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Rapid determination of mercury in dust emission using Cold Vapour Inductively Coupled Plasma Optical Emission Spectrometer (CV ICP OES)
摘要： Mercury emissions generated by the human activities were ranged between 60% and 90% from total mercury content determined in some industrialised regions. It is well known that urban dust has adverse health effects, being related to respiratory diseases. In this study, Cold Vapour Inductively Coupled Plasma Optical Emission Spectrometer (CV ICP OES) was optimised, validated, and applied in routine analysis for the determination of vapour mercury in dust emission samples collected from different Egyptian cement plants. The estimated detection limit, practical quantification limit, linearity (linear dynamic ranges and method linearity), accuracy (trueness and precision), and measurement uncertainty parameters were studied under optimised (CV ICP OES) conditions. The method showed that the estimated detection limit was found to be equal to 0.12 μg/L, and the quantification limit was found to be equal to 0.5 μg/L. The mean recoveries ± standard deviations at different levels were varied between 88.60 ± 8.18 and 110.20 ± 5.93% with a coefficient of variation expressed as relative standard deviation ranged from 0.64 and 7.25%. The method trueness was confirmed by using four different certified references materials purchased from Food Analysis Performance Assessment Scheme (FAPAS) and all obtained results were within satisfactory ranges and had acceptable recovery and Z-score values. The method precision, in terms of relative standard deviation (RSD), was being below 7.74%. The method uncertainty expressed as expanded uncertainty was found to be ≤ 16.11%. The results obtained make the method suitable for accurate determination of vapour mercury in dust emission samples at low concentration. The validated method was used for the determination of mercury in fifty-eight dust emissions samples and the results were compared with the maximum limit stated by European standard on the incineration of waste.
关键词： CV ICP OES,cement plants,mercury,Method validation,Egypt
更新于2025-09-19 17:13:59
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Direct Determination of Ni2+-Capacity of IMAC Materials Using Near-Infrared Spectroscopy
摘要： The present paper reports a new method for the quanti?cation of the Ni2+-capacity of an immobilized metal af?nity chromatography (IMAC) material using near-infrared spectroscopy (NIRS). Conventional analyses using UV absorption spectroscopy or atomic absorption spectrometry (AAS) need to dissolve the silica-based metal chelate sorbent as sample pretreatment. In the ?rst step, those methods were validated on the basis of an ideal homogenous NiSO4-solution and unveiled that UV with an intermediate precision of 2.6% relative standard deviation (RSD) had an advantage over AAS with an intermediate precision of 6.5% RSD. Therefore, UV analysis was chosen as reference method for the newly established NIRS model which has the advantage of being able to measure the material directly in diffuse re?ection mode. Partial least squares regression (PLSR) analysis was used as multivariate data analysis tool for quanti?cation. The best PLSR result obtained was: coef?cient of determination (R2) = 0.88, factor = 2, root mean square error of prediction (RMSEP) = 22 μmol/g (test-set validation) or 7.5% RSDPLSR. Validation of the Ni2+-capacity using UV absorption spectroscopy resulted in an intermediate precision of ±18 μmol/g or 5.0% RSD. Therefore, NIRS provides a fast alternative analysis method without the need of sample preparation.
关键词： Ni2+-capacity,partial least squares regression,IMAC,near-infrared spectroscopy,method validation
更新于2025-09-09 09:28:46
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VALIDATION STUDY OF STEROIDAL DRUGS (DEXAMETHASONE AND BETAMETHASONE) BY U.V. SPECTROPHOTOMETRIC METHOD
摘要： Objective: The present investigation involves development and validation of ultraviolet (UV) spectroscopic method for estimation of dexamethasone and betamethasone in a pharmaceutical dosage as per International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines. Method: Betamethasone and dexamethasone were dissolved in 50 mL Methanol: water (1:2) and 50 mL distilled water, respectively. The method was validated for accuracy, precision, linearity, ruggedness, and robustness to check its consistency. Result: The λmax or the absorption maxima of both the drugs was found to be 241 nm. A linear response was observed in the range of 10–20 μg/mL. Conclusion: The method could be applied for the analysis of marketed tablets and also can be used for the routine analysis of dexamethasone and betamethasone in bulk formulations using UV method. It is suitable for the intended purpose especially in forensic science laboratories and other laboratories involved in the pharmaceutical analysis.
关键词： Accuracy,Method validation,Betamethasone,Precision,Dexamethasone,Ultraviolet spectroscopy
更新于2025-09-04 15:30:14