A chromatographic procedure separates 2.0 mg of sample on a 4.6 i.d. x 150 mm column with a flow rate of 1.0 mL/min. What size column and flow rate are required to separate 500.0 mg of the same mixture?
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A chromatographic procedure separates 2.0 mg of sample on a 4.6 i.d. x 150 mm column with a flow rate of 1.0 mL/min. What size column and flow rate are required to separate 500.0 mg of the same mixture?
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- Titration purity NxVx mEq weight weight of sample (g) x 100 Volume (Weight of sample (g) Nx mEw Weight V = 100 Normality Weight of sample (g) Vx mEw Weight N = 100 mEq Weight mEq Weight % x Weight of sample (g) V xN /100 Weight of sample Nx Vx mEq weight (9)= x 100 %3D % Purity Volume 2 Normality 1 Normality 2 Volume 1What are the advantages and disadvantages of volumetric and gravimetric analysis?What are the differences between systematic and random errors and how do they effect accuracy and precision? In what circumstances would you use standard addition (versus a normal calibration curve) to determine the amount of an analyte in a sample? A urine sample, containing analyte Z is analysed by the standard addition method where 5 mL of the original sample was mixed with increasing amounts of a Z standard and each solution diluted to a volume of 50 mL prior to analysis. A plot of the final concentration of the standard in each of the 50 mL samples (x axis) versus The measured signal from the analysis of each 50 mL sample (on y axis) produced a straight line with the general equation: y = 44.72x + 4.06 what was the final concentration of Z in the 50 mL standard addition sample? what was the initial concentration of Z in the original urine sample?
- Internal standard (As , Cs ), analyte with known concentration (Ax , Cx ) In a chromatographic equipment, a solution containing 0.006727 X and 0.008331 M S give peak area of Ax= 2316 and As= 207. To analyze an unknown sample, 5.0mL of 0.008331M S was added to 5.0mL of X, and the mixture was diluted to 50.0mL. This mixture gave a chromatography spectrum with area Ax= 3206 and As= 200. Find Cx.For a concentration technique, Stotal is given as 19.31 ± 0.035, Smb is 0.22 ± 0.008, and kA is 0.154 1 0.007 ppm, where Stotal is the signal, kA is the method's sensitivity for the analyte and Smb is the signal from the method blank. If we want the absolute percent uncertainty of the concentration CA to be 2.6%, which statement is false below? (Hint: refer to sections 4B.1 and example 4.7 in your textbook) We must improve the uncertainty in KA to 10.004 ppm-¹. O Uncertainty in the method's sensitivity dominates the absolute uncertainty. O Improving the signal's uncertainty will improve the absolute uncertainty.ASSAY Calibration solutions Calibration solutions of naproxen in the range 5 – 25 μg/mL were prepared. Sample preparation 20 tablets weighing 12.3819 g were crushed to a fine powder. A portion of the powder (145.4 mg) was shaken with approximately 150 mL of acetic acid (0.05 M) for 5 min and then made up to volume in a 250 mL volumetric flask (stock solution). Approximately 50 mL of the stock solution was filtered and a 25 mL aliquot was diluted to 100 mL in a volumetric flask. 10 mL of the resulting solution was further diluted to 100 mL with acetic acid (0.05 M). Analysis The standards and sample solutions were analyzed by HPLC under the following conditions: Column: octadecylsilyl (ODS), 4.6 mmx150 mm, mobile phase: acetonitrile : 0.05 M acetic acid (85:15), flow rate: 1 ml/min, UV detection at 243 nm. Results: A calibration curve of concentration versus peak area was constructed for the standard solutions and gave the straight-line equation: y = 3555.6x + 85, r = 0.9999 The area…
- Suppose you have a 11.4 cm long chromatography column with an inner diameter of 5.47 mm that is packed with a stationary phase that occupies 66.0% of the volume. What is the linear flow rate, ux, in centimeters per minute, if the volumetric flow rate, F, is 1.98 mL/min? Ux = cm/min How long will it take, in minutes, for the solvent to pass through the column? min tM = What is the retention time, in minutes, on this column for a solute with the retention factor, k, of 11.0? min tR = %3DExplain the difference between random sampling and haphazard sampling as used in Analytical chemistry.A method for the determination of the corticosteroid methylprednisolone acetate in solutions obtained from pharmaceutical preparations yielded a mean value of 3.7 mg mL with a standard deviation of 0.3 mg mL. For quality control purposes, the relative uncertainty in the concentration should be no more than 3%. How many samples of each batch should be analyzed to ensure that the relative standard deviation does not exceed 9% at the 95% confidence level? samples
- [References) A method for the determination of the corticosteroid methylprednisolone acetate in solutions obtained from pharmaceutical preparations yielded a mean value of 3.7 mg mL with a standard deviation of 0.3 mg mL. For quality control purposes, the relative uncertainty in the concentration should be no more than 3%. How many samples of each batch should be analyzed to ensure that the relative standard deviation does not exceed 9% at the 95% confidence level? samplesA titrimetric method for the determination of calcium in limestone was tested with the analysis of a NIST limestone containing 30.15% CaO. The mean of the four analyzes is 30.26% CaO with a standard deviation of 0.085%. From the data accumulated from many analyzes, s→ϭ=0.094% CaO was found.a) Do the data indicate the presence of systematic error at the 95% confidence level?b) When a value for ϭ is unknown, do the data show a systematic error at the 95% confidence level?A titrimetric method for the determination of calcium in limestone was tested by analysis of an NIST limestone containing 30.15% CaO. The mean result of four analyses was 30.26% CaO, with a standard deviation of 0.085%. By pooling data from several analyses, it was established that s = 0.094% CaO.a. Do the data indicate the presence of a systematic error at the 95% confidence level?b. Do the data indicate the presence of systematic error at the 95% confidence level if no pooled value for s was available?