sequence optimization provides a template for analyzing REEs in barite-associated ores.
研究领域:
地球化学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2012
·
IF 3.048
Yi Wu,Yong-Ill Lee,Li Wu,Xiandeng Hou
A simple method was proposed for mercury cold vapor generation (CVG) in tetramethylammoniumhydroxide (TMAH) solution for speciation analysis of ultratrace inorganic mercury and total mercury in biological samples by inductively coupled plasma mass spectrometry (ICP-MS). Prior to analysis, 100–300 mg of the biological sample was accurately weighed into a conical tube. Then, 2 mL of 25% (m/v) TMAH solution was added to the sample, incubated at room temperature for several hours (hair, 3 h), and diluted to 25 mL with water. Finally, inorganic mercury was directly determined by CVG-ICP-MS, while microwave-assisted oxidation with H 2 O 2 was needed for total mercury detection. The concentration of organic mercury, mainly methylmercury , was obtained by difference of total mercury and inorganic mercury. Only one calibration curve against mercury aqueous standards in 2% TMAH medium was needed for both procedures. Optimum conditions for mercury CVG, as well as sample preparation and microwave-assisted digestion were investigated in detail. A limit of detection (LOD, 3σ) of 3 ng L − 1 was obtained and the linear working range was 0.1–100 μg L − 1 . Validation data were provided based on the analysis of water samples, as well as a CRM human hair sample (GBW 070601). This is a simple, rapid, ultrasensitive and relatively green method for the determination of mercury in water and biological samples.
研究领域:
分析化学
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环境科学
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生物学
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DOI
高影响因子
Food Analytical Methods
·
2021
·Vol. 14
·期 11
·2420-2429
·
IF 3.366
Cao Jinping,Cheng Yuanzhi,Xu Bocheng,Wang Yizhen,Wang Fengqin
To ensure reasonable intake of selenium for humans and provide insights on the development and nutritional analysis of high-quality selenium-enriched food, we established a reliable and highly sensitive method for the determination of selenium species in Z0206 selenium-enriched polysaccharide (Se-EPS). By optimizing the pre-treatment conditions (different enzymes, enzyme combinations, enzymatic time, concentration of enzymes, and centrifugation time), we found that Se-EPS can be effectively hydrolyzed by proteinase K for 18 h, followed by HPLC-ICP-MS determination. The developed method presented high sensitivity with the limit of detection and quantitation in the range of 0.44–2.35 μg L −1 and 1.54–7.21 μg L −1 . The relative standard deviation (RSD) was all less than 10% and recovery was greater than 80% except for SeCys2, which further validated the repeatability and accuracy of the proposed method. Under the optimized conditions, we could determine 4 selenium species: elemental selenium (78.37%), seleno-methionine (14.27%), selenocystine (0.03%), and Se-methylselenocysteine (5.22%) in Se-EPS. This work provides new insights into the determination of different selenium species in selenium-enriched food.
研究领域:
分析化学
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营养科学
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食品科学
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产品关联
DOI
高影响因子
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
·
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
✓ 已验证
DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2021
·
IF 6.986
Xiuhong Liao,Zhaochu Hu,Wen Zhang,Yantong Feng,Tao Luo,Zaicong Wang,Ming Li,Keqing Zong,Yongsheng Liu,Shenghong Hu
Using boron as a test analyte, laser ablation (LA) solution sampling multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is proposed and validated as a fast method for isotopic analysis in natural liquids and digested samples without any prior purification process. We demonstrated that the solution reference standard can be used as a bracketing standard for in situ δ11B analysis in solids. Based on a sensitivity enhancement of 8- to 9-fold, all testing solutions were diluted in a 5% (v/v) NH3·H2O instead of classical 2% (v/v) HNO3. With a discrete and minimal sample solvent loading by the LA sampling strategy, it produces nearly “dry” plasma conditions that tolerate the sample matrix remarkably. The memory effect, one of the most difficult challenges in boron analysis, was dramatically eliminated with only 15 s wash time; thus, each analysis took less than 100 s. No significant matrix effects were observed for varying 50–100% boron concentrations in the samples and varying 20–60% NH3·H2O matrix used for the dilution, as well as for samples doped with a 1/100 synthetic seawater matrix. The external precision of δ11B measurements in NIST 951a was ± 0.30‰ (2SD). Good agreement with the values described in literature studies was achieved for δ11B measurements in eight geological reference materials, with precisions between 0.4 and 0.7‰ (2SD), confirming the accuracy of the proposed method. The proposed method offers advantages of simple sample preparation, fast analysis, and little use of chemical reagents.
研究领域:
地球化学
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分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
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2024
·
IF 3.1
Qinyuan Qu,Wengang Liu,Wang Zheng,Benjamin Chetelat,Qingchuan Liu,Jiubin Chen
The geological and environmental applications of tin (Sn) isotopes have been hindered by the shortcomings of chemical purification, as severe loss of Sn would occur during sample preparation (evaporation and re-dissolution) and column separation, triggering isotope measurement bias. In this study, we develop a novel and robust separation method to purify Sn from natural samples for accurate isotope measurements. The protocol is established by combining two chromatographic columns loaded with AG 1-X8 and AG 50W-X12 resins, and optimizing the sample evaporation and re-dissolution procedures. The method is proven to efficiently eliminate the main interferents such as Ag, Zn, Mo, Cd and Sb and results in low procedural blank (0.54 ± 0.21 ng, n = 3), quantitative recovery (95–102%, n = 32) and good external precision (δ120Sn of 0.02–0.04‰, in 55 measurements) for isotope measurement. The protocol is further applied to seven geological and environmental reference materials (BCR-2, BHVO-2, AGV-2, JG-2, AC-E, PACs-2 and GSS 7) and new values are reported for both odd (δ119Sn and δ117Sn) and even (δ120Sn and δ122Sn) Sn isotope ratios. This study demonstrates clearly the potential application of our method for studying the geochemical behaviors of Sn and its isotopes in various aspects.
研究领域:
地球化学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
MARINE CHEMISTRY
·
2019
·
IF 2.713
Yuxi Lu,Xuelu Gao,Chen-Tung Arthur Chen
In this study, a method was developed for the desalination and pre-concentration of three colloidal trace metals in seawater , namely Cd, Cu and Pb, using diethylammonium diethyldithiocarbamate and ammonium 1-pyrrolidine dithiocarbamate as chelates. Seawater samples were first treated with cross-flow ultrafiltration (CFUF) for the separation of the colloidal matter of different molecular weights , i.e. 1–3 kDa, 3–10 kDa and 10 kDa-0.22 μm. Then, after acid digestion , the organic chelates and the extracting agent chloroform were added at pH = 3.8. Finally, the organic phase was back extracted, and the target metals in all samples were measured using inductively coupled plasma mass spectrometry (ICP-MS) with low detection limits in the range of 0.13–1.18 pmol L −1 . The extraction efficiencies for the three metals were in the range of 92.2%–100.3% with an enrichment factor of 40, and their mass recoveries in the studied colloidal fractions were in the range of 83.1%–103.5%. The developed method has been successfully applied for the analysis of seawater samples collected from the sites off the south coast of North Yellow Sea in Shandong Peninsula , China. For the first time, the distribution of colloidal Cd, Cu and Pb in different molecular weights in this area is reported. The results obtained from real samples demonstrate that the developed method is simple, efficient and convenient for routine analysis with low detection limit.
研究领域:
海洋化学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
Micromachines
·
2024
·Vol. 15
·期 4
·460
·
IF 3
Yu Wu,Xianshan Dong,Xuefang Wang,Junfeng Xiao,Quanquan Sun,Lifeng Shen,Jie Lan,Zhenfeng Shen,Jianfeng Xu,Yuqingyun Du
In this paper, we proposed an efficient and high-precision process for fabricating large-area microlens arrays using thermal reflow combined with ICP etching. When the temperature rises above the glass transition temperature, the polymer cylinder will reflow into a smooth hemisphere due to the surface tension effect. The dimensional differences generated after reflow can be corrected using etching selectivity in the following ICP etching process, which transfers the microstructure on the photoresist to the substrate. The volume variation before and after reflow, as well as the effect of etching selectivity using process parameters, such as RF power and gas flow, were explored. Due to the surface tension effect and the simultaneous molding of all microlens units, machining a 3.84 × 3.84 mm2silicon microlens array required only 3 min of reflow and 15 min of ICP etching with an extremely low average surface roughness Sa of 1.2 nm.
研究领域:
微纳米技术
·
光学工程
·
材料科学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Jinhui Liu,Jiasen Cui,Xing Wei,Weitao Li,Chunran Liu,Xuewen Li,Mingli Chen,Yu Fan,Jianhua Wang
It is the first time to investigate local distribution patterns of mercury (Hg) in mice organs after Hg and Se exposure with detection of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Two batch of adult mice were employed to be exposed to inorganic mercury (iHg) and methylmercury (MeHg) with or without Se at the dose of 55 μmol kg −1 . Tissue sections of brain, kidney, liver, and spleen from one batch mice were prepared to get local imaging of Hg by LA-ICP-MS. Tissues from another batch mice were used to quantify Hg and Se in tissues with ICP-MS after acid digestion . The results indicated that, for mice exposed to iHg, Hg mainly distributed in kidney, a little in liver, and hardly in brain and spleen; for mice exposed to MeHg, lower amount of Hg was found in kidney, liver and spleen, and almost no Hg was found in brain. It was interesting that for Hg and Se co-administration groups, higher level of Hg was observed in kidney, liver, spleen and even in brain than single Hg administration groups. In addition, Se level in organ tissues increased obviously not only in Se exposure group but also in MeHg exposure group, while the phenomenon was not observed in iHg exposure group. HepG2 cells were employed to investigate Se and Hg interactions in single cell level, similar bioaccumulation behavior of Hg was found between cells and mice organs. Higher level of Hg was observed in cells cultured with Se and Hg medium than cells cultured with single Hg medium. The results are expected to provide new insight to investigate Hg and Se interactions in animal bodies and in-vitro cells.
研究领域:
环境科学
·
毒理学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2021
·
IF 6.986
Lin-Hui Dong,Wei Wei,Cheng-Long Yu,Zhen-Hui Hou,Zhen Zeng,Tianyu Chen,Fang Huang
Vanadium isotope compositions (δ(51V)) in marine carbonates are a potential proxy to trace global redox states of ancient oceans. Although high-precision δ(51V) analyses are available for many geological materials, carbonate-hosted δ(51V) data have not been reported yet due to extremely high matrix elements and low V contents (generally below 10 μg g–1). In this study, we developed an Fe coprecipitation method combined with an Fe column to preconcentrate V from the major matrix elements and subsequent four-step chromatographic procedures to further purify V in carbonates. The δ(51V) values were measured using a sample–standard bracketing method by MC-ICP-MS. The robustness of this method was assessed by analyzing element-doped and matrix-spiked synthetic carbonate solutions containing an in-house δ(51V) standard, USTC-V. The mean δ(51V) value of the synthetic carbonate solutions (0.06 ± 0.08‰; 2SD, n = 33) is in good agreement with the recommended value of the USTC-V relative to the Oxford AA solution (0.07 ± 0.08‰; 2SD, n = 347). In addition, the consistency in the δ(51V) value of the igneous carbonatite standard, COQ-1, which was processed in parallel with the whole purification (−0.48 ± 0.04‰; 2SD, n = 3) and a four-step chromatographic procedure (−0.43 ± 0.08‰; 2SD, n = 3), further validates the robustness of our method. For the first time, we obtained δ(51V) values of four carbonate reference materials: JDo-1, −0.56 ± 0.09‰ (2SD, n = 27); JLs-1, −0.61 ± 0.14‰ (2SD, n = 33); GBW07217a, −0.79 ± 0.09‰ (2SD, n = 6); GBW07214a, −0.51 ± 0.13‰ (2SD, n = 48). The long-term external precision of carbonate-hosted δ(51V) analyses is better than ±0.14‰ (2SD). Our method can be applied to measure carbonate-hosted δ(51V) to trace the evolution in global marine redox states throughout the Earth’s history.
研究领域:
地球化学
·
海洋科学
✓ 已验证
DOI
PubMed
高影响因子
BIOSENSORS & BIOELECTRONICS
·
2017
·
IF 7.78
Bin Yang,Yuan Zhang,Beibei Chen,Man He,Xiao Yin,Han Wang,Xiaoting Li,Bin Hu
Inductively coupled plasma-mass spectrometry (ICP-MS) based bioassay and multimodal imaging have attracted increasing attention in the current development of cancer research and theranostics. Herein, a sensitive, simple, timesaving, and reliable immunoassay for cancer cells counting and dual-modal imaging was proposed by using ICP-MS detection and down-conversion fluorescence (FL)/upconversion luminescence (UCL) with the aid of a multifunctional probe for the first time. The probe consisted of a recognition unit of goat anti-mouse IgG to label the anti-EpCAM antibody attached cells, a fluorescent dye (Cy3) moiety for FL imaging as well as upconversion nanoparticles (UCNPs) tag for both ICP-MS quantification and UCL imaging of cancer cells. Under the optimized conditions, an excellent linearity and sensitivity were achieved owing to the signal amplification effect of nanoparticles and low spectral interference. Accordingly, a limit of detection (3σ) of 1×10 2 HepG2 cells and a relative standard deviation of 7.1% for seven replicate determinations of 1×10 3 HepG2 cells were obtained. This work proposed a method to employ UCNPs with highly integrated functionalities enabling us not only to count but also to see the cancer cells, opening a promising avenue for biological research and clinical theranostics.
研究领域:
分析化学
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生物医学工程
·
肿瘤学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）