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METHOD 8410 

 GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED

SPECTROMETRY FOR SEMIVOLATILE ORGANICS:

CAPILLARY COLUMN

1.0 SCOPE AND APPLICATION 

1.1 This method covers the automated identification, or compound class assignment of 

unidentifiable compounds, of solvent-extractable semivolatile organic compounds which are 

amenable to analysis by gas chromatograph/Fourier transform-infrared spectrometer (GC/FTIR). GC/FT-IR can be a useful complement to gas chromatograph/mass spectrometer (GC/MS) 

analysis (Method 8270). It is particularly well suited for the identification of specific isomers that 

are not differentiated using GC/MS. Compound class assignments are made using infrared (IR) 

group absorption frequencies. The presence of an IR band in the appropriate group frequency 

region may be taken as evidence of the possible presence of a particular compound class, while 

its absence may be construed as evidence that the compound class in question is not present. 

This evidence will be further strengthened by the presence of confirmatory group frequency 

bands. Identification limits of the following compounds have been demonstrated by this method. 

Compound Name CAS No.a

Acenaphthene 83-32-9 

Acenaphthylene 208-96-8 

Anthracene 120-12-7 

Benzo(a)anthracene 56-55-3 

Benzo(a)pyrene 50-32-8 

Benzoic acid 65-85-0 

Bis(2-chloroethoxy)methane 111-91-1 

Bis(2-chloroethyl)ether 111-44-4 

Bis(2-chloro-1-methylethyl)etherb

108-60-1 

Bis(2-ethylhexyl)phthalate 117-81-7 

4-Bromophenyl phenyl ether 101-55-3 

Butyl benzyl phthalate 85-68-7 

4-Chloroaniline 106-47-8 

4-Chloro-3-methylphenol 59-50-7 

2-Chloronaphthalene 91-58-7 

2-Chlorophenol 95-57-8 

4-Chlorophenol 106-48-9 

4-Chlorophenyl phenyl ether 7005-72-3 

Chrysene 218-01-9 

Dibenzofuran 132-64-9 

Di-n-butyl phthalate 84-74-2 

1,2-Dichlorobenzene 95-50-1 

1,3-Dichlorobenzene 541-73-1 

1,4-Dichlorobenzene 106-46-7 

2,4-Dichlorophenol 120-83-2 

Diethyl phthalate 84-66-2 

Dimethyl phthalate 131-11-3 
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Compound Name CAS No.a

4,6-Dinitro-2-methylphenol 534-52-1 

2,4-Dinitrophenol 51-28-5 

2,4-Dinitrotoluene 121-14-2 

2,6-Dinitrotoluene 606-20-2 

Di-n-octyl phthalate 117-84-0 

Di-n-propyl phthalate 131-16-8 

Fluoranthene 206-44-0 

Fluorene 86-73-7 

Hexachlorobenzene 118-74-1 

1,3-Hexachlorobutadiene 87-68-3 

Hexachlorocyclopentadiene 77-47-4 

Hexachloroethane 67-72-1 

Isophorone 78-59-1 

2-Methylnaphthalene 91-57-6 

2-Methylphenol 95-48-7 

4-Methylphenol 106-44-5 

Naphthalene 91-20-3 

2-Nitroaniline 88-74-4 

3-Nitroaniline 99-09-2 

4-Nitroaniline 100-01-6 

Nitrobenzene 98-95-3 

2-Nitrophenol 88-75-5 

4-Nitrophenol 100-02-7 

N-Nitrosodimethylamine 62-75-9 

N-Nitrosodiphenylamine 86-30-9 

N-Nitroso-di-n-propylamine 621-64-7 

Pentachlorophenol 87-86-5 

Phenanthrene 85-01-8 

Phenol 108-95-2 

Pyrene 129-00-0 

1,2,4-Trichlorobenzene 120-82-1 

2,4,5-Trichlorophenol 95-95-4 

2,4,6-Trichlorophenol 88-06-2 

 

a

 Chemical Abstract Services (CAS) Registry Number. 

b

 Chemical name was changed by the Integrated Risk Information System (IRIS) on 

November 30, 2007 from Bis(2-chloroisopropyl)ether to Bis(2-chloro-1-

methylethyl)ether (common name). This compound is also known as 2,2’-oxybis(1-

chloropropane) (CAS index name). See the link at 

http://www.epa.gov/iris/subst/0407.htm, Section VII for the “Revision History” and 

Section VIII, for “Synonyms” of this chemical. 

 1.2 This method is applicable to the determination of most extractable, semivolatileorganic compounds in wastewater, soils and sediments, and solid wastes. Benzidine can be 

subject to losses during solvent concentration and analysis by gas chromatograph (GC); α-BHC, 

β-BHC, Endosulfan I and II, and Endrin are subject to decomposition under the alkaline 

conditions of the extraction step; Endrin is subject to decomposition during GC analysis; and 

Hexachlorocyclopentadiene and N-Nitrosodiphenylamine may decompose during extraction and 
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GC analysis. Other extraction and/or instrumentation procedures should be considered for 

unstable analytes. 

 1.3 The identification limit of this method may depend strongly upon the level and type 

of semivolatile extractants amenable to GC analysis. The values listed in Tables 1 and 2 

represent the minimum quantities of semivolatile organic compounds which have been identified 

by the specified GC/FT-IR system, using this method and under routine environmental analysis 

conditions. Capillary GC/FT-IR wastewater identification limits of 25 μg/L may be achieved for 

weak IR absorbers with this method, while the corresponding identification limit for strong IR 

absorbers is 2 μg/L. Identification limits for other sample matrices can be calculated from the 

wastewater values after choice of the proper sample workup procedure (see Sec. 11.1). 

2.0 SUMMARY OF METHOD 

 Prior to using this method, the samples should be prepared for chromatography using the 

appropriate sample preparation and cleanup methods. This method describes chromatographic 

conditions that will allow for the separation of the compounds in the extract and uses FT-IR for 

detection and quantitation of the target analytes. 

3.0 DEFINITIONS 

Refer to Chapter One, the individual determinative methods, and the manufacturer's 

instructions for definitions that may be relevant. 

4.0 INTERFERENCES 

 4.1 Glassware and other sample processing hardware must be thoroughly cleaned to 

prevent contamination and misinterpretation. All of these materials must be demonstrated to be 

free from interferences under the conditions of the analysis by running method blanks. Specific 

selection of reagents or purification of solvents by distillation in all-glass systems may be 

required. 

 4.2 Matrix interference will vary considerably from source to source, depending upon 

the diversity of the residual waste being sampled. While general cleanup techniques are 

provided as part of this method, unique samples may require additional cleanup to isolate the 

analytes of interest from interferences in order to achieve maximum sensitivity. 

 4.3 4-Chlorophenol and 2-nitrophenol are subject to interference from coeluting 

compounds. 

 4.4 Clean all glassware as soon as possible after use by rinsing with the last solvent 

used. Glassware should be sealed/stored in a clean environment immediately after drying to 

prevent any accumulation of dust or other contaminants. 

5.0 SAFETY 

This method does not address all safety issues associated with its use. The laboratory is 

responsible for maintaining a safe work environment and a current awareness file of 

Occupational Safety and Health Administration (OSHA) regulations regarding the safe handling 
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of the chemicals and instrumentation included in this method. A reference file of material safety 

data sheets (MSDSs) should be available to all personnel involved in these analyses. 

6.0 EQUIPMENT AND SUPPLIES 

 6.1 GC/FT-IR Spectrometric Equipment 

 6.1.1 FT- IR spectrometer – A spectrometer capable of collecting at least one 

scan set per second at 8 cm-1 resolution is required. In general, a spectrometer purchased 

after 1985, or retrofitted to meet post-1985 FT-IR improvements, will be necessary to meet 

needed sensitivity of this protocol. A state-of-the-art analog/digital (A/D) converter is 

required, since it has been shown that the signal-to-noise ratio of single-beam GC/FT-IR 

systems is A/D converter limited. 

 6.1.2 GC/FT-IR interface – The interface should be lightpipe volume-optimized 

for the selected chromatographic conditions (lightpipe volume of 100-200 μL for capillary 

columns). The shortest possible inert transfer line (preferably fused silica) should be used 

to interface the end of the chromatographic column to the lightpipe. If fused silica capillary 

columns are employed, the end of the GC column can serve as the transfer line if it is 

adequately heated. It has been widely demonstrated that the optimum lightpipe volume is 

equal to the full width at half height of the GC eluate peak. 

 6.1.3 Capillary column – A fused silica DB-5 30 m x 0.32 mm capillary column 

with 1.0 μm film thickness (or equivalent) 

 6.1.4 Data Acquisition – A computer system dedicated to the GC/FT-IR system 

to allow the continuous acquisition of scan sets for a full chromatographic run. Peripheral 

data storage systems should be available (magnetic tape and/or disk) for the storage of all 

acquired data. Software should be available to allow the acquisition and storage of every 

scan set to locate the file numbers and transform high signal/noise (S/N) scan sets, and to 

provide a real-time reconstructed chromatogram. 

 6.1.5 Detector – A cryoscopic, medium-band mercury/cadmium/tellurium 

(HgCdTe or MCT) detector with the smallest practical focal area. Typical narrow-band 

MCT detectors operate from 3800-800 cm-1, but medium-band MCT detectors can reach 

650 cm-1. A 750 cm-1 cutoff (or lower) is desirable since it allows the detection of typical 

carbon-chlorine stretch and aromatic out-of-plane carbon-hydrogen vibrations of 

environmentally important organo-chlorine and polynuclear aromatic compounds. The 

MCT detector sensitivity (D)* should be ≥ 1 x 1010 cm. 

 6.1.6 Lightpipe – Constructed of inert materials, gold-coated, and volumeoptimized for the desired chromatographic conditions (see Sec. 11.3) 

 6.1.7 GC – The FT-IR spectrometer should be interfaced to a temperature 

programmable GC equipped with a Grob-type (or equivalent) purged splitless injection 

system suitable for capillary glass columns or an on-column injector system. 

 A short, inert transfer line should interface the GC to the FT-IR lightpipe and, if 

applicable, to the GC detector. Fused silica GC columns may be directly interfaced to the 

lightpipe inlet and outlet. 

 6.2 Dry purge gas – If the spectrometer is the purge-type, provisions should be made 

to provide a suitable continuous source of dry purge-gas to the FT-IR spectrometer. 
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 6.3 Dry carrier gas – The carrier gas should be passed through an efficient cartridgetype drier. 

 6.4 Syringes – 1 μL, 10 μL 

7.0 REAGENTS AND STANDARDS 

 7.1 Reagent-grade inorganic chemicals shall be used in all tests. 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 (ACS), 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. 

 7.2 Organic-free reagent water. All references to water in this method refer to organicfree reagent water, as defined in Chapter One. 

 7.3 Solvents 

 7.3.1 Acetone, CH3COCH3 – Pesticide quality, or equivalent 

 7.3.2 Methylene chloride, CH2Cl2 – Pesticide quality, or equivalent 

 7.4 Stock standard solutions (1000 mg/L) – Standard solutions can be prepared from 

pure standard materials or purchased as a certified solution. 

 7.4.1 Prepare stock standard solutions by accurately weighing 0.1000±0.0010 

g of pure material. Dissolve the material in pesticide-quality acetone or other suitable 

solvent and dilute to volume in a 100-mL volumetric flask. Larger volumes can be used at 

the convenience of the analyst. When compound purity is assayed to be 96 percent or 

greater, the weight may be used without correction to calculate the concentration of the 

stock standard. Commercially prepared stock standards may be used at any 

concentration if they are certified by the manufacturer or by an independent source. 

 7.4.2 Transfer the stock standard solutions into bottles with Teflon-lined screw 

caps. Store at 4 °C and protect from light. Stock standard solutions should be checked 

frequently for signs of degradation or evaporation, especially just prior to preparing 

calibration standards from them. 

 7.4.3 Stock standard solutions must be replaced after 6 months or sooner if 

comparison with quality control (QC) reference samples indicates a problem. 

 7.5 Calibration standards and internal standards - For use in situations where GC/FTIR will be used for primary quantitation of analytes rather than confirmation of GC/MS 

identification. 

 7.5.1 Prepare calibration standards that contain the compounds of interest, 

either singly or mixed together. The standards should be prepared at concentrations that 

will completely bracket the working range of the chromatographic system (at least one 

order of magnitude is suggested). 

 7.5.2 Prepare internal standard solutions. Suggested internal standards are 1-

fluoronaphthalene and p-terphenyl-d14, or deuterated versions of 2-chlorophenol, phenol, 
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bis(2-chloroethoxy)methane, 2,4-dichlorophenol, phenanthrene, anthracene, and butyl 

benzyl phthalate. If deuterated versions aren’t used, compounds that are on the method 

target analyte list may be used as internal standards as long as they aren’t an analyte for a 

given site, and historical data are available to ensure their absence at a given site. 

Determine the internal standard concentration levels from the minimum identifiable 

quantities. See Tables 1 and 2. 

8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 

 See Chapter 4, Organic Analytes, Sec. 4.1 for more information on this topic. 

9.0 QUALITY CONTROL 

9.1 General guidance 

Refer to Chapter One for guidance on quality assurance (QA) and QC protocols. When 

inconsistencies exist between QC guidelines, method-specific QC criteria take precedence over 

both technique-specific and Chapter One criteria; technique-specific QC criteria take 

precedence over Chapter One criteria. Any effort involving collection of analytical data should 

include development of a structured and systematic planning document, such as a quality 

assurance project plan (QAPP) or a sampling and analysis plan (SAP), which translates project 

objectives and specifications into directions for those who will implement the project and assess 

the results. 

Each laboratory should maintain a formal QA program. The laboratory should also maintain 

records to document the quality of the data generated. Development of in-house QC limits for 

each method is encouraged, as described in Sec. 9.6 of Method 8000. Use of instrumentspecific QC limits is encouraged, provided such limits will generate data appropriate for use in 

the intended application. All data sheets and QC data should be maintained for reference or 

inspection. QC to validate sample extraction is covered in Method 3500 and in the extraction 

method utilized. If extract cleanup was performed, follow the QC in Method 3600 and in the 

specific cleanup method. 

9.2 Initial demonstration of proficiency (IDP) 

Prior to implementation of a method, each laboratory must perform an IDP consisting of at 

least four replicate reference samples spiked into a clean matrix taken through the entire 

sample preparation and analysis. Whenever a significant change to instrumentation or a 

procedure occurs, the laboratory must demonstrate that acceptable precision and bias can still 

be obtained by the changed conditions. Whenever new staff members are trained, an analyst 

IDP must be performed. 

9.2.1 Demonstration of proficiency for new analysts

Each laboratory should have a training program which documents that a new 

analyst is capable of performing the method, or portion of the method, for which the 

analyst is responsible. This demonstration should document that the new analyst is 

capable of successfully following the standard operating procedure (SOP) established by 

the laboratory. 

9.3 It is recommended that the laboratory adopt additional QA practices for use with 

this method. The specific practices that are most productive depend upon the needs of the 
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laboratory and the nature of the samples. Whenever possible, the laboratory should analyze 

standard reference materials and participate in relevant performance evaluation studies. 

9.4 Lower limit of quantitation (LLOQ) 

 The laboratory shall establish the LLOQ as the lowest point of quantitation, which 

in most cases, is the lowest concentration in the calibration curve. LLOQ verification is 

recommended for each project application to validate quantitation capability at low analyte 

concentration levels. This verification may be accomplished with either clean control material 

(e.g., reagent water, solvent blank, Ottawa sand, diatomaceous earth, etc.) or a representative 

sample matrix, free of target compounds. Optimally, the LLOQ should be less than the desired 

regulatory action levels based on the stated data quality objectives (DQOs). 

 9.5 One hundred percent line test – Set the GC/FT-IR operating conditions to those 

employed for the sensitivity test (see Sec. 11.5). Collect 16 scans over the entire detector 

spectral range. Plot the test and measure the peak-to-peak noise between 1800 and 2000 cm-1. 

This noise should be ≤ 0.15%. Store this plot for future reference. 

 9.6 Single beam test – With the GC/FT-IR at analysis conditions, collect 16 scans in 

the single-beam mode. Plot the co-added file and compare with a subsequent file acquired in 

the same fashion several minutes later. Note if the spectrometer is at purge equilibrium. Also, 

check the plot for signs of deterioration of the lightpipe potassium bromide windows. Store this 

plot for future reference. 

 9.7 Align test – With the lightpipe and MCT detector at thermal equilibrium, check the 

intensity of the centerburst versus the signal temperature calibration curve. Signal intensity 

deviation from the predicted intensity may mean thermal equilibrium has not yet been achieved, 

loss of detector coolant, decrease in source output, or a loss in signal throughput resulting from 

lightpipe deterioration. 

 9.8 Mirror alignment – Adjust the interferometer mirrors to attain the most intense 

signal. Data collection should not be initiated until the interferogram is stable. If necessary, 

align the mirrors prior to each GC/FT-IR run. 

 9.9 Lightpipe – The lightpipe and lightpipe windows should be protected from moisture 

and other corrosive substances at all times. For this purpose, maintain the lightpipe 

temperature above the maximum GC program temperature but below its thermal degradation 

limit. When not in use, maintain the lightpipe temperature slightly above ambient. At all times, 

maintain a flow of dry, inert, carrier gas through the lightpipe. 

 9.10 Beamsplitter – If the spectrometer is thermostated, maintain the beamsplitter at a 

temperature slightly above ambient at all times. If the spectrometer is not thermostated, 

minimize exposure of the beamsplitter to atmospheric water vapor. 

10.0 CALIBRATION AND STANDARDIZATION 

10.1 Calibration – Refer to Method 8000 for proper calibration techniques. 

10.2 Calibration must take place using the same sample introduction method that will be 

used to analyze actual samples. 
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11.0 PROCEDURE 

 11.1 Sample Preparation – Samples must be prepared by one of the following 

methods prior to GC/FT-IR analysis. 

Matrix Methods 

Water 

 

3510, 3520 

Soil/sediment 

 

3540, 3541, 3550 

Waste 3540, 3541, 3550, 3580 

 

 11.2 Extracts may be cleaned up by Method 3640, Gel-Permeation Cleanup. 

 11.3 Initial Calibration 

 

 Recommended GC/FT-IR conditions: 

 Scan time: At least 2 scan/sec 

 Initial column temperature and hold time: 40 °C for 1 minute 

 Column temperature program: 40-280 °C at 10 °C/min 

 Final column temperature to hold: 280 °C 

 Injector temperature: 280-300 °C 

 Transfer line temperature: 270 °C 

 Lightpipe: 280 °C 

 Injector: Grob-type, splitless or on-column 

 Sample volume: 2-3 μL 

 Carrier gas: Dry helium at about 1 mL/min 

 11.4 With an oscilloscope, check the detector centerburst intensity versus the 

manufacturer’s specifications. Increase the source voltage, if necessary, to meet these 

specifications. For reference purposes, laboratories should prepare a plot of time versus 

detector voltage over at least a five-day period. 

 11.5 Capillary column interface sensitivity test – Install a 30 m x 0.32 mm fused silica 

capillary column coated with 1.0 μm of DB-5 (or equivalent). Set the lightpipe and transfer lines 

at 280 °C (if used). Under splitless Grob-type or on-column injection conditions, inject 25 ng of 

nitrobenzene, dissolved in 1 μL of methylene chloride. The nitrobenzene should be identified by 

the on-line library software search within the first five hits (nitrobenzene should be contained 

within the search library). 

 11.6 Interferometer – If the interferometer is air driven, adjust the interferometer drive 

air pressure to manufacturer’s specifications. 

 11.7 MCT detector check – If the centerburst intensity is 75 percent or less of the 

mean intensity of the plot maximum obtained by the procedure of Sec. 11.4, install a new 

source and check the MCT centerburst with an oscilloscope versus the manufacturer’s 

specifications (if available). Allow at least five hours of new source operation before data 

acquisition. 
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 11.8 Frequency calibration – At the present time, no consensus exists within the 

spectroscopic community on a suitable frequency reference standard for vapor phase FT-IR. 

One reviewer has suggested the use of indene as an on-the-fly standard. 

 11.9 Minimum identifiable quantities – Using the GC/FT-IR operating parameters 

specified in Sec. 11.3, determine the minimum identifiable quantities for the compounds of 

interest. 

 11.9.1 Prepare a plot of lightpipe temperature versus MCT centerburst intensity 

(in volts or other vertical height units). This plot should span the temperature range 

between ambient and the lightpipe thermal limit in increments of about 20 °C. Use this 

plot for daily QA/QC (see Sec. 9.7). Note that modern GC/FT-IR interfaces (1985 and 

later) may have eliminated most of this temperature effect. 

 11.10 GC/FT-IR extract analysis 

 11.10.1 Analysis – Analyze the dried methylene chloride extract using the 

chromatographic conditions specified in Sec. 11.3 for capillary column interfaces. 

 11.10.2 GC/FT-IR identification – Visually compare the analyte IR spectrum 

versus the search library spectrum of the most promising on-line library search hits. 

Report, as identified, those analytes with IR frequencies for the five (maximum number) 

most intense IR bands (S/N ≥ 5) which are within ± 5.0 cm-1 of the corresponding bands in 

the library spectrum. Choose IR bands which are sharp and well resolved. The software 

used to locate spectral peaks should employ the peak "center of gravity" technique. In 

addition, the IR frequencies of the analyte and library spectra should be determined with 

the same computer software. 

 11.10.3 Retention time confirmation – After visual comparison of the analyte and 

library spectra as described in Sec. 11.10.2, compare the relative retention times (RRT) of 

the analyte and an authentic standard of the most promising library search hit. The 

standard and analyte RRT should agree within ± 0.01 RRT units when both are 

determined at the same chromatographic conditions. 

 11.10.4 Compound class or functionality assignment – If the analyte cannot be 

unequivocally identified, report its compound class or functionality. See Table 3 for gasphase group frequencies to be used as an aid for compound class assignment. It should 

be noted that FT-IR gas-phase group stretching frequencies are 0-30 cm-1 higher in 

frequency than those of the condensed phase. 

 11.10.5 Quantitation – This protocol can be used to confirm GC/MS 

identifications, with subsequent quantitation. Two FT-IR quantitation techniques and a 

supplemental GC detector technique are also provided. 

 11.10.5.1 Integrated absorbance technique - After analyte identification, 

construct a standard calibration curve of concentration versus integrated IR 

absorbance. For this purpose, choose for integration only those FT-IR scans 

which are at or above the peak half-height. The calibration curve should span at 

least one order of magnitude and the working range should bracket the analyte 

concentration. 

 11.10.5.2 Maximum absorbance IR band technique – Following analyte 

identification, construct a standard calibration curve of concentration versus 
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maximum IR band intensity. For this purpose, choose an intense, symmetrical and 

well resolved IR absorbance band. 

 NOTE: IR transmission is not proportional to concentration. Select the FT-IR scan 

with the highest absorbance to plot against concentration. The calibration 

curve should span at least one order of magnitude and the working range 

should bracket the analyte concentration. This method is most practical for 

repetitive, target compound analyses. It is more sensitive than the 

integrated absorbance technique. 

 11.10.5.3 Supplemental GC detector technique – If a GC detector is 

used in tandem with the FT-IR detector, the following technique may be used: 

following analyte identification, construct a standard calibration curve of 

concentration versus integrated peak area. The calibration curve should span at 

least one order of magnitude and the working range should bracket the analyte 

concentration. This method is most practical for repetitive, target compound 

analyses. 

12.0 DATA ANALYSIS AND CALCULATIONS 

12.1 See Method 8000, Sec. 11 for information regarding data analysis and 

calculations. 

12.2 Results must be reported in units commensurate with their intended use and all 

dilutions must be taken into account when computing final results. 

13.0 METHOD PERFORMANCE 

 13.1 Method 8410 has been in use at the U.S. Environmental Protection Agency (EPA 

or the Agency) Environmental Monitoring Systems Laboratory for many years. Portions of it 

have been reviewed by key members of the FT-IR spectroscopic community (Ref 9). Side-byside comparisons with GC/MS sample analyses indicate similar demands upon analytical 

personnel for the two techniques. Extracts previously subjected to GC/MS analysis are 

generally compatible with GC/FT-IR. However, it should be kept in mind that lightpipe windows 

are typically water soluble. Thus, extracts must be vigorously dried prior to analysis. 

 13.2 Table 4 provides performance data for this method. 

14.0 POLLUTION PREVENTION 

14.1 Pollution prevention encompasses any technique that reduces or eliminates the 

quantity and/or toxicity of waste at the point of generation. Numerous opportunities for pollution 

prevention exist in laboratory operation. The EPA has established a preferred hierarchy of 

environmental management techniques that places pollution prevention as the management 

option of first choice. Whenever feasible, laboratory personnel should use pollution prevention 

techniques to address their waste generation. When wastes cannot be feasibly reduced at the 

source, the EPA recommends recycling as the next best option. 

14.2 For information about pollution prevention that may be applicable to laboratories 

and research institutions consult Less is Better: Laboratory Chemical Management for Waste 
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Reduction, a free publication available from the ACS, Committee on Chemical Safety, 

http://portal.acs.org/portal/fileFetch/C/WPCP_012290/pdf/WPCP_012290.pdf. 

15.0 WASTE MANAGEMENT 

The EPA requires that laboratory waste management practices be conducted consistent 

with all applicable rules and regulations. Laboratories are urged to protect air, water, and land 

by minimizing and controlling all releases from hoods and bench operations, complying with the 

letter and spirit of any sewer discharge permits and regulations and complying with all solid and 

hazardous waste regulations, particularly the hazardous waste identification rules and land 

disposal restrictions. For further information on waste management, consult The Waste 

Management Manual for Laboratory Personnel available from the ACS at the web address listed 

in Sec. 14.2 above. 
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16.0 REFERENCES 

1. U.S. Environmental Protection Agency, Environmental Monitoring and Support 

Laboratory, Handbook for Analytical Quality Control in Water and Wastewater 

Laboratories, ORD Publication Offices of Center for Environmental Research Information: 

Cincinnati, OH, Sec. 4, EPA-600/4-79-019, March 1979. 

2. R. R. Freeman, Hewlett Packard Application Note: "Quantitative Analysis Using a Purged 

Splitless Injection Technique", ANGC 7-76. 

3. R. H. Cole, Tables of Wavenumbers for the Calibration of Infrared Spectrometers; 

Pergamon: New York, 1977. 

4. J. G. Grasselli, P. R. Griffiths, and R. W. Hannah, "Criteria for Presentation of Spectra 

from Computerized IR Instruments", Appl. Spectrosc., 36, 87, 1982. 

5. R. A. Nyquist, The Interpretation of Vapor-Phase Infrared Spectra, Group Frequency 

Data, Volume I, Sadtler Laboratories: Philadelphia, PA, 1984. 

6. G. Socrates, Infrared Characteristic Group Frequencies, John Wiley and Sons: New York, 

NY, 1980. 

7. L. J. Bellamy, The Infrared Spectra of Complex Organic Molecules; 2

nd ed., John Wiley 

and Sons: New York, NY, 1958. 

8. H. A. Szymanski, Infrared Band Handbook, Volumes I and II, Plenum: New York, NY, 

1965. 

9. D. F. Gurka, "Interim Protocol for the Automated Analysis of Semivolatile Organic 

Compounds by Gas Chromatography/Fourier Transform-Infrared Spectrometry", Appl. 

Spectrosc., 39, 826, 1985. 

10. P. R. Griffiths, J. A. de Haseth and L. V. Azarraga, "Capillary GC/FT-IR", Anal. Chem., 55, 

1361A, 1983. 

11. P. R. Griffiths and J. A. de Haseth, Fourier Transform-Infrared Spectrometry, WileyInterscience: New York, NY, 1986. 

12. D. F. Gurka, I. Farnham, B. B. Potter, S. Pyle, R. Titus and W. Duncan, "Quantitation 

Capability of a Directly Linked Gas Chromatography/Fourier Transform Infrared/Mass 

Spectrometry System", Anal. Chem., 61, 1584, 1989. 

17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA 

The following pages contain the tables referenced by this method. 
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TABLE 1 

FUSED SILICA CAPILLARY COLUMN GC/FT-IR IDENTIFICATION LIMITS FOR 

BASE/NEUTRAL EXTRACTABLES 

Compound 

Identification Limit 

ν max, cm-1c ng injecteda

 μg/Lb

Acenaphthene 40(25) 20(12.5) 799 

Acenaphthylene 50(50) 25(25) 799 

Anthracene 40(50) 20(25) 874 

Benzo(a)anthracene (50) (25) 745 

Benzo(a)pyrene (100) (50) 756 

Bis(2-chloroethyl)ether 70(10) 35(5) 1115 

Bis(2-chloroethoxy)methane 50(10) 25(5) 1084 

Bis(2-chloro-1-methylethyl)ether 50(10) 25(5) 1088 

Butyl benzyl phthalate 25(10) 12.5(5) 1748 

4-Bromophenyl phenyl ether 40(5) 20(2.5) 1238 

2-Chloronaphthalene 110 55 851 

4-Chloroaniline 40 20 1543 

4-Chlorophenyl phenyl ether 20(5) 10(2.5) 1242 

Chrysene (100) (50) 757 

Di-n-butyl phthalate 20(5) 10(2.5) 1748 

Dibenzofuran 40 20 1192 

Diethyl phthalate 20(5) 10(2.5) 1748 

Dimethyl phthalate 20(5) 10(2.5) 1751 

Di-n-octyl phthalate 25(10) 12.5(5) 1748 

Di-n-propyl phthalate 25(5) 12.5(2.5) 1748 

1,2-Dichlorobenzene 50 25 1458 

1,3-Dichlorobenzene 50 25 779 

1,4-Dichlorobenzene 50 25 1474 

2,4-Dinitrotoluene 20 10 1547 

2,6-Dinitrotoluene 20 10 1551 

Bis-(2-ethylhexyl)phthalate 25(10) 12.5(5) 1748 

Fluoranthene 100(50) 50(25) 773 

Fluorene 40(50) 20(25) 737 

Hexachlorobenzene 40 20 1346 

Hexachlorocyclopentadiene 120 60 814 

Hexachloroethane 50 25 783 

1,3-Hexachlorobutadiene 120 60 853 

Isophorone 40 20 1690 

2-Methylnaphthalene 110 55 3069 

Naphthalene 40(25) 20(12.5) 779 

Nitrobenzene 25 12.5 1539 

N-Nitrosodimethylamine 20(5) 10(2.5) 1483 

N-Nitrosodi-n-propylamine 50(5) 25(2.5) 1485 

N-Nitrosodiphenylamined

 40 20 1501 

2-Nitroaniline 40 20 1564 

3-Nitroaniline 40 20 1583 
SW-846 Update V 8410 - 14 Revision 1 

 October 2012 

Compound 

Identification Limit 

ν max, cm-1c ng injecteda

 μg/Lb

4-Nitroaniline 40 20 1362 

Phenanthrene 50(50) 25(25) 729 

Pyrene 100(50) 50(25) 820 

1,2,4-Trichlorobenzene 50(25) 25(12.5) 750 

1-Fluoronaphthalenee (100) (50) 770 

p-Terphenyl-d14e

 (100) (50) 712 

a

 Determined using on-column injection and the conditions of Sec. 11.3. A medium-band 

HgCdTe detector [3800-700 cm-1; D*value (λpeak 1000 Hz, 1) 4.5 x 1010 cm Hz1/2W-1] type 

with a 0.25 mm2

 focal chip was used. The GC/FT-IR system is a 1976 retrofitted model. 

Values in parentheses were determined with a newer (1986) GC/FT-IR system. A narrow 

band HgCdTe detector [3800-750 cm-1; D*value (λpeak 1000 Hz, 1) 4 x 1010 cm Hz1/2W-1] 

was used. Chromatographic conditions are those of Sec. 11.3. 

b

 Based on a 2-μL injection of a 1-L sample that has been extracted and concentrated to a 

volume of 1.0 mL. Values in parentheses were determined with a newer (1986) GC/FT-IR 

system. A narrow band HgCdTe detector [3800-750 cm-1; D*value (λpeak 1000 Hz, 1) 4 x 

1010 cm Hz1/2W-1] was used. Chromatographic conditions are those of Sec. 11.3. 

c

 Most intense IR peak and suggested quantitation peak. 

d

 Detected as diphenylamine. 

e

 Suggested internal standard. Identification limit data is not actual, but is estimated high to 

assure sufficient amount or concentration. 
SW-846 Update V 8410 - 15 Revision 1 

 October 2012 

TABLE 2 

FUSED SILICA CAPILLARY COLUMN GC/FT-IR ON-LINE AUTOMATED IDENTIFICATION 

LIMITS FOR ACIDIC EXTRACTABLES 

Compound 

Identification Limit 

ν max, cm-1c

ng injecteda μg/Lb

Benzoic acid 70 35 1751 

2-Chlorophenol 50 25 1485 

4-Chlorophenold 100 50 1500 

4-Chloro-3-methylphenol 25 12.5 1177 

2-Methylphenol 50 25 748 

4-Methylphenol 50 25 1177 

2,4-Dichlorophenol 50 25 1481 

2,4-Dinitrophenol 60 30 1346 

4,6-Dinitro-2-methylphenol 60 30 1346 

2-Nitrophenold 40 20 1335 

4-Nitrophenol 50 25 1350 

Pentachlorophenol 50 25 1381 

Phenol 70 35 1184 

2,4,6-Trichlorophenol 120 60 1470 

2,4,5-Trichlorophenol 120 60 1458 

 

a

 Operating conditions are the same as those cited in Sec. 11.3. 

b

 Based on a 2-μL injection of a 1-L sample that has been extracted and concentrated to a 

volume of 1.0 mL. 

c

 Most intense IR peak and suggested quantitation peak. 

d

 Subject to interference from co-eluting compounds. 
SW-846 Update V 8410 - 16 Revision 1 

 October 2012 

TABLE 3 

GAS-PHASE GROUP FREQUENCIES 

Functionality Class Number of 

Compounds 

Frequency 

Range, ν cm-1 

Ether Aryl, Alkyl 14 1215-1275 

 Benzyl, Alkyl 3 1103-1117 

 Diaryl 5 1238-1250 

 Dialkyl 12 1084-1130 

 Alkyl, Vinyl 3 1204-1207 

 1128-1142 

 

Ester Unsubstituted Aliphatic 29 1748-1761 

 Aromatic 11 1703-1759 

 Monosubstituted Acetate 34 1753-1788 

 

Nitro Aliphatic 5 1566-1594 

 1548-1589 

 1377-1408 

 1327-1381 

 Aromatic 18 1535-1566 

 1335-1358 

 

Nitrile Aliphatic 9 2240-2265 

 Aromatic 9 2234-2245 

 

Ketone Aliphatic (acyclic) 13 1726-1732 

 (α,β unsaturated) 2 1638-1699 

 Aromatic 16 1701-1722 

 

Amide Substituted Acetamides 8 1710-1724 

 

Alkyne Aliphatic 8 3323-3329 

 

Acid Aliphatic 24 3574-3580 

 22 1770-1782 

 Dimerized-Aliphatic 2 3586-3595 

 Aromatic 10 3574-3586 

 10 1757-1774 

 

Phenol 1,4-Disubstituted 15 3645-3657 

 15 1233-1269 

15 1171-1190 

 1,3-Disubstituted 10 3643-3655 

 10 1256-1315 

10 1157-1198 

 1,2-Disubstituted 6 3582-3595 

 1255-1274 

 

 (continued) 
SW-846 Update V 8410 - 17 Revision 1 

 October 2012 

TABLE 3 

(Continued) 

Functionality Class Number of 

Compounds 

Frequency 

Range, ν cm-1 

Alcohol Primary Aliphatic 20 3630-3680 

 11 1206-1270 

16 1026-1094 

 Secondary Aliphatic 17 3604-3665 

 10 1231-1270 

 Tertiary Aliphatic 10 3640-3670 

 6 1213-1245 

 

Amine Primary Aromatic 15 3480-3532 

 Secondary Aromatic 5 3387-3480 

 Aliphatic 10 760-785 

 

Alkane 14 2930-2970 

 2851-2884 

 1450-1475 

 1355-1389 

 

Aldehyde Aromatic 12 1703-1749 

 12 2820-2866 

 12 2720-2760 

 Aliphatic 6 1742-1744 

 6 2802-2877 

6 2698-2712 

 

Benzene Monosubstituted 7 1707-1737 

 24 1582-1630 

24 1470-1510 

11 831-893 

23 735-790 

25 675-698 

 
SW-846 Update V 8410 - 18 Revision 1 

 October 2012 

TABLE 4 

FUSED SILICA CAPILLARY COLUMN GC/FT-IR QUANTITATION RESULTS 

Compound 

Concentration 

Range, and 

Identification 

Limit, nga

Maximum 

Absorbanceb

Correlation 

Coefficientd

Integrated 

Absorbancec

Correlation 

Coefficientd

 

Acenaphthene 25-250 0.9995 0.9985 

Acenaphthylene 25-250 0.9959 0.9985 

Anthracene 50-250 0.9969 0.9971 

Benzo(a)anthracene 50-250 0.9918 0.9921 

Benzoic acid 50-250 0.9864 0.9892 

Benzo(a)pyrene 100-250 0.9966 0.9074 

Bis(2-chloroethoxy)methane 25-250 0.9992 0.9991 

Bis(2-chloroethyl)ether 25-250 0.9955 0.9992 

Bis(2-chloro-1-methylethyl)ether 50-250 0.9981 0.9998 

4-Bromophenyl phenyl ether 25-250 0.9995 0.9996 

Butyl benzyl phthalate 25-250 0.9999 0.9994 

4-Chloroaniline 25-250 0.9991 0.9965 

4-Chloro-3-methylphenol 25-250 0.9975 0.9946 

2-Chloronaphthalene 100-250 0.9897 0.9988 

2-Chlorophenol 25-250 0.9976 0.9965 

4-Chlorophenole

- - - 

4-Chlorophenyl phenyl ether 25-250 0.9999 0.9997 

Chrysene 100-250 0.9985 0.9984 

Dibenzofuran 25-250 0.9697 0.8579 

Di-n-butyl phthalate 25-250 0.9998 0.9996 

1,2-Dichlorobenzene 25-250 0.9937 0.9947 

1,3-Dichlorobenzene 25-250 0.9985 0.9950 

1,4-Dichlorobenzene 25-250 0.9994 0.9994 

2,4-Dichlorophenol 25-250 0.9964 0.9969 

Dimethyl phthalate 25-250 0.9998 0.9996 

Dimethyl phthalate 25-250 0.9998 0.9997 

Dinitro-2-methylphenol 50-250 0.9936 0.9967 

2,4-Dinitrophenol 50-250 0.9920 0.9916 

2,4-Dinitrotoluene 25-250 0.9966 0.9928 

2,6-Dinitrotoluene 25-250 0.9947 0.9966 

Di-n-octyl phthalate 25-250 0.9983 0.9991 

Bis(2-ethylhexyl)phthalate 25-250 0.9991 0.9993 

Fluoranthene 25-250 0.9983 0.9966 

Fluorene 25-250 0.9987 0.9989 

Hexachlorobenzene 50-250 0.9981 0.9995 

1,3-Hexachlorobutadiene 50-250 0.9960 0.9979 

Hexachlorocyclopentadiene 100-250 0.9862 0.9845 

Hexachloroethane 25-250 0.9986 0.9992 

Isophorone 25-250 0.9984 0.9990 
SW-846 Update V 8410 - 19 Revision 1 

 October 2012 

Compound 

Concentration 

Range, and 

Identification 

Limit, nga

Maximum 

Absorbanceb

Correlation 

Coefficientd

Integrated 

Absorbancec

Correlation 

Coefficientd

2-Methylnaphthalene 50-250 0.9981 0.9950 

2-Methylphenol 25-250 0.9972 0.9964 

4-Methylphenol 25-250 0.9972 0.9959 

Naphthalene 25-250 0.9956 0.9954 

2-Nitroaniline 25-250 0.9996 0.9994 

3-Nitroaniline 25-250 0.9985 0.9990 

4-Nitroaniline 25-250 0.9936 0.9992 

Nitrobenzene 25-250 0.9997 0.9979 

2-Nitrophenole

 - - - 

4-Nitrophenol 50-250 0.9951 0.9953 

N-Nitrosodimethylamine 25-250 0.9982 0.9993 

N-Nitrosodiphenylamine 25-250 0.9994 0.9971 

N-Nitrosodi-n-propylamine 25-250 0.9991 0.9995 

Pentachlorophenol 50-250 0.9859 0.9883 

Phenanthrene 25-250 0.9941 0.9989 

Phenol 25-250 0.9978 0.9966 

Pyrene 50-250 0.9971 0.9977 

1,2,4-Trichlorobenzene 50-250 0.9969 0.991 

2,4,5-Trichlorophenol 25-250 0.9952 0.9966 

2,4,6-Trichlorophenol 25-250 0.9969 0.9965 

 

a

 Lower end of range is at or near the identification limit. 

b

 FT-IR scan with highest absorbance plotted against concentration. 

c

 Integrated absorbance of combined FT-IR scans which occur at or above the chromatogram 

peak half-height. 

d

 Regression analysis carried out at four concentration levels. Each level analyzed in 

duplicate. Chromatographic conditions are stated in Sec. 11.3. 

e

 Subject to interference from co-eluting compounds. 
SW-846 Update V 8410 - 20 Revision 1 

 October 2012 

METHOD 8410 

GC/FT-IR SPECTROMETRY FOR SEMIVOLATILE ORGANICS: CAPILLARY COLUMN 

 
SW-846 Update V 8410 - 21 Revision 1 

 October 2012 

Appendix A 

Changes in this version from the December 1994, Revision 0. 

1. Improved overall method formatting for consistency with new SW-846 methods style 

guidance. The format was updated to Microsoft Word 2007.docx. This includes the 

additions of all sections required by the new format. 

2. Many minor editorial and technical revisions were made throughout to improve method 

clarity. 

3. The revision number was changed to 1 and the date published was changed to October 

2012. 

4. This appendix was added showing changes from the previous revision. 

5. Chemical name was changed by the Integrated Risk Information System (IRIS) on 

November 30, 2007 from Bis(2-chloroisopropyl)ether to Bis(2-chloro-1-methylethyl)ether 

(common name). This compound is also known as 2,2’-oxybis(1-chloropropane) (CAS 

index name). See the link at http://www.epa.gov/iris/subst/0407.htm, Section VII for the 

“Revision History” and Section VIII, for “Synonyms” of this chemical. 

6. This appendix was added showing changes from the previous revision. 

7. The flowchart on page 19 was updated to reflect the current section numbers. 

8. Section 7.5.2 and Table 1 was updated to clarify use of internal standards.