ANALYTICAL PROCEDURES. For each measurement parameter, reference the applicable standard analytical procedure(s) or provide a written description of the analytical procedure(s) to be used. Provide performance information for each analytical procedure in terms of accuracy, precision and detection limits. Method performance information should meet or exceed the Quality Assurance objectives identified in element number 5. For the sake of convenience, all or part of elements number 8, 9, 10, 11, and 13 may be incorporated into this element. The choice of when to reference a manual's test procedure and when to document a complete Standard Operating Procedure (SOP) can only be made on a case‑by‑case basis. It has been observed that few laboratories, external to the Contract Laboratory Program (CLP), follow exactly, all important details of a standard reference method. Other times standard reference methods provide or allow options (example ‑ the use of different gas chromatography columns for polychlorinated biphenyl (PCB) determinations). Reference to analytical methods in the United States Environmental Protection Agency (EPA) Publications, the American Society for Testing and Materials (ASTM) or "Standard Methods" can be appropriate; however, required sample preparation procedures (filtration, digestion, etc.) also need to be referenced. For example, the United States Environmental Protection Agency’s “Methods for Chemical Analysis of Water and Wastes" provides three (3) different test procedures for most metal determinations and at least four (4) sample preparation protocols for each metal. Each combination of metal determination and sample preparation exhibits different degrees of accuracy, precision, and sensitivity of measurement. Different quality control audits are used for each combination of metal determination and sample preparation. The exact combination used for each metal must be specified.
ANALYTICAL PROCEDURES. Atomic Absorption Spectroscopy (AAS) and Other Analyses For the determination of Zn, Cu, Pb, Ni, Co, Ag, Mn, Fe, Cd, and As a 1 gram sample was reacted with 3 mL concentrated HNO3 in a test-tube overnight at room temperature. After digestion, the test-tube was immersed in a hot water bath at room temperature and brought up to 90° C and held at this temperature for 30 minutes with periodic shaking. 1 mL concentrated HCl was added and heating was continued for another 90 minutes. The sample solution was then diluted to 20 mL with metal free water and mixed. Zn, Cu, Pb, Ni, Co, Ag, Mn, Fe and Cd were determined by atomic absorption spectroscopy using an air-acetylene flame. Background corrections were made for Pb, Ni, Co, Ag and Cd. Arsenic was determined by atomic absorption using a hydride evolution method wherein the hydride (AsH3) is evolved and passed through a heated quartz tube in the light path of an atomic absorption spectrophotometer. The method is described by Xxxxx (1976). Detection limit = 1 ppm. Molybdenum and vanadium were determined by atomic absorption spectroscopy using a nitrous oxide acetylene flame. A 0.5 gram sample was reacted with 1.5 mL concentrated HNO3 at 90 ° C for 30 minutes. At this point 0.5 mL concentrated HCl was added and the digestion was continued at 90 ° C for an additional 90 minutes. After cooling, 8 mL of 1250 ppm Al solution were added and the sample solution was diluted to 10 mL before aspiration. Detection limit: Mo - 2 ppm; V - 5 ppm. Xxxxxxx was determined by the Hatch and Xxx Procedure with some modifications. The method is described by Xxxxxxxx et al. (1973). A 0.5 gram sample was reacted with 20 m L concentrated HNO3 and 1 mL concentrated HCl in a test-tube for 10 minutes at room temperature prior to 2 hours of digestion with mixing at 90° C in a hot water bath. After digestion, the sample solutions were cooled and diluted to 100 mL with metal free water. The Hg present was reduced to the elemental state by the addition of 10 mL 10 % w/ v Sn SO 4 in M H 2 SO 4. The Hg vapour was then f lushed by a stream of air into an absorption cell mounted in the light path of an atomic absorption spectrophotometer. Absorption measurements were made at 253.7 nm. Detection limit = 10 ppb. Loss on ignition was determined using a 500 mg sample. The sample, weighed into 30 ml beaker, was placed in a cold muffle furnace and brought up to 500° C over a period of 2 - 3 hours. The sample was left at this temperature for 4 hours, then...
ANALYTICAL PROCEDURES. Instrumental Neutron Activation Analysis (INAA) The weighed sample (generally 5 to 10 g) is irradiated for 20 minutes in a neutron flux whose approximate density is 5.3 x 10 to the exp. 11 neutrons/square cm/second. Counting is begun seven days after irradiation. The counting time is somewhat variable (6 to 11 minutes) and is matrix dependent. Counting is done on a germanium-lithium co-axial counter. The counting data is accumulated on a VAX computer and is subsequently converted to concentrations. Numerous international reference samples are irradiated with each batch of routine samples. Elements determined by INA analyses include: Na, Sc, Cr, Fe, Co, Ni, Zn, As, Se, Br, Rb, Zr, Mo, Ag, Cd, Sn, Sb, Te, Cs, Ba, La, Ce, Xx, Eu, Tb, Yb, Lu, Hf, Ta, W, Ir, Au, Th, and U. Data for Zn, Se, Zr, Ag, Cd, Sn, Te and Ir are not published because of inadequate detection limits and/or precision.
ANALYTICAL PROCEDURES. Atomic Absorption Spectroscopy (AAS) and Other Analyses The sample digestion procedure differed for stream and lake sediments as follows: for stream sediments, to determine of Zn, Cu, Pb, Ni, Co, Ag, Mn, Fe, Cd, and As a 1 gram sample was reacted with 3 mL concentrated HNO3 in a test-tube overnight at room temperature. After digestion, the test-tube was immersed in a hot water bath at room temperature and brought up to 90° C and held at this temperature for 30 minutes with periodic shaking. 1 mL concentrated HCl was added and heating was continued for another 90 minutes. The sample solution was then diluted to 20 mL with metal free water and mixed. Zn, Cu, Pb, Ni, Co, Ag, Mn, Fe and Cd were determined by atomic absorption spectroscopy using an air- acetylene flame. Background corrections were made for Pb, Ni, Co, Ag and Cd. For lake sediments, to determine Zn, Cu, Pb, Ni, Co, Ag, Mn, Fe, Cd, and As a 1 gram sample was reacted with 6 m L of a mixture of 4 M HNO 3 and M HCl in a test-tube overnight at room temperature. After digestion, the test-tube was immersed in a hot water bath at room temperature and brought up to 90° C and held at this temperature for 2 hours with periodic shaking. The sample solution was then diluted to 20 mL with metal free water and mixed. Zn, Cu, Pb, Ni, Co, Ag, Mn, Fe and Cd were determined by atomic absorption spectroscopy using an air- acetylene flame. Background corrections were made for Pb, Ni, Co, Ag and Cd. Arsenic was determined by atomic absorption using a hydride evolution method wherein the hydride (AsH3) is evolved and passed through a heated quartz tube in the light path of an atomic absorption spectrophotometer. The method is described by Xxxxx (1976). Detection limit = 1 ppm. Molybdenum and vanadium were determined by atomic absorption spectroscopy using a nitrous oxide acetylene flame. A 0.5 gram sample was reacted with 1.5 mL concentrated HNO3 at 90 ° C for 30 minutes. At this point 0.5 mL concentrated HCl was added and the digestion was continued at 90 ° C for an additional 90 minutes. After cooling, 8 mL of 1250 ppm Al solution were added and the sample solution was diluted to 10 mL before aspiration. Detection limit: Mo - 2 ppm; V - 5 ppm. Xxxxxxx was determined by the Hatch and Xxx Procedure with some modifications. The method is described by Xxxxxxxx et al. (1973). A 0.5 gram sample was reacted with 20 m L concentrated HNO 3 and 1 mL concentrated HCl in a test-tube for 10 minutes at room temperature prior to 2...
ANALYTICAL PROCEDURES. Analytical procedures are used in the planning and final stages of the audit. In the planning phase, we use analytical procedures to identify unusual financial transactions and compare relationships to expected results. We compare current-year information to the prior years for balance sheet items, revenues, and expenditures. In the final stages of the audit, the financial statements are reviewed to identify expected relationships, such as comparing debt paid to expenditures recorded on governmental funds, transfers between funds, depreciation expense, etc. For all significant relationships identified, explanations are obtained as to why the situation occurred and additional audit procedures are applied to resolve any concerns.
ANALYTICAL PROCEDURES. The internal auditor should apply analytical procedures as the risk assessment procedures at the planning and overall review stages of the internal audit. It involves various comparisons as depicted below: In determining the extent to which the analytical procedures should be used, the internal auditor should consider the following factors:
ANALYTICAL PROCEDURES. (a) Analytical Procedures applicable to the Goods have been provided by the Company to the Suppliers and/or are attached hereto. The Supplier acknowledges having received the Analytical Procedures and agrees to comply fully therewith.
ANALYTICAL PROCEDURES. Identification of Potential Audit Problems ............................................................................................ Resources Available for Standards Interpretations ...............................................................................
