Baixe Orgânicos não Halogenados usando GC/FID e outras Notas de estudo em PDF para Engenharia Ambiental, somente na Docsity! CD-ROM 8015B - 1 Revision 2 December 1996 METHOD 8015B NONHALOGENATED ORGANICS USING GC/FID 1.0 SCOPE AND APPLICATION 1.1 Method 8015 is used to determine the concentration of various nonhalogenated volatile organic compounds and semivolatile organic compounds by gas chromatography. The following compounds can be determined quantitatively by this method: Appropriate Technique Compound Name Purge-and- Direct Solvent CAS No. Trap Injection Extraction a Acetone 67-64-1 pp b,d I Acetonitrile 75-05-8 pp b,d I Acrolein 107-02-8 pp b,d I Acrylonitrile 107-13-1 pp b,d I Allyl alcohol 107-18-6 ht b,d I 1-Butanol (n-Butyl alcohol) 71-36-3 ht b,d I t-Butyl alcohol 75-65-0 pp b,d I 2-Chloroacrylonitrile (I.S.) 920-37-6 NA d NA Crotonaldehyde 123-73-9 pp b,d I Diethyl ether 60-29-7 b b I 1,4-Dioxane 123-91-1 pp b,d I Ethanol 64-17-5 I b,d I Ethyl acetate 141-78-6 I b,d I Ethylene glycol 107-21-1 I b I Ethylene oxide 75-21-8 I b,d I Hexafluoro-2-propanol (I.S.) 920-66-1 NA d NA Hexafluoro-2-methyl- 2-propanol (I.S.) 515-14-6 NA d NA Isobutyl alcohol 78-83-1 pp b,d I Isopropyl alcohol 67-63-0 pp b,d I Methanol 67-56-1 I b,d I Methyl ethyl ketone (MEK) 78-93-3 pp b,d I Methyl isobutyl ketone (MIBK) 108-10-1 pp b,d I N-Nitroso-di-n-butylamine 924-16-3 pp b,d b Paraldehyde 123-63-7 pp b,d I 2-Pentanone 107-87-9 pp b,d I 2-Picoline 109-06-8 pp b,d I 1-Propanol 71-23-8 pp b,d I Propionitrile 107-12-0 ht d I CD-ROM 8015B - 2 Revision 2 December 1996 Appropriate Technique Compound Name Purge-and- Direct Solvent CAS No. Trap Injection Extraction a Pyridine 110-86-1 I b,d b o-Toluidine 95-53-4 I b,d b Chemical Abstract Services Registry Number.a b Adequate response using this technique d Amenable to concentration by azeotropic distillation (Method 5031) ht Method analyte only when purged at 80EC I Inappropriate technique for this analyte pp Poor purging efficiency, resulting in high EQLs NA Not available I.S. Internal standard appropriate for Method 5031 1.2 This method may also be applicable to the analysis of petroleum hydrocarbons, including gasoline range organics (GROs) and diesel range organics (DROs). GROs correspond to the range of alkanes from C to C and covering a boiling point range of approximately 60EC - 170EC6 10 (Reference 6). DROs correspond to the range of alkanes from C to C and covering a boiling point10 28 range of approximately 170EC - 430EC (Reference 6). The identification of specific fuel types may be complicated by environmental processes such as evaporation, biodegradation, or when more than one fuel type is present. Methods from other sources may be more appropriate for GROs and DROs, since these hydrocarbons are not regulated under RCRA. Consult State and local regulatory authorities for specific requirements. 1.3 This method is restricted for use by, or under the supervision of, analysts experienced in the use of gas chromatographs and skilled in the interpretation of gas chromatograms. In addition, if this method is used for the analysis of petroleum hydrocarbons, it is limited to analysts experienced in the interpretation of hydrocarbon data. Each analyst must demonstrate the ability to generate acceptable results with this method. 1.4 The method can also be used as a screening tool (for both volatile and semivolatile organics) to obtain semiquantitative data for the prevention of sample overload during quantitative analysis on a GC/MS system. This may be accomplished using an automated (Method 5021) headspace method or by direct injection if a solvent extraction method has been utilized for sample preparation. Single point calibration would be acceptable in this situation. Performance data are not provided for screening. 2.0 SUMMARY OF METHOD 2.1 Method 8015 provides gas chromatographic conditions for the detection of certain nonhalogenated volatile and semivolatile organic compounds. 2.1.1 Samples may be introduced into the GC: @ following solvent extraction (Methods 3510, 3520, 3540, 3541, 3545, 3550, or 3560) CD-ROM 8015B - 5 Revision 2 December 1996 4.3.2 Microsyringes - 10- and 25-µL with a 0.006 in. ID needle (Hamilton 702N or equivalent) and 100-µL. 4.4 Volumetric flasks, Class A - Appropriate sizes with ground glass stoppers. 4.5 Analytical balance - 0 - 160 g capacity, capable of measuring differences of 0.0001 g. 5.0 REAGENTS 5.1 Reagent grade chemicals shall be used whenever possible. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 5.2 Organic-free reagent water - All references to water in this method refer to organic-free reagent water, as defined in Chapter One. 5.3 Methanol, CH OH. Pesticide quality or equivalent. Store away from other solvents.3 5.4 Fuels, e.g., gasoline or diesel. Purchase from a commercial source. Low boiling components in fuel evaporate quickly. If available, obtain fuel from the leaking tank on site. 5.5 Alkane standard. A standard containing a homologous series of n-alkanes for establishing retention times (e.g., C -C for diesel). 10 32 5.6 Stock standards - Stock solutions may be prepared from pure standard materials or purchased as certified solutions. When methanol is a target analyte or when using azeotropic distillation for sample preparation, standards should not be prepared in methanol. Standards must be replaced after 6 months or sooner, if comparison with check standards indicates a problem. 5.7 Secondary dilution standards - Using stock standard solutions, prepare secondary dilution standards, as needed, that contain the compounds of interest, either singly or mixed together. The secondary dilution standards should be prepared at concentrations such that the aqueous calibration standards prepared in Sec. 5.8 will bracket the working range of the analytical system. Secondary dilution standards should be stored with minimal headspace for volatiles and should be checked frequently for signs of degradation or evaporation, especially just prior to preparing calibration standards from them. 5.8 Calibration standards - Calibration standards at a minimum of five different concentrations are prepared in water (purge-and-trap or direct injection) or in methylene chloride (solvent injection) from the secondary dilution of the stock standards. One of the standards should be at or below the concentration equivalent to the appropriate quantitation limit for the project. The remaining concentrations should correspond to the expected range of concentrations found in real samples or should define the working range of the GC. Each standard should contain each analyte for detection by this method (e.g., some or all of the compounds listed in Sec. 1.1 may be included). Volatile organic standards are prepared in organic-free reagent water. In order to prepare accurate aqueous standard solutions, the following precautions must be observed: 5.8.1 Do not inject more than 20 µL of methanolic standards into 100 mL of water. CD-ROM 8015B - 6 Revision 2 December 1996 5.8.2 Use a 25-µL Hamilton 702N microsyringe or equivalent (variations in needle geometry will adversely affect the ability to deliver reproducible volumes of methanolic standards into water). 5.8.3 Rapidly inject the primary standard into the filled volumetric flask. Remove the needle as fast as possible after injection. 5.8.4 Mix diluted standards by inverting the flask three times only. 5.8.5 Fill the sample syringe from the standard solution contained in the expanded area of the flask (do not use any solution contained in the neck of the flask). 5.8.6 Never use pipets to dilute or transfer samples or aqueous standards when diluting volatile organic standards. 5.8.7 Aqueous standards used for purge-and-trap analyses (Method 5030) are not stable and should be discarded after 1 hour, unless held in sealed vials with zero headspace. If so stored, they may be held for up to 24 hours. Aqueous standards used for azeotropic distillation (Method 5031) may be stored for up to a month in polytetrafluoroethylene (PTFE)- sealed screw-cap bottles with minimal headspace, at 4EC, and protected from light. 5.9 Internal standards (if internal standard calibration is used) - To use this approach, the analyst must select one or more internal standards that are similar in analytical behavior to the compounds of interest. The analyst must further demonstrate that the measurement of the internal standard is not affected by method or matrix interferences. Because of these limitations, no internal standard can be suggested that is applicable to all samples. The following internal standards are recommended when preparing samples by azeotropic distillation: 2-chloroacrylonitrile, hexafluoro-2-propanol and hexafluoro-2-methyl-2-propanol. 5.10 Surrogate standards - Whenever possible, the analyst should monitor both the performance of the analytical system and the effectiveness of the method in dealing with each sample matrix by spiking each sample, standard, and blank with one or two surrogate compounds which are not affected by method interferences. 6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING See the introductory material to this chapter, Organic Analytes, Sec. 4.1. 7.0 PROCEDURE 7.1 Introduction/preparation methods Various alternate methods are provided for sample introduction. All internal standards, surrogates, and matrix spikes (when applicable) must be added to samples before introduction into the GC/FID system. Follow the introduction method on when to add standards. CD-ROM 8015B - 7 Revision 2 December 1996 7.1.1 Direct injection - This involves direct syringe injection into the GC injection port. 7.1.1.1 Volatile organics (includes gasoline range organics [GROs]) This may involve injection of an aqueous sample containing a very high concentration of analytes; injection of aqueous concentrates from Method 5031 (azeotropic distillation for nonpurgeable volatile organics); and injection of an organic solvent waste. Direct injection of aqueous samples (non-concentrated) has very limited applications. It is only permitted for the determination of volatiles at the toxicity characteristic (TC) regulatory limits or at concentrations in excess of 10,000 µg/L. It may also be used in conjunction with the test for ignitability in aqueous samples (along with Methods 1010 and 1020) to determine if alcohol is present at > 24%. 7.1.1.2 Semivolatile organics (includes diesel range organics [DROs]) This may involve syringe injection of extracts of aqueous samples prepared by Methods 3510 or 3520 or extracts of soil/solids prepared by Methods 3540, 3541, 3545, 3550 or 3560. WARNING: Ultrasonic extraction (Method 3550) is not as rigorous a method as the other extraction methods for soil/solids. This means it is very critical that the method be followed explicitly to achieve extraction efficiency which approaches that of Soxhlet extraction. Consult Method 3550 for information on the critical aspects of this extraction procedure. 7.1.2 Purge and trap - this includes purge and trap for aqueous samples (Method 5030) and purge and trap for solid samples (Method 5035). Method 5035 also provides techniques for extraction of solid and oily waste samples by methanol (and other water miscible solvents) with subsequent purge and trap from an aqueous matrix using Method 5030. Normally purge and trap for aqueous samples is performed at ambient temperatures while soil/solid samples utilize a 40EC purge to improve extraction efficiency. Occasionally, there may be a need to perform a heated purge for aqueous samples to lower detection limits; however, a 25-mL sample should provide the sensitivity needed in most situations. 7.1.3 Vacuum distillation - this is a device for the introduction of volatile organics from aqueous, solid or tissue samples (Method 5032) into the GC/FID system. 7.1.4 Automated static headspace - this is a device for the introduction of volatile organics from solid samples (Method 5021) into the GC/FID system. 7.2 Chromatographic conditions (recommended) 7.2.1 Column 1 Carrier gas (Helium) flow rate: 40 mL/min Temperature program: Initial temperature: 45EC, hold for 3 minutes Program: 45EC to 220EC at 8EC/min Final temperature: 220EC, hold for 15 minutes. CD-ROM 8015B - 10 Revision 2 December 1996 7.3.4.1 If the percent relative standard deviation (%RSD) of the calibration factor is less than 20% over the working range, linearity through the origin can be assumed, and the average calibration factor can be used in place of a calibration curve. 7.3.4.2 If the % RSD is more than 20% over the working range, linearity through the origin cannot be assumed. See Method 8000 for other calibration options that may be employed. 7.4 Retention time windows Single component target analytes (see Sec. 1.1) are identified on the basis of retention time windows. GROs and DROs are distinguished on the basis of the ranges of retention times for characteristic components in each type of fuel. 7.4.1 Before establishing retention time windows, make sure that the chromatographic system is functioning reliably and that the operating parameters have been optimized for the target analytes and surrogates in the sample matrix to be analyzed. Establish the retention time windows for single component target analytes using the procedure described in Sec. 7.0 of Method 8000. 7.4.2 The retention time range for GROs is defined during initial calibration. Two specific gasoline components are used to establish the range, 2-methylpentane and 1,2,4- trimethylbenzene. Use the procedure described in Sec. 7.0 of Method 8000 to establish the retention time windows for these two components. The retention time range is then calculated based on the lower limit of the RT window for the first eluting component and the upper limit of the RT window for the last eluting component. 7.4.3 The retention time range for DROs is defined during initial calibration. The range is established from the retention times of the C and C alkanes. Use the procedure10 28 described in Sec. 7.0 of Method 8000 to establish the retention time windows for these two components. The retention time range is then calculated based on the lower limit of the RT window for the first eluting component and the upper limit of the RT window for the last eluting component. 7.5 Calibration verification 7.5.1 The working calibration curve, and retention times must be verified at the beginning of each 12-hour work shift as a minimum requirement. Verification is accomplished by the measurement of one or more calibration standards (normally mid-concentration) that contain all of the target analytes and surrogates when individual target analytes are being analyzed. Verification is accomplished by the measurement of the fuel standard and the hydrocarbon retention time standard when petroleum hydrocarbons are being analyzed. Additional analyses of the verification standard(s) throughout a 12-hour shift are strongly recommended, especially for samples that contain visible concentrations of oily material. See Sec. 7.0 "calibration verification" of Method 8000 for more detailed information. 7.5.2 Calculate the % difference as detailed in Sec. 7.0 of Method 8000. If the response for any analyte is within ±15% of the response obtained during the initial calibration, then the initial calibration is considered still valid, and analyst may continue to use the mean CF or RF values from the initial calibration to quantitate sample results. For analyses employing azeotropic distillation as the sample introduction technique, the % difference may be up to ±20%. If the response for any analyte varies from the predicted response by more CD-ROM 8015B - 11 Revision 2 December 1996 than ±15% (±20% for azeotropic distillation), corrective action must be taken to restore the system or a new calibration curve must be prepared for that compound. 7.5.3 All target analytes and surrogates or n-alkanes in the calibration verification analyses must fall within previously established retention time windows. If the retention time of any analyte does not fall within the ± 3F window, corrective action must be taken to restore the system or a new calibration curve must be prepared for that compound. 7.5.4 Solvent blanks and any method blanks should be run with calibration verification analyses to confirm that laboratory contamination does not cause false positives. 7.6 Gas chromatographic analysis 7.6.1 Samples are analyzed in a set referred to as an analysis sequence. The sequence begins with calibration verification followed by sample extract analyses. Additional analyses of the verification standard(s) throughout a 12-hour shift are strongly recommended, especially for samples that contain visible concentrations of oily material. A verification standard is also necessary at the end of a set. The sequence ends when the set of samples has been injected or when retention time and/or % difference QC criteria are exceeded. If the criteria are exceeded, inspect the gas chromatographic system to determine the cause and perform whatever maintenance is necessary before recalibrating and proceeding with sample analysis. All sample analyses performed using external standard calibration must be bracketed with acceptable data quality analyses (e.g., calibration and retention time criteria). Therefore, all samples must be reanalyzed that fall within the standard that exceeded criteria and the last standard that was acceptable. 7.6.2 Samples are analyzed with the same instrument configuration as is used during calibration. When using Method 5030 for sample introduction, analysts are cautioned that opening a sample vial or drawing an aliquot from a sealed vial (thus creating headspace) will compromise samples analyzed for volatiles. Therefore, it is recommended that analysts prepare two samples for purge-and-trap analysis. The second sample can be stored for 24 hours to ensure that an uncompromised sample is available for analysis or dilution, if the analysis of the first sample is unsuccessful or if results exceed the calibration range of the instrument. Distillates from Method 5031 may be split into two portions and held at 4EC prior to analysis. It is recommended that the distillate be analyzed within 24 hours of distillation. Distillates must be analyzed within 7 days of distillation. 7.6.3 Sample concentrations are calculated by comparing sample response data with the initial calibration of the system (Sec. 7.3). Therefore, if sample response exceeds the limits of the initial calibration range, a dilution of the sample must be analyzed. For volatile organic aqueous samples, the dilution must be performed on a second aliquot of the sample which has been properly sealed and stored prior to use and reanalysis. Extracts should be diluted so that all peaks are on scale, as overlapping peaks are not always evident when peaks are off scale. Computer reproduction of chromatograms, manipulated to ensure all peaks are on scale over a 100-fold range, are acceptable as long as calibration limits are not exceeded. Peak height measurements are recommended over peak area integration when overlapping peaks cause errors in area integration. 7.6.4 Tentative identification of a single component analyte occurs when a peak from a sample extract falls within the daily retention time window. Confirmation is required on a second column or by GC/MS. Since the flame ionization detector is non-specific, it is highly CD-ROM 8015B - 12 Revision 2 December 1996 recommended that GC/MS confirmation be performed on single component analytes unless historical data are available to support the identification(s). 7.6.5 Second column confirmation is generally not necessary for petroleum hydrocarbon analysis. However, if analytical interferences are indicated, analysis using the second GC column is required. Also, the analyst must ensure that the sample hydrocarbons fall within the retention time range established during the initial calibration. NOTE: Identification of fuels, especially gasoline, is complicated by their inherent volatility. The early eluting compounds in fuels are obviously the most volatile and the most likely to have weathered unless sampled immediately following a spill. The most highly volatile fraction of gasoline constitutes 50% of the total peak area of a gasoline chromatogram. This fraction is least likely to be present in an environmental sample or present in only very low concentration in relation to the remainder of a gasoline chromatogram. 7.6.6 The performance of the entire analytical system should be checked every 12 hours, using data gathered from analyses of blanks, standards, and replicate samples. Significant peak tailing must be corrected. Tailing problems are generally traceable to active sites on the column, cold spots in a GC, the detector operation, or leaks in the system. See Sec. 7.9 for GC/FID system maintenance. Follow manufacturer's instructions for maintenance of the introduction device. 7.7 Calculations 7.7.1 The concentration of each analyte in the sample may be determined by calculating the amount of standard purged or injected, from the peak response, using the calibration curve or the mean CF or RF from the initial curve. 7.7.2 While both diesel fuel and gasoline contain a large number of compounds that will produce well resolved peaks in a GC/FID chromatogram, both fuels contain many other components that are not chromatographically resolved. This unresolved complex mixture results in the "hump" in the chromatogram that is characteristic of these fuels. In addition, although the resolved peaks are important for the identification of the specific fuel type, the area of the unresolved complex mixture contributes a significant portion of the area of the total response. 7.7.2.1 For the analysis of DROs, sum the area of all peaks eluting between C10 and C . This area is generated by projecting a horizontal baseline between the retention28 times of C and C . 10 28 7.7.2.2 Because the chromatographic conditions employed for DRO analysis can result in significant column bleed and a resulting rise in the baseline, it is appropriate to perform a subtraction of the column bleed from the area of the DRO chromatogram. In order to accomplish this subtraction, a methylene chloride blank should be analyzed during each 12-hour analytical shift during which samples are analyzed for DROs. The area of this chromatogram is measured in the same fashion as is used for samples (see Sec. 7.7.2.1), by projecting a horizontal baseline across the retention time range for DROs. This area is then subtracted from the area measured for the sample and the difference in areas is used to calculate the DRO concentration, using the equations in Method 8000. CD-ROM 8015B - 15 Revision 2 December 1996 potential problem due to the sample matrix itself, the LCS results are used to verify that the laboratory can perform the analysis in a clean matrix. 8.4.3 See Method 8000, Sec. 8.0 for the details on carrying out sample quality control procedures for preparation and analysis. 8.5 Surrogate recoveries - The laboratory must evaluate surrogate recovery data from individual samples versus the surrogate control limits developed by the laboratory. See Method 8000, Sec. 8.0 for information on evaluating surrogate data and developing and updating surrogate limits. 8.6 It is recommended that the laboratory adopt additional quality assurance practices for use with this method. The specific practices that are most productive depend upon the needs of the laboratory and the nature of the samples. Whenever possible, the laboratory should analyze standard reference materials and participate in relevant performance evaluation studies. 9.0 METHOD PERFORMANCE 9.1 Specific method performance information for non-purgeable volatiles prepared using the azeotropic microdistillation technique from Method 5031 is included in Tables 1, 3 and 4 for aqueous matrices and in Tables 2 and 5 for solid matrices. 9.2 Specific method performance information is provided for diesel fuel spiked into soil in Tables 6 and 7. 10.0 REFERENCES 1. Bellar, T.A., and J.J. Lichtenberg. "Determining Volatile Organics at Microgram-per-Liter Levels by Gas Chromatography", J. Amer. Water Works Assoc., 66(12), pp. 739-744 (1974). 2. Bellar, T.A., and J.J. Lichtenberg. "Semi-Automated Headspace Analysis of Drinking Waters and Industrial Waters for Purgeable Volatile Organic Compounds", in Van Hall, ed., Measurement of Organic Pollutants in Water and Wastewater, ASTM STP 686, pp. 108-129, 1979. 3. Development and Application of Test Procedures for Specific Organic Toxic Substances in Wastewaters: Category 11 - Purgeables and Category 12 - Acrolein, Acrylonitrile, and Dichlorodifluoromethane, Report for EPA Contract 68-03-2635. 4. Bruce, M.L., R.P. Lee, and M.W. Stevens. "Concentration of Water Soluble Volatile Organic Compounds from Aqueous Samples by Azeotropic Microdistillation", Environ. Sci. Technol. 1992, 26, 160-163. 5. Tsang, S.F., N. Chau, P.J. Marsden, and K.R. Carter. "Evaluation of the EnSys PETRO RISc kit for TPH", Report for Ensys, Inc., Research Triangle Park, NC, 27709, 1992. 6. "Interlaboratory Study of Three Methods for Analyzing Petroleum Hydrocarbons in Soils," API Publication Number 4599, American Petroleum Institute, March 1994. CD-ROM 8015B - 16 Revision 2 December 1996 TABLE 1 METHOD DETECTION LIMITS FOR NON-PURGEABLE VOLATILE COMPOUNDS IN AQUEOUS MATRICES BY AZEOTROPIC MICRODISTILLATION (METHOD 5031) MDL (µg/L)a Analyte Reagent Water Ground Water TCLP Leachate Acetone 48 16 63b Acetonitrile 15 6 14 Acrolein 13 15 7 Acrylonitrile 8 9 14 1-Butanol 14 8 7 t-Butyl alcohol 8 7 17 1,4-Dioxane 12 15 16 Ethanol 18 12 13 Ethyl acetate 9 8 16 Ethylene oxide 8 9 10 Isobutyl alcohol 11 8 4 Isopropyl alcohol 18 17 7 Methanol 21 21 22 Methyl ethyl ketone 4 5 9 Methyl isobutyl ketone 4 2 8 2-Pentanone 2 2 7 1-Propanol -- 7 -- Propionitrile 10 6 13 Pyridine 11 9 21 Produced by analysis of 7 aliquots of water spiked at 25 µg/L, using internal standarda calibration. Problematic due to transient laboratory contamination.b CD-ROM 8015B - 17 Revision 2 December 1996 TABLE 2 METHOD DETECTION LIMITS FOR NON-PURGEABLE VOLATILE COMPOUNDS IN SOLID MATRICES BY AZEOTROPIC MICRODISTILLATION (METHOD 5031) MDL (mg/kg) Analyte Incinerator Ash Kaolin Acrylonitrile 0.42 0.09 1-Butanol 0.23 0.09 t-Butyl alcohol 0.34 0.13 1,4-Dioxane 0.31 0.16 Ethanol 0.47 0.19 Ethyl acetate 0.18 0.07 Isopropyl alcohol 0.40 0.19 Methanol 0.46 0.31 Methyl ethyl ketone 0.27 0.12 Methyl isobutyl ketone 0.12 0.05 2-Pentanone 0.16 0.07 Pyridine 0.20 0.08 The MDLs calculated for this table were produced by the analysis of 7 replicates spiked at 0.50 mg/kg, using internal standard calibration. CD-ROM 8015B - 20 Revision 2 December 1996 TABLE 5 METHOD PERFORMANCE DATA FOR NON-PURGEABLE VOLATILE COMPOUNDS IN SOLID MATRICES BY AZEOTROPIC MICRODISTILLATION (METHOD 5031) Incinerator Ash Kaolin Low Conc. High Conc. Low Conc. High Conc.a b a b Average Average Average Averagec c c c %Rec %RSD %Rec %RSD %Rec %RSD %Rec %RSD Acrylonitrile 50 53 10 31 102 6 12 52 1-Butanol 105 14 61 12 108 5 58 25 t-Butyl alcohol 101 21 60 13 97 9 59 23 1,4-Dioxane 106 19 48 18 105 10 48 25 Ethanol 117 25 52 20 108 11 48 24 Ethyl acetate 62 19 39 12 90 5 41 25 Isopropyl alcohol 119 21 61 15 108 11 58 24 Methanol 55 53 33 28 117 17 37 22 Methyl ethyl ketone 81 21 40 12 91 8 42 20 Methyl isobutyl ketone 68 11 57 14 71 5 55 23 2-Pentanone 79 13 54 10 91 5 54 19 Pyridine 52 24 44 20 50 10 49 31 0.5 mg/kg spikes, using internal calibration.a 25 mg/kg spikes, using internal calibration.b Average of 7 replicatesc CD-ROM 8015B - 21 Revision 2 December 1996 TABLE 6 RESULTS FROM ANALYSIS OF LOW AROMATIC DIESEL BY GC/FIDa b (5 replicates/test) Spike Concentration Analysis Results 12.5 ppm ND 75 ppm 54 ± 7 ppm 105 ppm 90 ± 15 ppm 150 ppm 125 ± 12 ppm 1000 ppm 960 ± 105 ppm Samples were prepared using 2 g aliquots of sandy loam soil spiked with knowna amounts of low aromatic diesel. Extractions were accomplished using methylene chloride as a solvent (Method 3550, high concentration option). Low aromatic diesel is sold in California (Section 2256, CCR). For this study it wasb purchased at a gas station in San Diego, California. TABLE 7 RESULTS FROM ANALYSIS OF LOW AROMATIC DIESEL BY GC/FIDa b (5 replicates/test) Spike Concentration Analysis Results 25 ppm 51.2 ± 6.4 ppm 75 ppm 75.9 ± 7.8 ppm 125 ppm 98.9 ± 5.2 ppm 150 ppm 162 ± 10.4 ppm Samples were prepared using 10 g aliquots of sandy loam soil spiked with knowna amounts of regular #2 diesel purchased at a gas station in Northern Virginia. Extractions were accomplished using methylene chloride as a solvent (Method 3550). CD-ROM 8015B-22 Revision 2 December 1996 FIGURE 1 CHROMATOGRAM OF A 300 PPM GASOLINE STANDARD CD-ROM 8015B - 25 Revision 2 December 1996 FIGURE 4 CHROMATOGRAM OF SEVERAL NONPURGEABLE VOLATILE COMPOUNDS IN SPIKED REAGENT WATER USING AZEOTROPIC MICRODISTILLATION (METHOD 5031) CD-ROM 8015B - 26 Revision 2 December 1996 FIGURE 5 CHROMATOGRAM OF SEVERAL NONPURGEABLE VOLATILE COMPOUNDS IN SPIKED REAGENT WATER USING AZEOTROPIC MICRODISTILLATION (METHOD 5031) CD-ROM 8015B - 27 Revision 2 December 1996 METHOD 8015B NONHALOGENATED ORGANICS USING GC/FID