Analytical methods laboratories

This chapter has considered two of the types of interlaboratory comparison exercise in which your laboratory may participate. It is important to remember that proficiency testing schemes and collaborative studies have different aims. The former is a test of the performance of the laboratory, whereas the latter is used to evaluate the performance of a particular analytical method. Laboratories should participate in proficiency testing schemes (where an appropriate scheme is available) as this provides an independent check of the laboratory s performance. This chapter has described the key features of proficiency testing schemes and explained how the results from participation in a scheme should be interpreted. 

Normality is an older unit of concentration that, although once commonly used, is frequently ignored in today s laboratories. Normality is still used in some handbooks of analytical methods, and, for this reason, it is helpful to understand its meaning. For example, normality is the concentration unit used in Standard Methods for the Examination of Water and Wastewaterf a commonly used source of analytical methods for environmental laboratories. 

An external standardization allows a related series of samples to be analyzed using a single calibration curve. This is an important advantage in laboratories where many samples are to be analyzed or when the need for a rapid throughput of samples is critical. Not surprisingly, many of the most commonly encountered quantitative analytical methods are based on an external standardization. 

An important step in developing a standard method is to determine which factors have a pronounced effect on the quality of the analytical method s result. The procedure can then be written to specify the degree to which these factors must be controlled. A procedure that, when carefully followed, produces high-quality results in different laboratories is considered rugged. The method by which the critical factors are discovered is called ruggedness testing. ... 

The importance of between-laboratory variability on the results of an analytical method can be determined by having several laboratories analyze the same sample. In one such study seven laboratories analyzed a sample of homogenized milk for a selected alfatoxin. The results, in parts per billion, are summarized in the following table. 

The EPA Contract Laboratory Program (CLP) has responsibility for managing the analysis programs required under the U.S. Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA). The approved analytical methods are designed to analyze water, soil, and sediment from potentially hazardous waste sites to determine the presence or absence of certain environmentally harmful organic compounds. The methods described here all require the use of GC/MS. 

The EPA publishes Series Methods that describe the exact procedures to be followed with respect to sample receipt and handling, analytical methods, data reporting, and document control. These guidelines must be followed closely to ensure accuracy, reproducibility, and reliability within and among the contract laboratories. 

Scientific Apparatus Makers Association 1140 Coimecticut Avenue, NW Washington, D.C. 20036 Standards for analytical instmments, laboratory apparatus, measurement and test instmments, nuclear instmments, optical instmments, process measurement and control, and scientific laboratory furniture and equipment (see Analytical methods). 

High Performance Liquid Chromatography (hpic). Hplc is currently the fastest growing analytical method and is now available in many laboratories. DL-Analysis by hplc has already been described and hplc methods have been reviewed (122). 

Analytical and Laboratory Operations. Sulfamic acid has been recommended as a reference standard in acidimetry (55). It can be purified by recrystaUization to give a stable product that is 99.95 wt % pure. The reaction with nitrite as used in the sulfamic acid analytical method has also been adapted for determination of nitrites with the acid as the reagent. This reaction is used commercially in other systems for removal of nitrous acid impurities, eg, in sulfuric and hydrochloric acid purification operations. 

Modem analytical techniques have been developed for complete characteri2ation and evaluation of a wide variety of sulfonic acids and sulfonates. The analytical methods for free sulfonic acids and sulfonate salts have been compiled (28). Titration is the most straightforward method of evaluating sulfonic acids produced on either a laboratory or an iadustrial scale (29,30). Spectroscopic methods for sulfonic acid analysis iaclude ultraviolet spectroscopy, iafrared spectroscopy, and and nmr spectroscopy (31). Chromatographic separation techniques, such as gc and gc/ms, are not used for free... 

Analytical Methods. Most of the analytical and testing methods used for ethyl ether are conventional laboratory methods. Ethyl ether that is to be used for anesthetic purposes or in processes that involve heating or distiHation must be peroxide-free, and should pass the USP standard test with potassium iodide. This test detects approximately 0.001% peroxide as hydrogen peroxide. 

Inductively coupled plasma-mass spectrometry (ICP-MS) is a multielement analytical method with detection limits which are, for many trace elements, including the rare earth elements, better than those of most conventional techniques. With increasing availability of ICP-MS instalments in geological laboratories this method has been established as the most prominent technique for the determination of a large number of minor and trace elements in geological samples. 

B01 L.M. Barker and R.E. Hollenbach, J. Appl. Phys. 41, 4208-4226 (1970). 70B02 R.R. Boade, Experimental Shock Loading Properties of Porous Materials and Analytical Methods to Describe these Properties, Sandia Laboratories Report No. SC-DC-70-5052, August, 1970. 

Gas-liquid chromatography (GLC) finds many applications outside the chemistry laboratory. If you ve ever had an emissions test on the exhaust system of your car, GLC was almost certainly the analytical method used. Pollutants such as carbon monoxide and unbumed hydrocarbons appear as peaks on a graph such as that shown in Figure 1.7. A computer determines the areas under these peaks, which are proportional to the concentrations of pollutants, and prints out a series of numbers that tells the inspector whether your car passed or failed the test. Many of the techniques used to test people lor drugs (marijuana, cocaine, and others) or alcohol also make use of gas-liquid chromatography. 

Manual of Analytical Methods, J. F. Thompson, Ed. Quality Assurance Section, Chemistry Branch, EPA, Environmental Toxicology Division, Pesticides, Health Effects Research Laboratory, Research Triangle Park, NC 27711. 

This system includes measures and activities related to laboratory procedures, testing, analytical methods development and validation or verification, and the stability program. 

The objectives of this presentation are to discuss the general behavior of non isothermal chain-addition polymerizations and copolymerizations and to propose dimensionless criteria for estimating non isothermal reactor performance, in particular thermal runaway and instability, and its effect upon polymer properties. Most of the results presented are based upon work (i"8), both theoretical and experimental, conducted in the author s laboratories at Stevens Institute of Technology. Analytical methods include a Semenov-type theoretical approach (1,2,9) as well as computer simulations similar to those used by Barkelew LS) ... 

Reliability This encompasses factors such as the laboratory environment and organization, equipment design and maintenance, personnel training, skills and experience, design and handling of the analytical method, etc. 

---