This document has been replaced. View the most recent version. If sampling is for the precise determination of volatility, use Practice D in conjunction with this practice. For sample mixing and handling of samples, refer to Practice D The practice does not cover sampling of electrical insulating oils and hydraulic fluids.

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Environmental Protection Agency, have been grouped into seven series. These seven broad categories were established to facilitate further development and application of environmental technology. Elimination of traditional grouping was consciously planned to foster technology transfer and a maximum interface in related fields. The seven series are: 1. Environmental Health Effects Research 2. Environmental Protection Technology 3. Ecological Research 4. Environmental Monitoring 5. Socioeconomic Environmental Studies 6.

These studies relate to EPA's mission to protect the public health and welfare from adverse effects of pollutants associated with energy systems. The goal of the Program is to assure the rapid development of domestic energy supplies in an environ- mentally-compatible manner by providing the necessary environmental data and control technology. Investigations include analyses of the transport of energy-related pollutants and their health and ecological effects; assessments of, and development of, control technologies for energy systems; and integrated assessments of a wide range of energy-related environmental issues.

Approval does not signify that the contents necessarily reflect the views and policies of the Government, nor does mention of trade names or commercial products constitute endorsement or recommendation for use. This document is available to the public through the National Technical Information Service, Springfield, Virginia Davidson, W. Lyman, D. Shooter, and J. Valentine Arthur D. Little, Inc. Objectives 1 2. General Recommendations 2 3.

Contents of the Manual 3 4. Introduction 7 2. Sampling 8 3. Analysis Methods 9 4. Sampling 18 3. Analyses 19 4. Shale Oil 33 B. Coal Liquids 35 2. Sampling 37 3. Analyses 38 4. Sampling 52 3. Analyses 53 4. Coal 63 B. Coke 64 2. Sampling 65 A. Coal 65 B. Coke 66 3. Analyses 67 A. Coal 67 B. Coke 67 4.

Refuse-Derived Solid Fuels 75 B. Peat 76 2. Sampling 77 A. Refuse-Derived Solid Fuels 77 B. Peat 79 3. Analyses 79 A. Refuse-Derived Solid Fuels 79 B. Peat 80 4. The infor- mation given is basically a description and discussion of established methods of sampling analysis for a variety of hydrocarbon fuels. The analyses covered are those that are of prime concern to the engineer, or project director, involved in a pollution related research project.

The coverage of non-standard methods and of additional parameters that may be required in environmental assessments will be included in a forth- coming Level 2 sampling and analysis manual.

The non-standard methods will include, for example, those that are state-of-the-art or that use rapid instrumental techniques. The parameters added will be those yielding information on the chemical nature of the fuel e. This manual indicates what fuel analyses are normally required in connection with fuel-utilization research, and what established methods are applicable for the analysis.

If this manual serves only to point out the importance of methods specification in fuel analysis, it will have been of value. Too frequently, analyses of samples - including fuels - result in inaccurate or meaningless results because an inappro- priate method was used. It should not be assumed by the researcher or project director that the analytical laboratories Government or private will use the method that is both appropriate and standard.

There are, however, a large number of ASTM methods available for various fuels, including two or more alternative methods for many parameters, and the choice of the most applicable method is important. In addition, many standard methods, including some ASTM methods, leave certain options to the parties con- cerned - e.

If the researcher or project director does not specify the options to be used, the laboratories may run the test in an inappropriate manner. It is recommended that, such statements aside, the exact method of analysis be specified for every parameter by the re- searcher or project director. In many cases, the method chosen will be one that is routinely carried out by the laboratory, and this is a de- sirable feature.

If the laboratory indicates that it normally uses a different method for one or more of the parameters, then a determination must be made on the applicability of the method and the desirability of its use. One area where such determinations may be frequently required is that of instrumental methods for carbon, hydrogen, and nitrogen anal- yses. If the method normally used with the instrument is applicable for the fuel in question, then it may be desirable to use that instrumental method since it may result in time and cost savings.

If a large number of samples are to be analyzed by any such non-standard method, then steps should be taken to check both the accuracy and precision of the method. For each method of analysis listed - preferred plus alter- nates in many cases - the manual gives a summary of the method, a dis- cussion of its applicability, and information on the accuracy and preci- sion of the method, if known.

The main emphasis is on methods of anal- ysis; sampling methods are, in general, only discussed briefly. What is implied is a recommenda- tion over the other available methods based on considerations of appli- t cability, precision and accuracy, availability of detailed instructions, and current or expected usage. The criteria for the selection of methods to be included in this manual, and for the selection of "preferred" meth- i ods, are given in the following subsection. For a given research project, the parties con- cerned should use the given list as a starting point and then add or sub- tract parameters as the program's informational needs dictate.

The fuels covered in this manual are: gaseous fuels, coal and coke, coal liquids, shale oil, liquid petroleum fuels broken into several cate- gories , waste lubricating oil, methyl fuel, refuse-derived solid fuel from municipal refuse , and peat. Not all of the fuels covered are in commercial use, at present. These unconventional fuels were included, however, because of their likely use in the future and the need, there- fore, for research programs to be carried out on them.

Each subsequent chapter of this manual covers a fuel or fuel grouping. The introduction to each chapter defines the fuels being discussed, in- dicates the analyses covered and the preferred method of analysis , and gives other supplemental information about the fuel that may be of in- terest in any environmental assessment of processes using the fuel.

A section on sampling is given and is followed by the main section describ- ing the methods of analysis. References for each chapter are given at the end of the text portion of that chapter. Appendices give 1 information of the availability of Standard Reference Materials for fuel-related analyses; 2 a listing of laboratory direc- tories; 3 typical values ranges for the parameters specified for each fuel; and, 4 the results of fuel analysis tests conducted by the con- tractor and three analytical service laboratories.

Applicability of the method to the fuel in question; 2. The availability of the publication containing the method and the extent to which the method is currently used in laboratories con- ducting fuel analyses.

The considerations listed in 1 and 2 were dominant in most instances. No attempt was made - in the preparation of this manual - to review all available methods because of limitations on time and funds. If a parti- cular method was deemed applicable and "available", then it was consi- dered. No method was considered for inclusion in this manual unless it had been reported in sufficient detail in the open literature.

Addi- tionally, no attempt was made to resolve, by laboratory tests, the nu- merous uncertainties concerning the applicability of specified methods to fuels other than those the method was originally intended for. Some laboratory tests on unconventional fuels were carried out as part of this program see Appendix D , but the scope of these tests was insufficient to make a defensible decision on the applicability of the method used. The relatively small number of compounds possible in gaseous fuels has re- sulted in the development of methods for the identification and measure- ment of individual major and minor components using either gas chromato- graphy or mass spectrometry.

While standardized procedures for such mea- surements have been established, continuing improvements in instrumentation and chromatographic column technology have resulted in modified procedures which allow the analyses to be carried out more quickly and conveniently with no loss in precision or accuracy.

Laboratories which are very active in the area of gas analyses often develop and utilize procedures and equip- ment based upon these modifications and improvements before such improve- ments have been incorporated into standards such as the ASTM methods. Section 3 of this chapter provides additional in- formation on analytical procedures, as well as alternate methods.

A more complete listing and description of methods applicable to the various composition and physical property parameters is given in Table II Pressure in natural gas streams, for example, may vary from several thousands of pounds at the well-head and some transmission lines down to a few inches of water in service feed lines. In some industrial applications where the gasification process equipment is close to the end use, gases may be at temperatures above ambient.

Grab samples representative of the gas stream at one point in time are generally taken, although continuous, integrated samples can be obtained by use of a slow, regulated flow into a large sample container. In sampling from a pipe, or other vessel, it is generally good practice to use a sampling probe, or tip, which protrudes some distance into the vessel and away from the wall, in order to avoid any effects of condensation,or reaction at the wall which might alter the composition of the sample being taken.

In some cases, the product fuels may be hot and may still contain some amounts of sulfur compounds, higher hydro- carbons, and ammonia which have not been removed. When more than one method is available, the preferred method is listed first.


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Representative samples of petroleum and petroleum products are required for the determination of chemical and physical properties, which are used to establish standard volumes, prices, and compliance with commercial and regulatory specifications. The following concepts must be considered when selecting a specific sampling procedure. A series of spot samples may be combined to create a representative sample. In these cases, manual sampling is appropriate under the following conditions. The practice does not cover sampling of electrical insulating oils and hydraulic fluids.


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