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NOTE: Combination electrodes incorporating both measuring and referenced functions are <br /> convenient to use and are available with solid, gel-type filling materials that require <br /> minimal malintenance. <br /> 4.4 Magnetic stirrer and Teflon-coated stirring bar. <br /> 4.5 Thermometer and/or temperature sensor for automatic compensation. <br /> 5.0 REAGENTS <br /> 5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is <br /> intended that all reagents shall conform to the specifications of the Committee on Analytical <br /> Reagents of the Am rican Chemical Society, where such specifications are available. Other <br /> grades may be use , provided it is first ascertained that the reagent is of sufficiently high purity <br /> to permit its use wit out lessening the accuracy of the determination. <br /> 5.2 Primary standard buffer salts are available from the National Institute of Standards <br /> and Technology (NI T) and should be used in situations where extreme accuracy is necessary. <br /> Preparation of refer nce solutions from these salts requires some special precautions and <br /> handling, such as to -conductivity dilution water, drying ovens, and carbon-dioxide-free purge <br /> gas. These solution should be replaced at least once each month. <br /> 5.3 Second ry standard buffers may be prepared from NIST salts or purchased as <br /> solutions from co m ercial vendors. These commercially available solutions have been <br /> validated by compar son with NIST standards and are recommended for routine use. <br /> 6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING <br /> Samples shoul be analyzed as soon as possible. <br /> 7.0 PROCEDURE <br /> 7.1 Calibrati n <br /> 7.1.1 Because of the wide variety of pH meters and accessories, detailed <br /> operating proc dures cannot be incorporated into this method. Each analyst must be <br /> acquainted wit the operation of each system and familiar with all instrument functions. <br /> Special attenti n to care of the electrodes is recommended. <br /> 7.1.2 Each instrument/electrode system must be calibrated at a minimum of <br /> two points that racket the expected pH of the samples and are approximately three pH <br /> units or more apart. (For corrosivity characterization, the calibration of the pH meter <br /> should include 6 buffer of pH 2 for acidic wastes and a pH 12 buffer for caustic wastes; <br /> also, for corrosivity characterization, the sample must be measured at 25 ± 1 •C if the pH <br /> of the waste is Bove 12.0.) Various instrument designs may involve use of a dial (to <br /> "balance" or "st ndardize") or a slope adjustment, as outlined in the manufacturer's <br /> instructions. R peat adjustments on successive portions of the two buffer solutions until <br /> readings are wi I <br /> hin 0.05 pH units of the buffer solution value. <br /> 7.2 Place thsample or buffer solution in a clean glass beaker using a sufficient volume <br /> to cover the sensinglements of the electrodes and to give adequate clearance for the <br /> 9040C - 2 Revision 3 <br /> November 2004 <br />