Recovery Test Procedure

The purpose is to determine the capabilities of the system to recover from internally generated contamination. 

It is the responsibility of validation team members to follow the procedures. The quality assurance (QA) manager is responsible for SOP compliance. 

The recovery time should be not more than 2 minutes or as specified for individual work zone in the validation master plan. 

Equipment calibrated on Next calibration due on Test performed date  

Grid Area Smoke Generation Time Particulate Count Meeting Acceptance Criteria (Recovery Time) 

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Also, the test procedure (protocol) is fundamental because it allows comparing results from different laboratories and from different experimental sets. Moreover, selected test protocol could affect the interpretation of the results, the information content and its application in the safety evaluation process, as stated by Frazer if the biological system is exposed to a test chemical for 24 h and the endpoint assay is immediately conducted, the data produced would be most relevant to the acute toxicity of the test material. If, on the other hand, the system is exposed to material for 24 h and the system is cultured in the absence of the test material for additional 48 h before the endpoint assay is conducted, the data would be more relevant to recovery from toxicity rather than acute toxicity [7]. 

Recovery — Overall procedural recovery was evaluated. The results from spiked plasma QC (evaluation) samples that went through the analytical procedure were compared to the results from neat spiking (control) solution samples. The neat spiking solutions used to prepare the plasma evaluation samples were evaporated and reconstituted at the same volumes as the extracted samples. The analyte was tested at three concentration levels and the internal standard was tested at one. Mean recovery for the analyte was approximately 122.9% the level was 55.2% for the internal standard. 

Accuracy. In the quantitative method that is used to measure the heavy metal quantity in the drug substance, the accuracy is usually represented by the recovery rate obtained from a spiked recovery test where lead is added to the samples. Since the heavy metals limit test specified in monograph specifications is a test where the intensity of coloring of the samples with sodium sulfide is compared with that of the control solution, it is necessary to confirm that heavy metal components can be detected fully in the process of test solution preparation. The Heavy Metals Limit Test in JP specifies four preparation methods for the test solutions. An appropriate method will be selected and used for further testing. The test method that gives the best recovery rate is to be adopted. The procedure is as follows ... 

In this study, a factorial experiment was set up to evaluate the effects of four variables at two levels on extraction efficiencies by using bonded-phase isolation techniques and a 27-component synthetic test mixture. The compounds studied and the respective mass ions used for quantitation are given in the box. The compounds in the mix vary greatly in water solubility and volatility and, in general, represent a wide class of organic compounds typical of those present in environmental samples. To maximize solute recoveries, the procedure was... 

Table D2.4.1 Differences in the Conversion Factor (K)a Used in the Spectrophotometric 2-Thiobarbituric Acid (TBA) Test Due to Variability in Recovery and Procedures 3...

Two of the most common methods of determining accuracy are by comparing the proposed test procedure to a second test procedure whose accuracy is known and the recovery of drug above and below the range of use. Average recovery of the drug should be 98-102% of the theoretical value. Recoveries can be determined by either external or internal standard methods. 

As in analytical liquid chromatography (LC), analyte retention depends on sample concentration, solvent strength, and sorbent characteristics. An empirical approach to methods development initially involves screening the available sorbents. The first step is to determine which sorbents best retain the analyte. The second consideration is to evaluate the solvents needed to elute the compound and the compatibility of those sorbents to the chromatographic testing procedure. The third step is to test the blank sample matrix to evaluate the presence of possible interferents. Finally, recoveries of known quantities of analyte added to the sample matrix must be determined. 

This is a procedure that is regularly given more importance than deserved in the efforts to guarantee the trueness of experimental results when determining trace elements in foodstuffs. The information value of recovery tests in element analysis by AAS in food is very limited. Recovery information is important in chemical analysis where there is an extraction step in order to elucidate the efficiency of... 

The series of observations outlined above have a number of implications for any program directed at preserving the quality of cellulosic materials. These can be categorized broadly as relating to three types of objectives (1) prevention of further deterioration, (2) recovery of some of the properties already lost through aging, and (3) the interpretation of accelerated testing procedures. 

It is absolutely essential that the accuracy be validated with the same quantitation method that is used in the control test procedure. Recovery deviations from the theoretical values while performing a calibration with a drug substance alone may indicate interferences between the analyte and placebo components. In such a case, the calibration should be done with a synthetic mixture of placebo and drug substance standard. Such interferences may also be detected by the separate determination of linearity for dilutions of the drug substance and for a spiked placebo. 

The best statistical acceptance/rejection criteria for immunoassay results have proved to be the use of confidence intervals for total measurement error (e.g., including both accuracy and precision) and equivalence testing procedures [15], and a 90% two-sided confidence interval has been proposed for the acceptance of immunoassay data [145]. Recoveries of 70-120% are considered acceptable according to US-EPA guidelines and the maximum permissible level of false negatives is 5% [38]. 

A procedure for the determination of molybdenum in serum, red blood cells, and urine is described. The low concentration of molybdenum in most unexposed individuals requires the sensitivity obtained using atomic absorption spectrophotometry and electrothermal atomization. Spike recovery tests indicate that low temperature ashing is required for accuracy. Severe matrix interferences preclude wet ashing or high-temperature ashing as sample pretreatments. Using the method described, it is possible to distinguish between industrially exposed and unexposed individuals. 

Direct information on elastic recovery, relative hardness, work of indentation, and strain rate-stress relationship (Fig. 2.15) can provide a comprehensive fingerprint of a particular sample resulting, for example, from a change in either a production process or a wear test procedure. It is ideally suited to the comparison of one sample with a control or reference. The wider assumptions that are needed to derive indirect... 

Discussions arose on the verification of the extraction recoveries. At present, there is no standardised procedure to check the extraction efficiency the methods used are briefly summarised above, showing that they differed widely from one laboratory to another. The participants recognised that it would be necessary to find out the most suitable recovery test to propose a standardised procedure in order to avoid possible discrepancies the technique which was most supported was standard addition (e.g. three levels on wet sediment), equilibrating the spiked mixture overnight. 

A complementary approach to virus safety is the design of virus kill and removal steps of the protein recovery process. These include the physical and chemical principles of separating (theoretical) viral contaminants from the product, or inactivating them. Again, appropriate testing procedures and the demonstration of inactivation and removal of model viruses, as discussed by Wiebe et al. [139] is considered a major provision for the safety of recombinant products from hamster cells. 

In most cases, chemical analysis of environmental samples relies on an extraction step, followed by determination of the target chemical species in the extract obtained. Complete extraction is not possible for most contaminants, unless very onerous procedures are followed. As a result, the extent and variability of extraction must be known as otherwise the held concentrations of contaminant may be underestimated. When dealing with water samples it is possible to introduce a recovery spike into the sample, preferably immediately on sampling in the held, in which case the efficiency of the whole testing procedure, including extraction, can be assessed. For soil samples, with the exception of more volatile organic contaminants, dispersion of the spike throughout the sample is very poor, so that this approach does not work. 

Recovery tests were run on samples of various industrial waters by the above proposed atomic absorption-solvent extraction procedure. However before extraction, all samples were acidified with I ml. concentrated hydrochloric acid per 100 ml. sample and boiled for five minutes to dissolve precipitated metals. The samples were then cooled and filtered to remove any remaining particulate matter which could clog the atomizer. For the determination of iron, 0.1 gram potassium persulfate was added in addition to the acid and then boiled to oxidize ferrous iron to the ferric state. The values shown in Table III are typical of the results that can be expected. 

Digestion by boiling in the presence pf 30% hydrogen peroxide (Jackson (8)) yielded incomplete recoveries of total soluble phosphorus from all the estuarine water samples tested and from organic media such as Difco tryptone and peptone. Moreover, the method failed to yield quantitative recovery of an orthophosphate standard carried through the test procedure. 

Testing Procedures. The tensile properties of dry and wet warp yarns from control and treated samples were measured by ASTM D2256-66T on an Instron Tensile Tester, Model TM using a gauge length of 3 inches and a rate of extension of 33% per minute (Table I). Wrinkle recovery (dry and wet) values were determined by AATCC test method 66-1978 (Table 11). The felting shrinkage and alkali solubilities were determined by the methods outlined by Haron (14) (Table II). 

In situations where the analyte is present in trace quantities (as usually occurs in environmental samples), it is vitally important to maximize the recovery of the analyte from the sample matrix and to lose as little of the analyte as possible during any subsequent processing or work-up stages in the analytical process. Extensive recovery testing is usually required to determine the efficiency of the collection and processing procedures. 

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