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
·
环境科学
✓ 已验证
DOI
高影响因子
Journal of Marine Science and Engineering
·
2022
·Vol. 10
·期 1
·93
·
IF 2.744
Yuhua Gao,Xiaoyuan Wang,Xianwen Fang,Xuebo Yin,Lu Chen,Jianling Bi,Yao Ma,Shuai Chen
Fluorine and chlorine are important tracers for geochemical and environmental studies. In this study, a rapid alkaline digestion (NaOH) method for the simultaneous determination of fluorine and chlorine in marine and stream sediment reference samples using ion chromatography is developed. The proposed method suppresses the volatilization loss of fluorine and chlorine and decreases the matrix effects. The results are in good agreement with fluorine ~100%, chlorine ranging from 90 to 95% of the expected concentrations. The detection limits of this method were 0.05 μg/g for fluorine and 0.10 μg/g for chlorine. This method is simple, economical, precise and accurate, which shows great potential for the rapid simultaneous determination of fluorine and chlorine in large batches of geological and environmental samples commonly analyzed for environmental geochemistry studies.
研究领域:
地球化学
·
环境科学
✓ 已验证
DOI
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2018
·Vol. 42
·期 3
·309-318
·
IF 3.929
Tao He,Junyi Xie,Zhaochu Hu,Ting Liu,Wen Zhang,Haihong Chen,Yongsheng Liu,Keqing Zong,Ming Li
Bromine and iodine are important tracers for geochemical and environmental studies. In this study, a rapid acid digestion (HNO 3 + HF) with ammonia dilution for the simultaneous determination of bromine and iodine in soils and sediments using ICP-MS was developed. The recoveries of Br and I were controlled by the synergic effect of temperature and time. It took only 15 min at 140 °C for the complete recovery of Br and I in sediment (GSD-2) and soil (GSS-24) reference materials, which is a process that needs 2–6 h at 90 °C. A serious loss of Br and I was found at a higher digestion temperature of 190 °C. A 5% v/v NH 4 OH dilution effectively eliminated the memory effects and stabilised the signals of Br and I. Moreover, ammonia dilution also avoided the corrosiveness of HF on the sample introduction system and torch of ICP-MS. Tellurium is a more suitable internal standard element than In in the ammonia medium. To avoid the adsorption of residues of dissolution on Te, addition of Te should be carried out after centrifuging the solution. The developed method was successfully applied to determine Br and I in fifty-three Chinese soil and sediment reference materials. This simple method shows great potential for the rapid determination of Br and I in large batches of geological and environmental samples commonly analysed for mineral exploration and environmental geochemistry studies.
研究领域:
环境科学
·
地球化学
✓ 已验证
产品关联
DOI
高影响因子
Journal of Analytical Methods in Chemistry
·
2024
·
IF 2.3
Yajie Hao,Guang Yin,Xuemei Wang,Juan Fu,Qihui Cao,Qinyong Sun,Guimin Zhang,Zhong Feng
Rosuvastatin calcium is a widely used 3-hydroxy-3-methylglutaryl coenzyme A-reductase inhibitor developed for the treatment of dyslipidemia. To establish a control strategy for the elemental impurities, a new digestion method combined with an inductively coupled plasma-mass spectrometer (ICP-MS) was developed and validated by our team to determine elements Cd, Pb, As, Hg, Co, V, and Ni in rosuvastatin calcium tablets, which digest the sample perfectly even in the presence of a large number of excipients, especially titanium dioxide. The measurement mode was collision cell mode with kinetic energy discrimination (KED). 209Bi+, 115In+, and 89Y+ were chosen as internal standard elements. The recoveries of the limit of quantitation (LOQ) ranged from 90.5% to 106.4%, concentrations of the abovementioned elements in LOQ were 0.25 µg·L−1, 0.25 µg·L−1, 0.75 µg·L−1, 1.5 µg·L−1, 2.5 µg·L−1, 5 µg·L−1, and 8 µg·L−1 , respectively, linear correlation coefficients were above 0.9997, the recoveries in accuracy item ranged from 91.8% to 103.6%, and relative standard deviations (RSDs) of recovery in precision were not more than 1.8%, reflecting a reliable method of high sensitivity, strong anti-interference capacity, and good precision, and that it was suitable for the determination of elemental impurities in drugs.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
WATER AIR AND SOIL POLLUTION
·
2020
·Vol. 231
·期 12
·1-13
·
IF 1.9
Rao Jifa,Chen Ling,Xiang Yujia,Li Jiayu,Chen Xiao,Zhou Yaoyu
In this study, a practical and excellent method was used to determine the famoxadone and cymoxanil via high-performance liquid chromatography equipped utilizing ultraviolet detector lamp (HPLC-UV) for investigating the dissipation behavior and residue distribution of famoxadone and cymoxanil in cucumber and soil ecosystem. The limit of quantification (LOQ S ) of famoxadone and cymoxanil in cucumber were 0.50, 1.00, 2.00 and 0.05, 0.50, 1.00 mg kg −1 in soil, respectively. The limit of detection (LOD S ) of both famoxadone and cymoxanil were 8.0 ng. The average recoveries ( n = 5) of the fungicide ranged from 84.10 to 108.02% with the relative standard deviations (RSDs) typically < 9.23%. The fungicide was applied to cucumber and soil at the range of doses (275.6–413.4 g a.i.ha −1 ) three or four times. The half-lives of famoxadone and cymoxanil in cucumber and soil were 1.34–16.12 days, which followed the first-order chemical reaction kinetics equation C t = C 0 × e -kt . The residues of famoxadone and cymoxanil in cucumber at the pre-harvest interval (PHI, 3 days) were below 8.0 × 10 −8 g and 8.0 × 10 −9 g, respectively. Overall, this study evaluated the food safety and the environmental fate of famoxadone and cymoxanil in cucumber and soil ecosystem. In addition, this study would promote the series of work on the pesticide exposure assessment of these fungicides as well.
研究领域:
农业科学
·
环境科学
✓ 已验证
DOI
高影响因子
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
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2013
·Vol. 38
·期 1
·37-50
·
IF 2.77
Jie Li,Xiao-Ying Jiang,Ji-Feng Xu,Li-Feng Zhong,Xuan-Ce Wang,Gui-Qin Wang,Pei-Pei Zhao
en This link goes to a English section fr This link goes to a French section We report an improved procedure for the determination of the platinum-group elements (PGE) and Re, and Os isotopes from a single sample aliquot by isotope dilution (ID) using inductively coupled plasma-mass spectrometry (ICP-MS) and negative thermal ionisation mass spectrometry (N-TIMS), respectively. A two-stage column method was used to purify PGE-Re from their sample matrix and interfering elements (e.g., Mo, Zr and Hf) after Os had been separated by CCl 4 solvent extraction. The first column separation step used cation exchange resin (AG50W-X8) to concentrate PGE-Re and some potential interfering elements (e.g., Mo, Zr and Hf). In the second step, N -benzoyl- N -phenylhydroxylamine (BPHA) extraction resin was used to separate PGE-Re from the remaining interfering elements, which all remained strongly absorbed to the resin. The method was used to determine the PGE and rhenium, and Os isotope ratios in a range of geochemical reference materials (TDB-1, WGB-1, BHVO-2 and UB-N). The obtained results agree well with those previously published. This new method enables PGE-Re abundances and Os isotopic ratios to be determined on the same sample digestion, and circumvents the problems created by sample heterogeneity when comparing PGE and Re-Os isotope data. en This link goes to a English section fr This link goes to a French section Nous décrivons une procédure améliorée pour la détermination des abondances des éléments du groupe du platine (EGP), du Re et des isotopes de l'Os à partir d'un même aliquot d'échantillon par dilution isotopique (ID) en utilisant respectivement la spectrométrie de masse à source plasma (ICP-MS) et la spectrométrie de masse par ionisation thermique négative (N-TIMS). Une méthode sur colonne en deux étapes a été utilisé pour purifier les EGP et le Re de la matrice de l'échantillon et des éléments interférents (par exemple, Mo, Zr et Hf) et ceci après que l'Os ait été séparé par extraction par solvant CCl 4 . La première étape de séparation sur colonne utilise une résine échangeuse de cations (AG50W-X8) pour concentrer les EGP et le Re et certains éléments interférents potentiels (par exemple, Mo, Zr et Hf). Au cours de la seconde étape, la résine d'extraction N-benzoyl-N-phénylhydroxylamine (BPHA) a été utilisée pour séparer les EGP et le Re des éléments interférents restants, qui sont tous fortement absorbé par cette résine. La méthode a été utilisée pour déterminer les concentrations en PGE et Re, et les rapports isotopiques de l'Os dans une gamme de matériaux de référence géochimiques (TDB-1, WGB-1, BHVO-2 et UB-N). Les résultats obtenus sont en bon accord avec ceux publiés antérieurement. Cette nouvelle méthode permet la détermination des abondances en PGE et Re et des rapports isotopiques de l'Os sur la même portion d'échantillon digérée, et contourne ainsi les problèmes liés à l'hétérogénéité des échantillons lorsqu'on compare les données élémentaires des EGP et les données isotopiques Re-Os.
研究领域:
地球化学
·
分析化学
✓ 已验证
DOI
高影响因子
International Journal of Analytical Chemistry
·
2019
·
IF 1.682
Mingbo Ma,Pirah Ayaz,Wanhui Jin,Munir Hussain,Wenlong Zhou
Defoliants carried by cotton fiber could harm production workers and consumers through respiratory and dermal exposure. This study was carried out to evaluate the dissipation behavior of four commonly used defoliants tribufos, diuron, thidiazuron, and ethephon in cotton fiber during field stage and also in cotton scouring using liquid chromatography and gas chromatography. Field trials showed that although all the defoliants dissipated fast, however, the fiber from the tribufos and ethephon applied field had considerable potential to exceed the maximum residue limit when the fiber was harvested at common intervals after application of defoliants. The defoliant residues could be removed completely from the defoliant-carrying cotton textiles during alkaline scouring. The results indicated that attention should be paid to the risk of occupational exposure to these defoliants rather than consumer exposure. Fiber harvest on the tribufos and ethephon applied fields is recommended after a 1-week delay in order to reduce the residues to an acceptable level.
研究领域:
农业科学
·
环境科学
✓ 已验证
DOI
PubMed
高影响因子
International Journal of Electrochemical Science
·
2023
·
IF 1.5
Hua Feng,Min Hu,Qunying Xu,Zhongwei Zhang,Yongning Wu
Currently, a large amount of harmful heavy metals is discharged into the soil environment, which will eventually affect the quality of food and harm human health through the food chain. Therefore, it is of great theoretical and practical significance to establish an analytical method for the determination of trace heavy metals in food. In this paper, a differential pulse stripping voltammetric method for the determination of chromium in food was established, and the sample was pretreated with a wet digestion method suitable for rapid detection in the field. Finally, this HNO 3 -H 2 O 2 wet digestion electrochemical determination method was evaluated.
研究领域:
分析化学
·
环境科学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2019
·
IF 6.35
Tao He,Zhaochu Hu,Wen Zhang,Haihong Chen,Yongsheng Liu,Zaicong Wang,Shenghong Hu
In this study, a simple and effective method for the simultaneous analysis of Cl, Br, and I in geological materials based on NH4HF2 digestion in open vessels (Savillex Teflon vials) is proposed. It is very interesting to note that Cl, Br, and I are not lost during NH4HF2 digestion at temperatures of 200–240 °C for 0.5–12 h in open vessels. This should be related to the alkaline atmosphere environment caused by the NH3 produced during NH4HF2 digestion, which suppresses the volatilization loss of Cl, Br, and I. A 100 mg sample of geological materials can be completely digested by using 400 mg of NH4HF2 at 220 °C for 2 h in Savillex Teflon vials. The use of new Savillex Teflon vials significantly reduced the procedural blanks of halogens compared with the old Savillex Teflon vials. The developed method was successfully applied to the simultaneous determination of Cl, Br, and I in a series of international geological reference materials. Most of the results were found to be in reasonable agreement with values reported in the literature. This simple, rapid, effective, and economical analytical method will significantly promote the development of halogen geochemistry.
研究领域:
地球化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Shanshan Di,Yunye Xie,Tao Cang,Zhenzhen Liu,Yanyan Chu,Huiyu Zhao,Peipei Qi,Zhiwei Wang,Xinquan Wang
A comprehensive evaluation of chiral pesticide at the stereoisomeric level is an effective strategy to improve efficiency and reduce risk on foods. For chiral sedaxane with four stereoisomers , there were 517–1013 fold differences in bioactivity for three kinds of phytopathogens and 3.73 fold differences in toxicity against model organism ( Danio rerio ) between the best ( trans -1 R 2 S -sedaxane) and worst stereoisomer ( cis -1 S 2 S -sedaxane). Trans -1 R 2 S -sedaxane had the strongest affinity with the active site than other stereoisomers, which might contribute to the highest bioactivity. Trans -sedaxane was 28.2–331 fold more effective than cis -sedaxane. The dissipation half-lives of sedaxane stereoisomers ranged from 3.28 to 30.7 d in the test crops and soils. Trans -1 S 2 R -sedaxane and cis -1 S 2 S -sedaxane were preferentially dissipated in corn plants, while the preferential dissipation of trans -1 R 2 S -sedaxane was found in wheat plants, potato plants and corn soil. The preferential dissipation of trans -sedaxane in corn plants, wheat plants, potato plants and corn soil would be environmentally friendly.
研究领域:
环境科学
·
植物保护
·
毒理学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2024
·
IF 1.6
Chunli Fan,Mingying Cao,Qiuju Zheng,Youfa Cheng,Ping Wang,Jinyu Feng
The evaluation of the flow direction of platinum group elements (PGEs) during gold-copper ore mining is challenging due to the uneven distribution and low content. Therefore, it is vital to accurately and simultaneously determine ultra-trace PGEs Pt, Pd, Rh, and Ir in gold mining residue samples. In this study, a method to simultaneously determine ultra-trace Pt, Pd, Rh, and Ir in gold mining residue is reported using Sb–Cu fire assay, microwave digestion, and inductively coupled plasma-mass spectrometry (ICP-MS). The Sb–Cu fire assay was used to enrich Pt, Pd, Rh, and Ir, obtaining Sb–Cu alloy particles that concentrate these elements. An optimal microwave method was employed to digest the Sb–Cu alloy particles. In ICP-MS, the collision reaction interface was used to eliminate the interferences of other elements and improve the accuracy. Moreover, the matrix-matched multi-external standards combined with internal standard calibration were utilized to reduce the error. High concentrations of Au, Ag, and Pb showed no interferences with Pt, Pd, Rh, or Ir determination. The limits of detection for Pt, Pd, Rh, and Ir were 0.018, 0.052, 0.064, 0.035 ng·g−1, respectively, and the relative standard deviation was 5.18, 4.66, 1.55, and 3.17%. Additionally, the determination of Pt, Pd, Rh, and Ir in standard reference materials showed good agreement with the certified values. In summary, a reliable and efficient method is provided to determine various PGEs which is of great significance for gold-copper ore mining.
研究领域:
分析化学
·
矿物加工工程
·
地质学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）