Analytical Support Laboratories

The functions of these laboratories usually are sterility testing of production samples, and chemical assays of raw materials for approval to use in the processes, blends or batches of raw materials before sterilization, scheduled samples of production batches, fermenter feeds, waste streams and miscellaneous sources. In many instances the analytical work for the culture laboratories will also be performed. 

Typical laboratories have Technicon Auto-analyzers for each of the common repetitive assays (the product of the fermentations, carbohydrates, phosphate, various ions, specific enzymes, etc.). Other equipment generally includes balances, gas chromatographs, high pressure liquid chromato- 

Fermenter sterility testing requires a room with a laminar flow hood to prepare plates, tubes and shake flasks. Space needs to be provided for incubators and microscopes. Since it is very important to identify when infection occurs in large scale production, microscopic examination of shake flasks is usually preferred because a large sample can be used, and it gives the fastest response. Similarly, stereo microscopes are used for reading spiral streaks on agar plates before the naked eye can see colonies. 

Chemical and glassware storage, dish washing, sample refrigerators, glassware dryers, autoclaves for the preparation of sterile sample bottles for the plant, computer(s) for assay calculations, water baths, fume hoods, etc., are additional basic equipment items needed. Typical overall space requirements are 450 ft of floor space per working chemical technician. 

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The RRS can be either driven to or flown to locations where CAIS have been recovered. Transporting by air requires the use of two C-17 aircraft (one for the RRS operations and utility trailers and one for transporters, a supply trailer, and a mobile analytical support laboratory). The RRS can treat one PIG12 of CAIS per day. 

Example of a prescriptive approach to quality assurance. Adapted from Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, "Handbook for Analytical Quality Control in Water and Wastewater Laboratories," March 1979. 

Coordinating with analytical laboratories, including sample scheduling, sample bottle acquisition reporting, chain-of-custody records, and procurement of close support laboratories or other in-field analytical capabilities... 

This work was funded under a Laboratory Directed Research and Development (LDRD) grant administered by Pacific Northwest National Laboratory (PNNL). PNNL is operated by Battelle for the US Department of Energy. We acknowledge the help of April Getty with 13C NMR and Catherine Petersen with MALDI Mass Spectra. Keith Peterson assisted in reactor support and Tom Wietsma in analytical support. Finally we appreciate the help of Jim White and Dennis Miller for helpful discussions. 

Sample analyses were carried out by a number of laboratories. We are grateful to Mr. Mark E. Peden and Ms. Loretta M. Skowron of the Water Survey s Analytical Chemistry Laboratory Unit for atomic absorption spectrophotometry, Mr. L. R. Henderson of the Illinois State Geological Survey for X-ray Fluorescence specto-scopy, and Dr. T. A. Cahill of the University of Califomia-Davis for elemental analysis. Mr. R. G. Semonin reviewed the manuscript. This material is based upon work supported by the National Science Foundation under Grant No. ATM-7724294, and by the Department of Energy, Division of Biomedical and Environmental Research, under Contract No. EY-76-S-02-1199. 

DCLS is the analytical regulatory laboratory for the State of Virginia, and is staffed by nearly 350 employees analyzing over a million samples a year. The laboratory consists of a Quality Assurance Section and the Bureaus of Chemistry, Forensic Science, Microbiological Science, and Technical and Logistic Support. The QA program is based on a Division QA Policy mandated by the Laboratory Director, and a Division QA Plan which establishes broad guidelines for more specific Bureau QA Plans. Each Bureau is divided into diverse analytical sections which operate under even more individualized QA plans that are patterned after the Bureau Plan. 

It is important to point out that the quality of analytical results is not immediate it can only be achieved if an extensive set of measures are adopted and complied with. Therefore, in parallel to the development of the QA concept, QC systems were introduced as an important tool supporting the QA of chemical measurements. The QC process of examination of laboratory performance in time should always follow QA. QC thus comprises a set of operational techniques and activities used to check whether the requirements for quality are fulfilled. In practice, QC in an analytical chemistry laboratory implies operations carried out daily during the collection, preparation, and analysis of samples, which are designed to ensure that the laboratory can provide accurate and precise results. QC procedures are intended to ensure the quality of results for specific samples or batches of samples and include the analysis of reference materials (RMs), blind samples, blanks, spiked samples, duplicate, and other control samples.2... 

Supplement to the 15 th edn. of Standard Methods for the Examination of Water and Waste Water. Selected Analytical Methods Approved and Cited by the US Environmental Protection agency. American Public Health Association, American Waterworks Association, Water Pollution Control Federation, Sept. (1978). Methods S60 and S63. Methods for benzidine, chlorinated organic compounds, pentachlorophenol and pesticides in water and waste water (Interim, Pending issuance of methods for organic analysis of water and wastes, Sept. 1978), Environmental Protection Agency, Environmental Monitoring and Support Laboratory (EMSL). 

The Analytical Chemistry Branch (ACB) of the Environmental Mon-itoring and Support Laboratory of the U.S. Environmental Protection Agency has a number of responsibilities for analytical support. Analyses of fuels, sources, and ambient samples are performed along with the analyses of divers other types of specimens including tissue, both plant and animal. One of the major areas of support rendered by the ACB is in support of the National Air Siurveillance Networks (NASN) a portion of this support consists of the analysis of collected material for airborne metallic elemental content. This chapter will, in the main, be a summary of the work done by the ACB with respect to the collection and analysis of airborne metallic elements. 

Ethylene glycol intoxication is relatively rare, but when it does occur, it is important for the laboratory to provide rapid (<2 hours) analytical support. A GC-MS method is included in the Chapter 34 Appendix that is found on this book s accompanying Evolve site (http //evolve.elsevier.com/ Tietz/textbook/) it allows for the simultaneous determination of ethylene glycol and glycolic acid. It is relatively... 

Process considerations to prepare for and execute a scale-up run can be broken down into seven areas safety, documentation, personnel, equipment ability, analytical support, chemicals, and operations. The following checklists will help prepare for a scale-up run and provide guidelines for implementing the run in the pilot plant or the kilo laboratory. Section IV.B reviews the salient points of the checklists, and IV.C provides special reminders about kilo lab procedures. 

The authors are indebted to G. L. Bridger for many helpful suggestions. The laboratory phase of the research was ably assisted by Manuel Eisenstadt and Bruce L. MacEwen. Credit is due David E. Kramm for analytical support. The thermogravimetric measurements were made by Saul Gordon, 12 Brookfield Way, Morristown, N. J. 

In addition to the engineering skills and the access to the full range of supporting laboratory capabilities (bench development, in-process, analytical, physical chemistry, microbiology), scaling-up requires a variety of measurement apparatus (e.g., compressibility cell to measure flows through beds of solids at different compression), as well as the frequent assembly of dedicated apparatus or pilot units (e.g., units to measure fouling rates of surfaces over short-term test, small-scale... 

Support a clean porcelain crucible with the cover slightly tilted on a wire triangle, and heat the crucible as hot as possible for 5 minutes (Laboratory Methods D). The bottom of the crucible should glow a dull red (red heat) for the full 5 minutes. Use only tongs to handle the crucible and cover after it has been heated. From this point on in the experiment the crucible and cover must not be touched with your hands. Place the hot crucible and cover in a dessicator, if available, and allow it to cool to room temperature. Then weigh the crucible and cover on an analytical balance (Laboratory Methods C), and record the mass in TABLE 6.1. 

Support a clean crucible and cover on a wire triangle, and heat them for 5 minutes until they are thoroughly dry (Laboratory Methods M). Allow the crucible and cover to cool to room temperature. Then weigh them on an analytical balance (Laboratory Methods C), and record the mass in TABLE 7.1. Use tongs to handle the crucible. 

For completeness, it should be mentioned that laboratories providing QC and analytical support to pharmaceutical production, and also to the production of medical devices and diagnostic materials, are subject to assessment to ensure they comply with the relevant requirements of the Guide to GMP. These requirements are very similar to those found in the other standards. The laboratories are not accredited, but compliance with requirements is a condition of granting and maintaining a manufacturing license for the products concerned. 

Of the many people who have worked in this area, particular mention must be made of W. E. Carroll, J. N. Drescher-Reidy, K. B. Kelby, W. L. Renz, J. van Horn, A. Kotz, F. Prozonic, and D. J. Nagy who contributed in significant measure to the laboratory, analytical support, and commercial work. 

W Goldschmidt, D Gallis, D Catherman. On-site analytical support a cost-effective alternative to fixed laboratory services. Remediation 4 425, 1994. 

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