• Analytical Science and Technology
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• v.37 no.4
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• pp.211-219
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• 2024

This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R² > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

• Analytical Science and Technology
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• v.9 no.1
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• pp.72-77
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• 1996

In the process of solar energy conversion into electrical energy using the photoelectrochemical cell containing the sensitizer, rose bengal and supersensitizer. $I^-$, the photocurrent is stabilized and durable. But the long time span of irradiation causes the decrease of photocurrent monotonically. Spectroscopic and electrochemical analyses of rose bengal solution containing $I^-$ revealed that the decrease of concentration of rose bengal was attributed to the reaction of rose bengal in the dark with $I_2$ formed as a result of the possible photocatalytic reaction of rose bengal with $I^-$.

• Analytical Science and Technology
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• v.11 no.4
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• pp.311-315
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• 1998

Ultra trace metal impurities of high-purity sulfuric acid for semiconductor process have been determined in the concentration of lower than ppb (ng/g) level using high resolution inductively coupled plasma mass spectrometer (HR-ICP-MS).The acid samples were evaporated and concentrated by the factor of 20. No clement in the acids exceeded 1ppb level and most of the clements were determined below 10ppt (pg/g). Elements without spectral interference in mass spectrum, such as In, V, Mn, etc, were determined in the concentration of below 1 ppt level The recoveries in the range of 72% to 127.2% for 0.5 ppb spiked sample were obtained.

• Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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• 2001.06a
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• pp.1081-1081
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• 2001

The constant need for quality improvement and production rationalization in the chemical and related industries has led to the increasing replacement of conservative control procedures by more specific and environmentally compatible analytical techniques. In this respect, vibrational spectroscopy has developed over the last yews - in combination with new instrumental accessories and statistical evaluation procedures - to one of the most important analytical tools for industrial chemical quality control and process monitoring in a wide field of applications. In the present communication this potential is demonstrated in order to further support the implementation of mid-infrared (MIR), near-infrared (NIR) and Raman spectroscopy Primarily as industrial on-line tools. To this end the data of selected feasibility studies will be discussed in terms of the individual strengths of the different techniques for the respective application.

• Analytical Science and Technology
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• v.13 no.3
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• pp.291-296
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• 2000

The SIMFUEL which composition is similar to PWR nuclear spent fuels was dissolved with a acid digestion bomb. An analytical conditions of ICP-AES for the direct determination of molybdenum in the uranium matrices without separation process were investigated. Based on the effect of uranium on molybdenum intensity. the most optimum wavelengths of molybdenum were found to be 202.030 and 203.844 nm. However, the method of standard additions is applied to overcome the effects of changing background caused by analyzing the sample solutions containing high concentration of uranium and the standard calibration solutions. The relative error of two methods, direct and indirect measurements with cation exchange resin separation procedures, was less than 5%. Therefore it was possible for this procedure to directly measure molybdenum in uranium matrices without separation. And this method was also applied to the determination of several percent of molybdenum in a U-Mo alloy.

• Korean Journal of Clinical Laboratory Science
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• v.39 no.1
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• pp.31-36
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• 2007

The purpose of the clinically reportable range (CRR) in clinical chemistry is to estimate linearity in working range. The reportable range includes all results that may be reliably reported, and embraces two types of ranges: the analytical measurement range (AMR) is the range of analyte values that a method can directly measure on the specimen without any dilution, concentration, or other pretreatment not part of the usual assay process. CAP and JCAHO require linearity on analyzers every six months. The clinically reportable range is the range of analyte values that a method can measure, allowing for specimen dilution, concentration, or other pretreatment used to extend the direct analytical measurement range. The AMR cannot exceed the manufacturer's limits. Establishing AMR is easily accomplished with Calibration Verification Assessment and experimental Linearity. For example: The manufacturer states that the limits of the AST on their instrument are 0-1100. The lowest level that could be verified is 2. The upper level is 1241. The verified AMR of the instrument is 2-1241. The lower limit of the range is 2, because that is the lowest level that could be verified by the laboratory. The laboratory could not use the manufacturer's lower limit of 2 because they have not proven that the instrument values below 2 are valid. The upper limit of the range is 1241, because although the lab has shown that the instrument is linear to 1241, the manufacturer does not make that claim. The laboratory needs to demonstrate the accuracy and precision of the analyzer, as well the validation of the patient AMR. Linearity requirements have been eliminated from the CLIA regulations and from the CAP inspection criteria, however, many inspectors continue to feel that linearity studies are a part of good lab practice and should be encouraged. If a lab chooses to continue linearity studies, these studies must fully comply with the calibration/calibration verification requirements of CLIA and/or CAP. The results of lower limit and upper limit of clinically reportable range were total protein (2.1 - 79.9), albumin (1.3 - 39), total bilirubin (0.2 - 106.2), alkaline phosphatase (13 - 6928.2), aspartate aminotransferase (24 - 7446), alanine aminotransferase (13 - 6724.2), gamma glutamyl transpeptidase (16.64 - 9904.2), creatine kinase (15.26 - 4723.8), lactate dehydrogenase (127.66 - 13231.8), creatinine (0.4 - 129.6), blood urea nitrogen (8.67 - 925.8), uric acid (1.6 - 151.2), total cholesterol (48.52 - 3162), triglycerides (36.91 - 3367.8), glucose (31 - 4218), amylase (21 - 6694.2), calcium (3.1 - 118.2), inorganic phosphorus (1.11 - 108), HDL (11.74 - 666), NA (58.3 - 1800), K (1.0 - 69.6), CL (38 - 1230).

• Analytical Science and Technology
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• v.18 no.3
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• pp.216-223
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• 2005

In this study, several kinds of volatile amines in ambiant air were collected and their concentrations were expected from the calibration curves prepared by standard solutions of 7 amines by the official measuring method prescribed in Japanese Offensive Odor Law. The obtained calibration curves showed a good linearity and the detection limit of trimethyl amine was found to be about 0.033 ppb (0.040 ng) in case of 50 liters air. It means that trimethyl amine could be detected with the concentration of lower than its permitting level at the border line of companies. As typical examples of measuring amines in air, results of investigation of two sewage works and one rendering plant around the capital area indicated that 4 kinds of amines, i.e. methyl amine, dimethyl amine, trimethyl amine and isopropyl amine were detectable and concentrations of trimethyl amine at the primary sedimentation pond and sludge dewatering building of the sewage plant A showed 9.07 ppb and 7.79 ppb respectively, being over the concentration of odor strength 2.5, And the aeration tank, excrement input facility and indoor of maintenance room of excrement process building in the sewage plant B showed 70.0 ppb of dimethyl amine and 2.44 ppb of trimethyl amine.

• Analytical Science and Technology
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• v.37 no.1
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• pp.63-78
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• 2024

The continuous increasing of the global demand of copper and nickel metals raises the interest in developing alternative technologies to produce them from copper sulfide ore. Also, in line with Egypt's vision 2030 for achieving the sustainable socioeconomic development which aims at developing alternative and eco-friendly technologies for processing the Egyptian ores to produce these strategic products instead of its importing. These metals enhance the advanced electrical and electronic industries. The current work aims at investigating the recovery of copper and nickel from Abu Swayeil copper ore using pug leaching technique by sulfuric acid. The factors affecting the pug leaching process including the sulfuric acid concentration, leaching time and temperature have been investigated. The copper ore sample was characterized chemically using X-ray fluorescence (XRF) and scanning electron microscope (SEM-EDX). A response surface methodology develops a quadratic model that expects the nickel and copper leaching effectiveness as a function of three controlling factors involved in the procedure of leaching was also investigated. The obtained results showed that the maximum dissolution efficiency of Ni and Cu are 99.06 % and 95.30%, respectively which was obtained at the following conditions: 15 % H₂SO₄ acid concentration for 6 hr. at 250 ℃. The dissolution kinetics of nickel and copper that were examined according to heterogeneous model, indicated that the dissolution rates were controlled by surface chemical process during the pug leaching. The activation energy of copper and nickel dissolution were 26.79 kJ.mol^-1 and 38.078 kJ.mol^-1 respectively; and the surface chemical was proposed as the leaching rate-controlling step.

• Resources Recycling
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• v.18 no.6
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• pp.3-9
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• 2009

The present review paper deals the liquid-liquid extraction (LLE) general principles and the basic fundamentals, general process of LLE followed by the importance of LLE reagents. LLE is a process of transferring a chemical compound from one liquid phase to a second liquid phase, immiscible with the first. In analytical chemistry, this method enjoys a favored position among separation techniques because of its simplicity, speed and wide scope. By utilizing apparatus no more complicated than a separatory funnel and requiring several minutes at most to perform, extraction procedures offer much to the analytical chemist.

• Membrane Journal
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• v.22 no.2
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• pp.104-112
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• 2012

Chemically stable Polyvinylidene fluoride-hexa-fluoropropane (PVDF-HFP) copolymer asymmetric membranes were prepared by the conventional phase inversion process, using Dimethyacetamide (DMAc) as a solvent and water as a non-solvent. To control the pore size and porosity of the PVDF-HFP membranes, tetra-ethoxysilane (TEOS) was used as a pore-forming agent. The prepared membranes were characterized, using several analytical methods such as Fourier Transform Infrared spectroscopy (FTIR), Thermo-gravimetric analyzer (TGA), Field Emission Scanning Electronic Microscopy (FESEM). TEOS turned out to increase porosity and make homogeneous pores on the membranes. Depending on the composition of the dope solutions, the pore size was ranged from 0.1 to 1.0 ${\mu}m$. The flux of the PVDF-HFP membranes prepared by using TEOS as a pore forming agent was increased substantially without much decrease in the rejection. When 15 wt% PVDF-HFP solution was blended with 13 wt% TEOS solution at composition ratio of 70/30 in wt%, the water flux at 2 bars was about 2 $m^3/m^2day$.