scholarly journals Validation of Modification of Volumetric Methode of Determination of Sn (Tin) Concentration on Tin Concentrates

2021 ◽  
Vol 3 (2) ◽  
pp. 41-48
Author(s):  
Onek Gunawan
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Volumetric Method ◽  
Limit Of Quantification ◽  
Validation And Verification ◽  
Analysis Techniques ◽  
Modified Method ◽  
Relative Standard ◽  
The 19Th Century

The analysis techniques for determining the concentration of Stanum (Sn) in Tin Concentrate has been developing since the 19th century. Various methods and analysis techniques are to find the most effective and efficient method enabling to achieve optimal results. In this study, a modification of the classic volumetric method that has been used includes modifications to the use of materials and tools in the analysis. In this study, validation and verification of the modified method was also carried out by determining the value of the parameters of Precision, Accuracy, Method of Detection Limit (MDL) and the Ruggedness and Robustness of the method and comparing the acceptability value based on the existing provisions. on the EURACHEM guide. After performing 25 tests using the NCS DC 35002 Certified Reference Material, it was revealed the value of the parameters for the Precision/Relative Standard Deviation (RSD)  to be   0.21% (<0.5 CV Horwitz), the accuracy value is 99.9% with bias 0.06%, the MDL values for Minimum Detection Limit (MDL) and Limit of Quantification (LOQ) are 0.4% and 1.32%, respectively. The value of the ruggedness and robustness of the method was carried out by testing at different times and by different analysts and obtained RSD 0.22% (<2/3 CV Horwitz). From the values of the parameters obtained, it can be concluded that the modification of this method fulfills the acceptance value required by EURACHEM.

scholarly journals MEAN CENTERING OF RATIO SPECTRA METHOD FOR THE ANALYSIS OF THEOPHYLLINE AND EPHEDRINE HCL MIXTURE IN TABLET

2018 ◽  
Vol 11 (5) ◽  
pp. 218
Author(s):  
Muchlisyam Muchlisyam ◽  
Sudarmi Sudarmi ◽  
Cindy Caroline
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Standard Addition ◽  
Addition Method ◽  
Limit Of Quantification ◽  
Mean Centering ◽  
Relative Standard

 Objective: Mean centering of ratio spectra method (MCR method) is one of the simplest methods for the determination of drug mixtures. The purpose of this research is to determine the content of theophylline (THEO) and ephedrine HCl (EPH) in tablets by MCR spectra method.Methods: This research was conducted with the MCR method. It was measured at 271 nm for THEO and 257 nm for EPH using 0.1 N HCL as a solution. The calculation was conducted with Matlab application. The analytical characteristics of the method are detection limit, accuracy, precision, and selectivity. Standard addition method was used to increase the concentration of EPH in the sample until it reached the range of calibration concentration.Result: The research has showed that validations for THEO were 100.57% for accuracy, 0.68% for relative standard deviation (RSD), 0.46 μg/mL for limit of detection (LOD), and 1.52 μg/mL for limit of quantification (LOQ). Meanwhile, the validations for EPH are 100.02% for accuracy, 0.07% for RSD, 43.12 μg/mL for LOD, and 143.72 μg/mL for LOQ. The level of THEO is 97.43 ± 0.17% and the level of EPH is 101.36 ± 0.25% for brand one’s tablet. Meanwhile, brand two’s tablet contains 98.72 ± 0.14% of THEO and 103.62 ± 0.23% of EPH.Conclusion: MCR ultraviolet spectrophotometric method can be used to determine the content of THEO and EPH in tablets and meets the detection limit, accuracy, precision, and selectivity.

The Improvement of Pretreatment on the Determination of Mercuryin Industrial Wastewater

2014 ◽  
Vol 587-589 ◽  
pp. 620-624
Author(s):  
Ming Ming Yang ◽  
Wei Tang
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Industrial Wastewater ◽  
Microwave Digestion ◽  
Hydride Generation ◽  
Mercury Determination ◽  
Absorption Method ◽  
Limit Of Quantification ◽  
Relative Standard

Discussed with the (MWD) for Nitrogen Oxide interference of the mercury determination in wastewater, studied the method of elimination volatile nitrogen oxides rapidly. Optimized the conditions by microwave-digestion hydride generation atomic absorption method for determination of mercury in daily chemical .The detection limit of the method was 0.4μg/L, the lower limit of quantification was 1.2μg/L, the relative standard deviation determined by spiked samples is 1.5% and recovery from 94% to 103%.

scholarly journals Spectrophotometric flow injection procedure to indirect determination of paracetamol in pharmaceutical formulations using o-tolidine as reagent

2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Flow Injection ◽  
Pharmaceutical Formulations ◽  
Injection Method ◽  
Indirect Determination ◽  
Analytical Curve ◽  
Relative Standard ◽  
Injection Procedure

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.

Cloud Point Extraction-Fluorimetric Combined Methodology for the Determination of Magnolol

2013 ◽  
Vol 699 ◽  
pp. 34-39
Author(s):  
Li Liu ◽  
Xia Shi Zhu
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Cloud Point ◽  
Relative Standard Deviation ◽  
Cloud Point Extraction ◽  
Calibration Graph ◽  
Optimum Conditions ◽  
Relative Standard ◽  
Triton X

A new Triton X-114 cloud point extraction combined with fluorometry method for analysis of magnolol in drug samples was developed. Under the optimum conditions, the calibration graph was linear in the range of 2.0-150.0ng/mL of magnolol in the initial solution with r = 0.9998. Detection limit (DL) was 0.03ng/mL (S/N=3) and the relative standard deviation (RSD) for 20.0ng/mL of magnolol was 2.79%(n=11). The method was successfully applied for the determination of magnolol in drug samples with satisfactory results.

Spctrophotometric Determination of Trace Ruthenium by its Catalytic Effect on Oxidation of 3,5-DiBr-PADAP with KIO4

2012 ◽  
Vol 554-556 ◽  
pp. 1999-2005
Author(s):  
Zhi Rong Zhou ◽  
Qun Wang ◽  
Shu Yuan Zhang
Keyword(s):  
Activation Energy ◽  
Standard Deviation ◽  
Detection Limit ◽  
Catalytic Reaction ◽  
Oxidation Reaction ◽  
Catalytic Effect ◽  
Optimum Conditions ◽  
Potassium Periodate ◽  
Relative Standard

A spectrophotometric method for the determination of ruthenium (III) is described, based on its catalytic effect on the oxidation reaction of 2-[(3,5-dibromo-2-pyridy)azo]-5-diethylaminophenol (3,5-diBr-PADAP) with potassium periodate in 0.008 mol/L sodium hydroxide medium and in the presence of OP emulsifier (p-iso-octyl phenoxy polyethoxy ethanol) at 100 °C. The above reaction is followed spectrophotometrically by measuring the decrease in the absorbance at 530 nm for the catalytic reaction of 3,5-diBr-PADAP. The calibration curve for the recommended method was linear in the concentration range over 0.04 µg/L–1.0 µg/L and the detection limit of the method for Ru (III) is 0.012 µg/L. The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 100.48 kJ/mol. The relative standard deviation for the determination of ruthenium (III) at the concentration of 0.02 µg/25mL is calculated to be 2.30 % (n=11). In combination with distilled separation, the method has been successfully applied for the determination of trace ruthenium (III) in some ores and metallurgy products with the relative standard deviations (RSD) over 1.8 %–2.9 % and the recovery over 98.1 %–103.1 %.

scholarly journals Interlaboratory Comparison of Methods for the Determination of Incurred Tilmicosin Residues in Bovine Liver

2002 ◽  
Vol 85 (6) ◽  
pp. 1260-1267
Author(s):  
Susan B Clark ◽  
John J O'rangers ◽  
W Douglas Rowe ◽  
Mark R Madson ◽  
Jeffrey A Hurlbut ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Carbon Tetrachloride ◽  
Interlaboratory Comparison ◽  
Drug Application ◽  
Bovine Liver ◽  
Comparison Of Methods ◽  
Tissue Samples ◽  
Modified Method ◽  
Relative Standard

Abstract The objective of this study was to compare 2 methods for the determination of tilmicosin residues in bovine liver samples. Three laboratories participated in the comparison of the 2 methods. The first method was described in a New Animal Drug Application (NADA 140–929), and the second was a modification of that method in which hexane was substituted for carbon tetrachloride in one cleanup step. Each of the 3 laboratories analyzed subsamples of 10 bovine livers containing incurred tilmicosin. Residues ranged from 2.3 to 81 ppm tilmicosin in the 10 liver samples with an 11.8% relative standard deviation obtained by using both methods. In addition, fortified-control liver tissue samples were analyzed concurrently with tissues containing incurred residues by using the modified method in one of the laboratories. The fortification levels ranged from 0.3 to 112 ppm, with recoveries ranging from 76 to 92%. The results from the 3 laboratories were comparable, indicating that the modified method was not only as effective as the original NADA method, but also more desirable because of the change to a less hazardous solvent.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals Spectrophotometric Method for the Determination of Drugs Containing Phenol Group by Using 2, 4- Dinitrophenylhydrazine

2010 ◽  
Vol 7 (2) ◽  
pp. 395-402
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Kumar Shrestha
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Phenolic Drugs

A spectrophotometric method has been proposed for the determination of four phenolic drugs; salbutamol, ritodrine, amoxicillin and isoxsuprine. The method is based on the oxidation of 2, 4- dinitrophenyl-hydrazine and coupling of the oxidized product with drugs to give intensely colored chromogen. Under the proposed optimum condition, beer’s law was obeyed in the concentration range of 2.5-17, 2-29, 4-33 and 5-30 μg/mL for salbutamol, ritodrine, amoxicillin and isoxsuprine respectively. The limit of detection (LOD) and limit of quantification (LOQ) were 0.2, 0.83, 0.09, 0.84 μg/mL and 0.66, 2.79, 0.3 and 2.81 μg/mL in the same order. No interference was observed from common pharmaceutical adjuvants. The ringbom plots and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical dosage forms, which was compared statistically with reference methods by means oft- test andF- test and were found not to differ significantly at 95% confidence level. The procedure is characterized by its simplicity with accuracy and precision.

Determination of Cl- and SO42- in Boric Acid

2012 ◽  
Vol 152-154 ◽  
pp. 507-512
Author(s):  
Dian Ting Gong
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Boric Acid ◽  
Linear Relationship ◽  
Recovery Rate ◽  
Heating Time ◽  
Measuring Time ◽  
Relative Standard ◽  
Precision And Accuracy

Microcontents of Cl- and SO42- in boric acid were determined by photoelectricity turbidimetry with acid as medium. The effects of stabilizer, acidity of solution, content of precipitant, heating time and temperature as well as measuring time on the turbidity of the solution were studied. After above experiment parameters were optimized, in the measurements to determine SO42- in boric acid, the stabilizer was glycerine-ethanol (1:4), the precipitant was acidic BaCl2. The solution was shaked and heated, as a result, the adding sequence of reagents had no effects on results. The detection limit was 0.10mg/L, relative standard deviation (RSD) was less than 3%, recovery rate was 98.85%~103.00%, and measuring time last over 40min. SO42- concentration in the range of 0.33 mg/L ~0.83mg/L showed a linear relationship with turbidity. In the determination of chlorine, the stabilizer was glycerine, measuring time held in 40min, detection limit was 0.03mg/L, RSD was less than 4%, and recovery rate was 102.2%~106.5%. Cl- concentration in the range of 0.10 mg/L ~0.25mg/L showed a linear relationship with turbidity. Photoelectricity turbidimetry improve the precision and accuracy of the measurements. The method of turbidimetry to determine Cl- and SO42- in boric acid is simple, reliable, innocuous and applicable in practice.

scholarly journals DETERMINATION OF ACETATE IN FOODS BY ION CHROMATOGRAPHY-FLOW INJECTION

1995 ◽  
Vol 3 (3) ◽  
pp. 9-22
Author(s):  
E. Esteve-Juan ◽  
R. Puchades ◽  
A. Maquieira
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Ion Chromatography ◽  
Chromatographic Analysis ◽  
Reference Method ◽  
Spectrophotometric Detection ◽  
Flow Rates ◽  
Injection Volume ◽  
Relative Standard

A method for acetate determination using IC separation and FI post-column spectrophotometric detection based on the La(OH)3-I2 reaction has been developed. The chromatographic conditions (eluants, flow-rates, sensitivity, and so on) and FI variables (length of coils, injection volume, pH, ... ) were optimized. Linearity was observed over the concentration range 0 to 1 gl-1 with HAc as standard (r = 0.9916) and a detection limit of 0.1 g AcH/l. The IC-FI method afforded a low relative standard deviation (3.6%) and was free from interferences. The IC-FI procedure was applied to the determination of acetate in mustard sauce and the results obtained agree with those provided by the reference method. Additionally, the developed method permits the simultaneous chromatographic analysis of other anions such as chloride, nitrate, phosphate, sulphate, and so on.

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