METHOD 8015D
NONHALOGENATED ORGANICS USING GC/FID
1.0SCOPE AND APPLICATION
1.1This method may be ud to determine the concentrations of various nonhalogenated volatile organic compounds and mivolatile organic compounds by gas chromatography. The following compounds have been determined quantitatively by this method, using the preparative techniques indicated.
Compound CAS No.a Purge-
and-Trap b Head-
早上起来恶心干呕space e
Direct
Aqueous
白玫瑰花语Injection
Azeo.
Dist.c
Vacuum
Dist.d
Acetonitrile75-05-8pp ne x x ne Acrolein107-02-8pp ne x x x Acrylonitrile107-13-1pp ne x x x Allyl alcohol107-18-6ht ne x x ne t-Amyl alcohol (TAA)75-85-4ht x ne ne x t-Amyl ethyl ether (TAEE)919-94-8x/ ht x ne ne x t-Amyl methyl ether (TAME)994-05-8x/ ht x ne ne x Benzene71-43-2x x ne ne x t-Butyl alcohol (TBA)75-65-0ht x x x x Crotonaldehyde123-73-9pp ne x x ne Diethyl ether60-29-7x ne x ne ne Diisopropyl ether (DIPE)108-20-3x/ ht x ne ne x Ethanol64-17-5I x x x x Ethyl acetate141-78-6I x x x ne Ethyl Benzene100-41-4x x ne ne x Ethylene oxide75-21-8I ne x x ne Ethyl tert-butyl ether (ETBE)637-92-3x/ ht x ne ne x Isopropyl alcohol (2-Propanol)67-63-0pp x x x ne Methanol67-56-1I x x x ne Methyl ethyl ketone (MEK,
2-Butanone)
强制进入qq空间78-93-3pp x x x x
Methyl tert-butyl ether (MTBE)1634-04-4x/ ht x x ne x N-Nitroso-di-n-butylamine924-16-3pp ne x x ne Paraldehyde123-63-7pp ne x x ne 2-Pentanone107-87-9pp x x x ne 2-Picoline109-06-8pp ne x x ne 1-Propanol (n-Propyl alcohol)71-23-8pp x x x ne Propionitrile107-12-0ht ne x x ne Pyridine110-86-1I ne x x ne Toluene108-88-3x x ne ne x
Compound
CAS No.a
Purge-and-Trap b
Head-space e
Direct Aqueous Injection
Azeo.Dist.c Vacuum Dist.d
o -Toluidine 95-53-4I ne x x ne o -Xylene 95-47-6x x ne ne x m -Xylene 108-38-3x x ne ne x p -Xylene 106-42-3
x
x
ne
ne
x
a Chemical Abstracts Service Registry Number
b Purge-and-Trap (Methods 5030 or 5035)
c Azeotropic distillation (Metho两地汤组成
d 5031)d Vacuum distillation (Method 5032)
e Headspace (Method 5021)
x Adequate respon using this technique耳机灵敏度
ht Method analyte only when purged at 80 E C (high temperature purge)
I Inappropriate technique for this analyte ne Not evaluated
pp
Poor purging efficiency, resulting in higher quantitation limits. U of an alternative sample preparative method is strongly recommended. May be amenable to purging at elevated temperature.
河车大造丸1.2This method is applicable to the analysis of other analytes, including triethylamine and petroleum hydrocarbons. The petroleum hydrocarbons include gasoline range organics (GRO) and diel range organics (DRO). The sample preparation techniques are shown in the table below.
Appropriate Technique
Compound
CAS No.a
Purge-and-Trap
Head-space Direct Aqueous Injection
Solvent Extraction
Triethylamine
121-44-8I ne x I Gasoline range organics (GRO)--x x x I Diel range organics (DRO)--
I
x
I
x
a Chemical Abstracts Service Registry Number x Adequate respon using this technique I Inappropriate technique for this analyte ne
Not evaluated
1.2.1This method has been applied to the analysis of triethylamine in water
samples by direct aqueous injection onto a different GC column than is ud for any other analytes. Descriptions of the GC column, temperature program, and performance data for triethylamine are provided in this method (e Secs. 6.2.5 and 11.2.6, and Table 8).1.2.2GRO corresponds to the range of alkanes from C 6 to C 10 and covering a
boiling point range of approximately 60E C - 170E C (Reference 6). DRO corresponds to the range of alkanes from C 10 to C 28 and covering a boiling point range of approximately 170E C -
430E C (Reference 6). The quantitative analys of the fuel types are bad on the procedures described in Sec. 11.11. The identification of specific fuel types may be complicated by environmental process such as evaporation, biodegradation, or when more than one fuel type is prent. Methods from other sources may be more appropriate for GRO and DRO, since the hydrocarbons are not regulated under RCRA. Consult State and local regulatory authorities for specific requirements.
1.2.3This method may be applicable to class of analytes and to fuel types and
petroleum hydrocarbons other than tho listed in Secs. 1.1 and 1.2. However, in order to be ud for additional analytes, fuel types, or petroleum hydrocarbons, the analyst must demonstrate that the
gas chromatographic conditions, including the GC column, are appropriate for the analytes of interest. The analyst must also perform the initial demonstration of proficiency described in Sec. 9.6 and Method 8000. Expansion of this method to other fuel types or petroleum hydrocarbons will also require that the boiling point range or carbon number range of the material be carefully defined and the quantitation approach be modified to match such ranges. Analysts are advid to consult authoritative sources, such as the American Petroleum Institute (API), for appropriate definitions of other fuel types or petroleum fractions.
NOTE:Mention of the analys of other fuel types and petroleum fractions does not imply a regulatory requirement for such analys, using this or any other method.
1.3The method can also be ud as a screening tool (for both volatile and mivolatile organics) to obtain miquantitative data to prevent overloading the GC/MS system during quantitative analysis. This may be accomplished using a purge-and-trap method (e.g., Method 5030), an automated headspace method (e.g., Method 5021), direct aqueous injection, or by direct injection, if a solvent extraction method has been utilized for sample preparation. Single-point calibration is acceptable in this situation. Performance data are not provided for screening.
什么地讨论1.4Prior to employing this method, analysts are advid to consult the ba method for each type of procedure that may be employed in the overall analysis (e.g., Methods 3500, 3600, 5000, and 8000) for additional information on quality control procedures, development of QC acceptance criteria, calculations, and general guidance. Analysts also should consult the disclaimer statement at the front of the manual and the information in Chapter Two for guidance on the intended flexibility in the choice of methods, apparatus, materials, reagents, and supplies, and on the responsibilities of the analyst for demonstrating that the techniques employed are appropriate for the analytes of interest, in the matrix of interest, and at the levels of concern.
安阳宾馆In addition, analysts and data urs are advid that, except where explicitly required in a regulation, the u of SW-846 methods is not mandatory in respon to Federal testing requirements. The information contained in this method is provided by EPA as guidance to be ud by the analyst and the regulated community in making judgments necessary to generate results that meet the data quality objectives for the intended application.
1.5This method is restricted for u by, or under the supervision of, analysts experienced in the u of a gas chromatograph and skilled in the interpretation of gas chromatograms. In addition, if this method is ud for the analysis of petroleum hydrocarbons, it is limited to analysts experienced in th
e interpretation of hydrocarbon data. Each analyst must demonstrate the ability to generate acceptable results with this method.
2.0SUMMARY OF METHOD
2.1This method provides gas chromatographic conditions for the detection of certain nonhalogenated volatile and mivolatile organic compounds.
2.2Depending on the analytes of interest, samples may be introduced into the GC by a variety of techniques, including:
•Purge-and-trap (Methods 5030 or 5035)
•Equilibrium headspace (Method 5021)
•Direct injection of aqueous samples
•Injection of the concentrate from azeotropic distillation (Method 5031)
•Vacuum distillation (Method 5032)
•Following solvent extraction (Methods 3510, 3520, 3535, 3540, 3541, 3545, 3546, 3550, 3560, or other appropriate technique)
2.3Groundwater or surface water samples generally must be analyzed in conjunction with Methods 5021, 5030, 5031, 5032, 3510, 3520, or other appropriate preparatory methods to obtain the necessary quantitation limits. Method 3535 (solid-pha extraction) may also be applicable to some of the target analytes, but has not been validated by EPA in conjunction with this determinative method.
2.4Samples to be analyzed for diel range organics may be prepared by an appropriate solvent extraction method.
2.5Gasoline range organics may be introduced into the GC/FID by purge-and-trap (Methods 5030 and 5035), automated headspace (Method 5021), vacuum distillation (Method 5032), or other appropriate technique.
2.6Triethylamine may be analyzed by direct injection of aqueous samples. This compound has not been found to be amenable to purge-and-trap techniques.
2.7An appropriate column and temperature program are ud in the gas chromatograph to parate the organic compounds. Detection is achieved by a flame ionization detector (FID).
2.8The method allows the u of packed or capillary columns for the analysis and confirmation of the non-halogenated individual analytes. The GC columns and conditions listed have been demonstrated to provide paration of tho target analytes. Other columns and conditions may be employed, provided that the analyst demonstrates adequate performance for the intended application.
2.9The quantitative analys of GRO and DRO are bad on the definitions provided in Sec. 1.2.2 and the procedures described in Sec. 11.11.
2.10Given the large number of components to be parated, fud-silica capillary columns are necessary for the analysis of petroleum hydrocarbons, including GRO and DRO, and are recommended for all other analytes. A capillary column is also necessary for the analysis of triethylamine.
3.0 DEFINITIONS
Refer to the SW-846 chapter of terms and acronyms for potentially applicable definitions.
4.0INTERFERENCES
4.1Solvents, reagents, glassware, and other sample processing hardware may yield artifacts and/or interferences to sample analysis. All the materials must be demonstrated to be free from interferences under the conditions of the analysis by analyzing method blanks. Specific lection of reagents and purification of solvents by distillation in all-glass systems may be necessary. Refer to each method for specific guidance on quality control procedures and to Chapter Four for guidance on the cleaning of glassware.
4.2When analyzing for volatile organics, samples can be contaminated by diffusion of volatile organics (particularly chlorofluorocarbons and methylene chloride) through the sample container ptum during shipment and storage. A trip blank prepared from organic-free reagent water and carried through sampling and subquent storage and handling will rve as a check on such contamination.
4.3Contamination by carryover can occur whenever high-concentration and low-concentration samples are analyzed in quence. To reduce the potential for carryover, the sample syringe or purging device must be rind out between samples with an appropriate solvent. Whenever an unusually concentrated sample is encountered, it should be followed by injection of
a solvent blank to check for cross contamination.
4.3.1Clean purging vesls with a detergent solution, rin with distilled water, and
then dry in a 105E C oven between analys. Clean syringes or autosamplers by flushing all surfaces that contact samples using appropriate solvents.
4.3.2All glassware must be scrupulously cleaned. Clean all glassware as soon
as possible after u by rinsing with the last solvent ud. This should be followed by detergent washing with hot water, and rins with tap water and organic-free reagent water.
Drain the glassware and dry it in an oven at 130E C for veral hours or rin it with methanol and drain. Store dry glassware in a clean environment.
4.4The flame ionization detector (FID) is a non-lective detector. There is a potential for many non-target compounds prent in samples to interfere with this analysis. There is also the potential for analytes to be resolved poorly, especially in samples that contain many analytes. The data ur should consider this and may wish to alter the target analyte list accordingly.
