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Field Screening Methods Catalog: User`s Guide (U.S. EPA

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3. ACCURACY Improved over conventional sampling techniques e loss of analyte during well pumping and sample storage In conventional techniques PRECISION REPEATABILITY Results of repeated analyses for chloroform from one well all fall within 3 using an organic chloride FOCS COMMENTS Organic chloride FOCS developed by EPA are integrating devices Slope of the response curve can be directly related to sample concentrations Chemical specificity of FOCS allows simplification of the spectrometer Independent GC MS analysis can be used to confirm results 64 USE LOCATION USED Henderson NV EPA SITE NUMBER CERCLIS Non CERCLA MATRIX Water air soil PREPARATION MAINTENANCE AND CLEANUP Reuse of FOCS requires cleanup e g for organic chloride FOCS bleach the fluorescent reaction product by raising the source power ANALYSIS TIME NA CAPITAL COSTS RFS Low developmental cost but high operational and equipment cost FOCS Individual FOCS elements should cost less than 25 Instruments would cost from 500 to 10 000 depending on configuration e g spectrometer or refractome ter single or multi channel etc CALIBRATION FCCS Experiments are run with each type of FOCS to produce a cali bration curve using precalibrated solutions COMMENTS Limited field experience with most FRS and FOCS applications Research amp commercialization effort underway by several agencies and companies PROTOCOL AVAILABLE No SOURC
4. Print Method Heading and Summary Print Complete Method Listing C Om woh After selecting one or more methods to print or display the user may elect to print the detection limit table for each method These tables will Include all the sub stances for which each method may be applied When the printing is complete the DISPLAY PRINT menu reappears At this point you can choose to repeat the DISPLAY PRINT process or exit to the main menu and conduct another search When a user selects options 3 or 6 methods selected for display or printing will produce fully detailed method descriptions In order to view or print Headings only or Headings and Summaries choose option 1 or 4 and 2 or 5 respectively 24 5 0 FSMC SYSTEM REQUIREMENTS 5 1 SOFTWARE CHARACTERISTICS The two sided 5 1 4 inch diskettes are the only software required to run the FSMC system Users are encouraged to make backup copies of these two diskettes Although users may freely copy the system diskettes only users of registered copies will receive software and documentation revisions To obtain additional copies of the FSMC system contact the FSMC Coordinator at the address provided in the Executive Summary and Appendix C of this manual The FSMC system was developed by CDM Federal Programs Corporation using dBASE iii Pius version 1 1 a product of Ashton Tate Inc The source code was compiled using Clipper a product of Nantucket Software Inc and will run on most
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6. install the FSMC system You will then be able to Install the system as described above Note Installation from option S Utilities will only work from the floppy disks It will not work from a hard disk because the FSMC copy of the program has already been installed to the hard disk drive 3 0 GETTING STARTED If the FSMC system has not yet been installed proceed as described in the section entitled Installing the System For a two floppy system insert disk A into drive A and disk B into drive B and enter A gt FSMC For a hard drive system change the current directory so that the FSMC is ac cessible then enter FSMC From this point on all instructions are the same for both computer configurations 17 3 1 SEARCHING THE DATA BASE The data base may be searched in several ways The user may enter a substance name or CAS number if a method for a specific chemical is desired by chemical group e g volatile organics or by method name The user s options are displayed and described in Figure 3 1 More detailed descriptions are included below The FSMC system provides several search options depending upon the information known about the substances and area to be sampled The sequence of the search routines are summarized a follows 1 Select an option in order to enter the chemical name group CAS number or method name or number Select each matrix that must be analyzed with this field method by e
7. repeated analyses of well homogenized soil Relative standard deviation of 22 for nine spiked soil samples for PCBs COMMENTS Flash chromatography can be used as a gross cleanup step before MS MS when interferences are likely e g isobaric compounds with overlapping collision induced dissociation spectra or compounds that react preferentially with the reagent gas Accurate quantification difficult In air samples if gt lO 000 ug l methane is present Because of the possibilities of self chemical ionization and source chemistry saturation quantitation in the mg l range is suspect The quantitation of many compounds in air is very sensitive to changes in the absolute humidity of the air sampled especially with the APCI source Quantitation of polar compounds by the APCI source is very sensitive to the presence of ammonia and mg l levels of amines LPCI is required source for most environmental sampling USE LOCATION USED Oceanside NJ Utica NY and numerous other sites EPA SITE NUMBER CERCLIS Not Available MATRIX Air ambient and indoor soil water soil gas and incinerator wastes PREPARATION MAINTENANCE AND CLEANUP Soil sample preparation for dioxin analysis typically consists of a single step extraction a rapid dual mini column cleanup 8 samples every 3 4 hours and flash gas chromatography temperture program at 25 C min Soil preparation for PCBs and chlorinated pesticides at mg kg concentrations 55 consists of
8. 45 minutes analysis 25 minutes CAPITAL COST Tenax tubes 50 75 probes 100 sampling pump 100 500 Gas Chromatograph 4 100 20 000 CALIBRATION Sampling pump requires calibration using a dummy Tenax tube and Buck Calibrator before and after sample collection COMMENTS Allows long term and time averaged sampling Comparatively easy sample collection May not show long term changes in soil gas concentration unless probe con tents mixed to provide equilibrium along probe length before sampling Provided more information about widespread low level contamination than Direct Injection Auger method but no more detailed plume map Allows more complete desorption than acti vated carbon and is easier to clean for reuse Samples can be refrigerated for later analysis PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT John Ryding AFFILIATION C C Johnson amp Malhotra TELEPHONE 303 433 6966 PREPARED May 6 1987 BIBLIOGRAPHY Jowise P P Vilinow J D Gorelik L I Ryding J M Comparative Analysis of Soil Gas Sampling Techniques Management of Uncontrolled Hazardous Waste Sites Washington D C December 1 3 1986 p 193 199 31 METHOD FM 16 SOIL GAS SAMPLING FOR DOWNHOLE PROFILING SUMMARY Soil gas samples are collected from borehole through Teflon tubing to deter mine vertical contamination gradient Soil temperature increase due to boring may in fluence results Analysis can be performed usi
9. Analytical Operations Branch VVH548A The Catalog was developed to assist the user in identifying field screening methods applicable to specific site characteristics The computer system was developed using dBase Ill Plus and operates on an IBM compatible microcomputer The user may search for field methods by entering selection criteria including chemical class name or CAS number method name or number matrix type air soil and or water and a minimum detection limit It is important to note that the methods presented in this Catalog are an option available to RPMs and SMs the methods are not designed to take the place of other analytical options They are intended to supplement existing methods and provide options based on the specific needs of the sampling analytical activity Based on the anticipated momentum that the FSMC will generate within the Agency and in the private sector this Catalog is provisional and is expected to be revised and updated as more information becomes available on existing screening analytical techniques and as new techniques are developed tested and applied to field analysis at hazardous waste sites In order to develop a historic data base on the range of data quality achieved by each method it is critical that users conduct sufficient QC analysis to allow a deter mination of data quality as defined by precision and accuracy Additional information which will assist in defining the overall utility
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11. ANALYSIS USING GC WITH AUTOMATED HEADSPACE SAMPLER SUMMARY Rapid determination of VOCs to 10 ug l in water and 10 ug kg in soil Requires field laboratory Results are tentative Method yet to be used in field METHOD DESCRIPTION Requires a field laboratory with an automated headspace sam pler interfaced to a GC equipped with a PID and ECD in series to screen VOCs in soil and water Identification and quantitation by comparison of standard peak retention times and peak areas with sample Method for water consists of transferring 1 ml of water sample to a 3 ml reaction vial For soil method consists of transferring 1 gram of sample to 3 ml reaction vial Add 1 ml of surrogate standard to each sample Set headspace sampler temperature at 6OoC Load sampler and analyze samples APPLICATION Good for most VOCs to low ug kg ranges halogenated hydrocarbons chlorinated hydrocarbons aromatics etc LIMITATIONS Complex samples give co eluting peaks Results especially for soil are semi quantitative Method has not been used in the field INSTRUMENTATION USED Perkin Elmer 2000 with HNU PID detector and Tracer Hall detector Hewlett Packard Model 19395A automated headspace sampler PERFORMANCE SPECIFICATION DETECTION LIMIT 10 ug l for most VOCs in water 20 ug l for some halogenated aro matics 10 ug kg for most VOCs in soil SELECTIVITY Peaks are separate occasional overlapping peaks ACCURACY At low concentrations 10 50 ug l goo
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13. Division David Bennett U S EPA Toxic Integration Branch Andrew P Szilagyi CDM Federal Programs Corporation Claire M Gesalman Roy F Weston Inc Brian Dougherty Roy F Weston Inc The following individuals were largely responsible for the technical development of the field screening analytical methods Thomas Spittler U S EPA Region Laboratory Tom Pritchett U S EPA Emergency Response Team S H Mo New York State Department of Environmental Conservation William Loy U S EPA Region IV Environmental Services Division James Jerpe U S EPA Region Ill Central Regional Laboratory Lisa Gatton Vidulich U S EPA Region Monitoring Management Branch John Kinrade Scintrex Limited Richard Chappell Camp Dresser amp McKee Inc Henry Kerfoot Lockheed Engineering and Management Services Co Inc Steve Simon Lockheed Engineering and Management Services Co Inc Andrew Hafferty Ecology and Environment Inc Hunt Chapman Ecology and Environment Inc John Ryding C C Johnson amp Malhotra Stacie Popp Roy F Weston Inc Patricia Gardner Analytichem International Joseph Paladino Westinghouse Bio Analytic Systems Company Helpful suggestions and comments on the draft document were provided by the following as well as other EPA and contractor staff Jeffery Sullivan Camp Dresser amp McKee inc Joan Fisk U S EPA Hazardous Site Evaluation Division Dennis VVesolovvskl U S EPA Region V Lisa Woo
14. IBM compatible computers under MS DOS The FSMC system does not require a copy of dBASE iii Pius to run and will execute faster than if it were uncompiled running under dBASE III 5 2 HARDWARE REQUIREMENTS The following are the minimal computer hardware requirements needed to run the FSMC system The system has been tested on Compaq DeskPro 386 Compaq Portable 2 Telex PC IBM PC clones and Tandon machines IBM compatible computer with 512 of available RAM a monochrome or color monitor Two floppy disk drives or one floppy disk drive and one hard disk drive A printer if printed reports are desired 25 APPENDIX A FIELD METHOD LISTING LISTING OF METHODS PRIMARY METHODS Field Atomic Absorption Analysis 2 X Ray Fluorescence in Laboratory for Heavy Metals X Ray Fluorescence for Heavy Metals On site FM 4 Air Monitoring for Volatile Organic Compounds Using Programmed Thermal Desorption and GC FM 5 Volatile Organic Compound Analysis Using GC with Automated Headspace Sampler FM 6 Headspace Technique Using an lon Detector for VOC Analysis FM 7 Headspace Technique Using an OVA for VOCs FM 8 Headspace Analysis Using HNU for Total Volatile Organics FM 9 Headspace Technique Using a Mobile GC for VOCs FM 10 Passive Soil Gas Sampling Using Industrial Hygiene Samplers FM 11 Soil Gas Sampling
15. Method for Volatile Organic Compounds EPA Region IV Mobile Laboratory Protocol January 1987 METHOD FM 6 HEADSPACE TECHNIQUE USING AN ION DETECTOR FOR VOC ANALYSIS SUMMARY Analysis of soil water and air samples for identification and quantitation of most VOCs to ug l range The ion detector is a GC MS system Requires field laboratory Soil results are semi quantitative METHOD DESCRIPTION Used to screen water soil and sediment samples for volatile organic compounds VOC on an ion trap detector a gas chromatograph mass spectral GC MS system in a field laboratory GC separates the compounds and Introduces them into MS which provides positive identification of peaks Quantitatlon is determined by peak areas on GC Method Involves collecting desired sample in a 40 ml vial prepar ing sample if soil and sampling the vapor headspace above solution It is then analyzed on ion trap detector Air is screened directly by collecting sample and injecting it into GC for analysis APPLICATION Good for most VOCs to 1 ug l concentrations unsaturated hydrocarbons halogenated hydrocarbons aromatics etc Mass spectrum good for more positive identi fication of compounds LIMITATIONS Results for soil are semi quantitative High initial cost INSTRUMENTATION USED Finnigan lon Trap Detector ITD 700 series with IBM PC XT PERFORMANCE SPECIFICATION DETECTION LIMIT 1 ug l for most VOCs SELECTIVITY Excellent identification capabilities
16. ONE LITER SYRINGE SUMMARY Rapid sampling of soil gas for on site analysis to determine contaminant plume repeated sampling not possible once auger removed GC analysis can be per formed in a field laboratory METHOD DESCRIPTION Sample is obtained as follows drill hole using hollow stem auger lower a length of Teflon tubing attached to a l liter gas tight syringe to the de sired sampling depth Condition Teflon line by drawing a 500 ml air sample detach and evacuate the syringe reattach and draw 1 liter sample which is injected Into a purge and trap unit for concentration and GC analysis APPLICATION Soil sampling for GC analysis to aid in contaminant plume delineation LIMITATIONS Relatively long analysis time no repeated sampling once auger is re moved variation in injection rate can lead to VOC breakthrough in the purge and trap unit INSTRUMENTATION USED Sampling l liter gas tight syringe syringe pump Analysis GC with a purge and trap unit PERFORMANCE SPECIFICATION DETECTION LIMIT Sensitivity improved over other sampling techniques by sample con centration 0 2 0 02 ug l for TCE SELECTIVITY Volatile organics depends on GC method used for analysis ACCURACY High correlation with other sampling techniques Correlation coefficients were 0 68 with direct injection auger 0 88 with soil headspace 0 87 with direct Injection stopper 0 90 with Tenax tube PRECISION REPEATABILITY N A COMMENTS Sensitivity de
17. Ryding J M Comparative Analysis of Soil Gas Sampling Techniques Management of Uncontrolled Hazardous Waste Sites Washington D C December 1 3 1986 p 193 199 27 METHOD FM 14 SOIL GAS SAMPLING USING A PERFORATED TUBE SUMMARY Grab or composite soil gas samples obtained using pipe with perforated tip driven into ground Analysis can be performed using portable GC field laboratory and or off site laboratory METHOD DESCRIPTION A non reactive rod or pipe with a perforated tip is driven into the ground to the desired sampling depth A pump is used to withdraw soil gas through Teflon tubing from which grab samples can be taken using a syringe or composite samples obtained by adding Tenax or other adsorbent material in the collection line along with a flow meter to measure air volume sampled A water trap is used in some applications APPLICATION Sampling of VOCs in the soil pore spaces in the unsaturated zone to assess extent of contamination LIMITATIONS Aerobic degradation of hydrocarbons may occur in some areas at shallow sampling depths Sample leakage from probe or syringe possible INSTRUMENTATION USED Perforated pipe Teflon tubing gas tight glass syringe vacuum pump PERFORMANCE SPECIFICATION DETECTION LIMIT Not Known SELECTIVITY Volatile organics affected by GC method used ACCURACY Not Known PRECISION REPEATABILITY Not Known COMMENTS Clay layers and horizons with lt 5 air filled porosity red
18. Standard Deviation SD of five replicates Phenols except phenol SD 5 2 25 8 PAHs and neutral compounds SD 2 3 15 8 Nitrogen heterocycles SD 4 4 32 2 COMMENTS Performance data given for method using acetonitrile and methyl chloride solvent USE LOCATION USED Not Available EPA SITE NUMBER CERCLIS Not Applicable MATRIX Water PREPARATION MAINTENANCE AND CLEANUP Columns are not reusable and must be discarded 80 ANALYSIS TIME Sample preparation 10 15 min analysis 20 30 min sample CAPITAL COST 85 000 100 000 for GC MS 1 extraction column CALIBRATION Standards are made of high purity solvents with 0 0001 ug l of various contaminants added These standards are used to spike water samples to obtain various concentrations The spikes are used for identification and quantitation COMMENTS Interpretation of results requires a trained chemist Capital cost varies de pending on the GC MS purchased HPLC analysis is alternative to GC MS PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT Patricia Gardner AFFILIATION Analytichem International TELEPHONE 800 421 2825 PREPARED April 21 1987 BIBLIOGRAPHY Rostad C E Pereiru W E and Rutcliff SM Bonded Phase Extraction Column Isolation of Organic Compounds in Ground Water at a Hazardous Waste Site Analytical Chemistry Vol 58 No 14 p 2856 2860 December 1984 Chladek E and Marano R S Use of Bonded Phase Silica Sor
19. all elements tested COMMENTS Detection limit is directly related to the total number of x rays counted and the number of x rays due to interferences and background Average RPD is about 27 18 may be due to sample non homogeneity 6 to instrument error and 3 due to the grinding process Laboratory XRF analyzer offers better sensitivity performance USE LOCATION USED Smuggler Mountain Site Aspen Colorado 1985 EPA SITE NUMBER CERCLIS COD980806277 MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP The XRF analyzer must be set up and programmed Maintenance includes checking the probe for cleanliness and dryness and checking for source decay ANALYSIS TIME 10 30 minutes for sample preparation depending on moisture content of the soil Actual analysis averages 5 minutes per sample CAPITAL COSTS 50 000 CALIBRATION Sample calibration includes measurements of pure element calibratior standards measurements of site specific samples with known analyte concentrations input of calibration standard concentrations and calculation of calibration coefficients Midpoint standards should be rechecked after five samples if deviation of standards is greater than 3 recalibrate instrument COMMENTS XRF is non destructive the samples can therefore be stored for future ref erence after analysis Personnel training is required Data reporting format is either direct LCD read out or paper printout if interfaced with a printer PRO
20. are forced into screw cap vials by a sampling extruder Deionized distilled water is added to the vial which is then heated agitated and samples are with drawn for GC analysis APPLICATIONS Suited for low concentration contaminants with low vapor pressures or where sample contaminants need to be concentrated in a headspace to be within detec tion limits of the analytical instrument LIMITATIONS INSTRUMENTATION USED Mini barrel borehole sampler and sample extruder PERFORMANCE SPECIFICATION DETECTION LIMITS Suited for low concentration contaminants SELECTIVITY Volatile organics ACCURACY Not Known PRECISION REPEATABILITY Not Known COMMENTS Clay layers and horizons with lt 5 air filled porosity reduce effectiveness of soil gas sampling Compare with other sampling techniques to determine applicability at each site USE LOCATION USED Not available EPA SITE NUMBER CERCLIS Not applicable MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP N A ANALYSIS TIME N A CAPITAL COST Not Available PROTOCOL AVAILABLE Yes 22 SOURCE TECHNICAL CONTACT Andrew Hafferty AFFILIATION Ecology and Environment Inc TELEPHONE 206 624 9537 PREPARED May 6 1987 BIBLIOGRAPHY Chapman H and Clay P Field Investigation Team FIT Screening Methods and Mobile Laboratories Complementary to Contract Laboratory Program CLP TDD HQ 8507 01 October 17 1986 Draft 23 METHOD FM 12 SOIL GAS SAMPLING USING A
21. detectors require occa sional cleaning and reconditioning ANALYSIS TIME 60 min sample 50 CAPITAL COST Shimadzu Mini 2F 4 100 00 Mini 3 5 200 00 CALIBRATION Retention times and peak areas of standards must be obtained for the compounds of interest Standards are used to generate a three point calibration curve COMMENTS Used fairly regularly in Region X PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Hunt Chapman AFFILIATION Ecology and Environment Inc TELEPHONE 703 522 6065 PREPARED April 14 1987 BIBLIOGRAPHY Chapman H and Clay P Field Investigation Team FIT Screening Methods and Mobile Laboratories Complementary to Contract Laboratory Program CLP EPA Document Number TDD HQ 8507 01 October 17 1986 Draft 51 METHOD FM 26 Total PNA Analysis using an Ultraviolet Fluorescence Spectrophotometer SUMMARY Rapid semi quantitative determination of total polynuclear aromatics PNAs in soil and water to 10 0 ug l in water and 1 000 ug kg in soil field laboratory required METHOD DESCRIPTION Requires a field laboratory with UV fluorescence spectropho tometer The compounds concentrations will determine the amount of a particular wavelength of light absorbed Method consists of measuring a set amount of soil or water a one step extraction followed by UV fluorescence spectrophotometric analysis Analysis occurs at ambient temperature constant temperature preferable Sodium sulfate i
22. even in the presence of co eluting peak ACCURACY SIX point calibration curve yielded 0 964 correlation coefficient PRECISION REPEATABILITY Six point calibration curve showed 20 relative standard deviation COMMENT Performance specifications were taken from headspace of water samples USE LOCATION USED Adamstown Maryland Well Water Analysis August 1986 EPA ID NUMBER Non CERCLIS MATRIX Air Headspace above soil sediment and water PREPARATION MAINTENANCE AND CLEANUP Columns and detector must be cleaned and reconditioned occasionally Care must be taken not to saturate the column with con centrated samples ANALYSIS TIME 10 20 minutes sample CAPITAL COST Approximately 40 000 for ITD with IBM PC XT CALIBRATION Standards necessary to identify and quantify compounds The standard is a known quantity of an organic vapor which is in equilibrium with either air or an aqueous or water organic solution Minimum of three points should be used to develop calibration curve COMMENTS The interpretation of results requires a trained chemist Method has seen limited use PROTOCOL AVAILABLE No SOURCE CONTACT NAME James Jerpe AFFILIATION EPA Region iii Central Laboratory TELEPHONE 301 266 9180 PREPARED April 23 1987 BIBLIOGRAPHY Chapman H and Clay P Field investigation Team FIT Screening Methods and Mobile Laboratories Complementary to Contract Laboratory Program CLP TDD HQ 8507 1 O
23. of Bonded Sorbents for Pesticide Analysis FM D3 Use of Bonded Sorbents for Semi Volatile Analysis FM D4 Immunoassays for Trace Organic Analysis FM D5 Use of Fiber Optic Sensors in Environmental Monitoring 38 40 42 44 Method FM I FIELD ATOMIC ABSORPTION ANALYSIS Summary Atomic absorption AA spectroscopy for metals analysis in field laboratory with the minimum detectable concentrations commonly below 1 ug kg for metals such as Au Ag Cu Cd and Pb Tungsten furnace requires a maximum of only 500 W of power and can be run off a portable generator Method description Low mass tungsten furnace is used to atomize samples making power requirements compatible with field lab use Dry ash atomize timing and tem perature controls must be set for element being analyzed final ashing temperature is adjustable between 1000 C and 10009 atomizing temperature is variable to 2500 Sample is prepared by procedures similar to those used in other AA tech niques Place 10 ul liquid sample by pipette onto atomizer Analysis results are displayed in about 90 seconds Applications Mobile field analysis for trace metals Limitations Requires 1 10 220 volt electrical connection Sample preparation required Instrumentation used Scintrix AAZ 2 Zeeman Modulated Atomic Absorption Spectrophotometer PERFORMANCE SPECIFICATION Sensitivity Detection Limits 0 1 mg kg for most metals Detec
24. of most pesticides to 100 ug l in water and to 20 ug kg In soil Low recovery of some pesticides Field laboratory required METHOD DESCRIPTION Requires field laboratory with GC and linearized ECD for pesti cide analysis in soil and water Identification and quantitation is determined by compar ing peak retention times and peak areas respectively of the standard and sample Sample preparation for water consists of adding 1 ml hexane to 100 ml of water mixing and separating hexane layer This step is repeated once Sample preparation for soil consists of mixing 1 to 2 grams of soil 2 ml methanol and 10 ml hexane and separating the hexane layer 1 ml sulfuric acid is added to the extract and mixed If pesticide is sensitive to acidification this step is omitted Hexane extract is ready for GC analysis APPLICATION Simple and rapid determination of most pesticides except for endrin ketone and methoxychlor Also determines PCBs LIMITATIONS Poor spike recoveries for some pesticides Method requires testing before use Results are semi quantitative INSTRUMENTATION USED Analytical Instrument Development Corp AID model 511 06 with ECD and 4 ft SE 30 column or Shimadzu Mini 2 with ECD and 4 ft OV 1 column PERFORMANCE SPECIFICATION DETECTION LIMITS 100 ug l in water and 20 ug kg in soil SELECTIVITY Compounds give separate peaks good selectivity ACCURACY 3 water matrix spikes of 13 compounds recovery 8 107 3 soil matrix sp
25. of the method includes method detec tion limits sensitivity determination matrix effects interferences as well as any sample preparation processing specifications and overall operator assessment of the method It Is requested that as this type of information is developed It be forwarded to the FSMC System Coordinator A User Comment form has been included in Appendix C FIELD SCREENING METHODS Catalog FSMC TABLE OF CONTENTS 1 0 Introduction and Background 1 1 Field Screening Methods Catalog 1 2 Intended Users 1 3 System Updates 1 4 Technical Considerations 1 5 Overview of Levels and II Analysis 2 0 Installing the System 2 1 Installation on a Two Disk Drive Computer System 2 2 Installation on a Hard Drive Computer System 2 3 Installing FSMC More Than Once 3 0 Getting Started 3 1 Searching the Data Base 3 1 1 Searching by Chemical Name 3 1 2 Searching by Chemical Abstract Services Number 20 3 1 3 Searching by Chemical Class 3 1 4 Searching by Method Name or Number 3 1 5 Searching by the Sample Matrix 3 1 6 Searching by the Detection Limit Values and Units 4 0 Displaying and Printing Reports 5 0 FSMC System Requirements 5 1 Software Characteristics 5 2 Hardware Requirements Appendix A Field Method Listing Appendix B Historic Precision and Accuracy Data Appendix C User Comment Form 21 22 23 23 24 25 25 25 3 1 3 2 3 3 3 4 3 5 LIST OF FIGURES Main Menu Searching by Chemical Nam
26. oreliminary sample and the second is a larger volume sample based on results from the first APPLICATION Air monitoring as a time weighted average for low molecular weight vola tile organic compounds aromatics unsaturated hydrocarbons chlorinated hydrocarbons ketones alcohols etc LIMITATIONS Time consuming samples take 4 8 hours to collect Desorption efficiency is less than 100 Pre packed Tenax tubes may be contaminated Packing own tubes is recommended but requires laboratory and chemist INSTRUMENTATION USED Century Systems Programmed Thermal Desorber Model 132 A Century Systems Foxboro Organic Vapor Analyzer or other comparable GC or GC MS e g Photovac Finnigan etc PERFORMANCE SPECIFICATION DETECTION LIMIT 1 0 ug l using the Photovac or Finnigan GC MS for most volatile or ganics or 500 ug l using Foxboro OVA for most volatile organics SELECTIVITY Good separation of peaks ACCURACY 99 recovery of eleven spiked vinyl chloride samples using freshly packed coconut charcoal tubes lower recovery In other tests possibly related to spiking method PRECISION REPEATABILITY Standard deviation of spiked vinyl chloride samples was approximately 10 COMMENT Recoveries varied according to type and condition of carbon tube used and number of components in sample With 8 components recovery ranged from 3 106 for 4 components recovery range was 63 135 USE LOCATION USED Has been used at 30 50 lo
27. recovery of phenol lt 27 Analysis can be performed in a field laboratory METHOD DESCRIPTION Uses bonded phase extraction column with GC MS analysis to determine polycyclic aromatic hydrocarbons PAHs and phenols concentrations in water The procedure involves passing 50 100 ml of filtered ground water through a cyclohexyl bonded phase extraction column with a solvent methanol or acetonitrile and methylene chloride and injecting an aliquot directly into GC for analysis Response factors were developed using standard mixtures and used to convert mass spectra to quantities based on area of internal standard base peak APPLICATION Determination of concentrations of many phenols and PAHs plus ben zothrophene dibenzofuran and some nitrogen heterocycles LIMITATIONS Possible interferences from other electron capturing species Does not detect some phenols and nitrogen heterocycles e g phenol and 2 4 dimethyipyridine INSTRUMENTATION USED Finnigan OWA 1020 computerized capillary gas chromatograph quadrupole mass spectrometry system GC MS with 30 m fused silica column PERFORMANCE SPECIFICATION DETECTION LIMITS Less than 20 ug l for most phenols and PAHs SELECTIVITY Separate peaks easily identifiable ACCURACY Spike recovery for phenolic compounds except phenol 80 105 Spike recovery for PAHs and other neutral compounds 51 111 for nitrogen hete rocycles 3 197 for phenol 0 27 PRECISION REPEATABILITY
28. screening or analysis using portable instruments Results are often not compound specific and not quantitative but results are available in real time Level II field analysis using more sophisticated portable analytical instru ments in some cases the instruments may be set up in a mobile or onsite laboratory There is a wide range in the quality of data that can be gener ated Quality depends on the use of suitable calibration standards reference materials and sample preparation equipment and the training of the opera tor Results are available in real time or several hours Level Ill all analyses performed in an offsite analytical laboratory using standard documented procedures The laboratory may or may not be a CLP laboratory Level IV CLP routine analytical services RAS All analyses are performed in an offsite CLP analytical laboratory following CLP protocols Precision and accuracy data are presented in tabular fashion Footnotes to each table cite the sources of the data and the concentration or concentration range at which the precision and accuracy were determined When no concentration is cited no concentra tion information was available in the source material Precision is a measure of the variability in repeated measurements of the same sample compared to the average value Precision is reported as Relative Standard Deviation RSD The lower the RSD the more precise the data ST T bn OLT SM O NOILLO
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33. 3 To start the FSMC system enter A gt FSMC RETURN ENTER 4 When asked Do you have a hard drive Y N enter N RETURN ENTER The installation procedure will take about one minute After the installation is com pleted the main menu will appear 2 2 INSTALLATION ON A HARD DRIVE COMPUTER SYSTEM Throughout this manual It Is assumed that the hard disk is named C and the directory on which FSMC resides 15 C FSMC Other combinations are valid and should be designated during the Installation process 1 Create a directory on your hard disk C gt MKDIR FSMC RETURN ENTER 2 Switch to the FSMC directory C gt CHDIR FSMC RETURN ENTER 3 Insert the FSMC program diskette into drive A Switch to A drive C gt A RETURN ENTER 4 Start the system A gt FSMC RETURN ENTER 5 When asked Do you have a hard drive Y N enter Y RETURN ENTER 6 Enter a valid hard disk name RETURN ENTER The installation will then proceed After the installation is completed the main menu will appear The C drive will now be your current drive Return the program diskettes to the manual for future installations 2 3 INSTALLING FSMC MORE THAN ONCE The FSMC system has no limit to the number of times it may be installed however the installation procedures will appear automatically only the first time To install the system more than once select option 5 Utillities from the main menu and select
34. E TECHNICAL CONTACT Steve Simon AFFILIATION Lockheed Engineering and Management Services Co Inc TELEPHONE 702 734 3285 PREPARED May 18 1987 BIBLIOGRAPHY Eccles L A Simon S J and Klainer S M n Situ Monitoring at Superfund Sites with Fiber Optics U S EPA Environmental Monitoring Systems Laboratory Las Vegas NV EPA 600 X 87 156 June 1987 Milanovick F P Klainer S M and Eccles L A Remote Detection of Organochlorlides with a Fiber Optic Based Sensor Analytical Instrum 1986 15 2 137 Milanovick F P Klainer S M and Eccles L A Remote Detection of Organochlorides with a Fiber Optic Based Sensor II A Dedicated Portable Fluorimeter Analytical Instrum 1986 65 APPENDIX B HISTORICAL PRECISION AND ACCURACY DATA CLASSIFIED BY MEDIA BY ANALYTICAL LEVEL HISTORICAL PRECISION AND ACCURACY TABLES Introduction Table VVater Level III Other than CLP RAS Table B 2 Water Level III SW 846 Table B 3 Water Level IV Table B 4 Soil Level Table B 5 Soil Level Il Table B 6 Soil Level IIl Table B 7 Soil Level IV Table B 8 Air Level Table B 9 Air Level Il Table B 10 Air Level Ill Table B 11 Other Media Level 111 INTRODUCTION The data in this Appendix have been compiled to assist the reader in selecting an ana lytical method appropriate for each data use The methods are classified by media and by analytical levels defined as follows Level field
35. EARCHING BY THE SAMPLE MATRIX The user may select specific matrices air soil and water in order to constrain the search The user must enter a Y for each matrix desired The middle portion of Figure 3 5 displays the matrix options 3 1 6 SEARCHING BY DETECTION LIMIT VALUES AND UNITS if the user requires a certain detection limit or sensitivity level on which to search a method the user may enter a value and units for each matrix selected Only the methods that are valid at that detection limit or less will be selected If a 0 0 Is entered for any matrix ail methods for that matrix will be selected regardless of the detection limit The default units of measure may be changed by the user Valid units of measure for the detection limit are PPM parts per million and PPB parts per billion The middle portion of Figure 3 5 displays the detection limit option The example shows a detection limit minimum for air 10 0 PPM and for water 50 0 PPB 23 4 0 DISPLAYING OR PRINTING REPORTS If a search has been successful and one or more methods have been selected a DISPLAY PRINT menu presents the option to display the method s on the screen or to print them on an attached printer This menu is shown in the bottom portion of Figure 3 5 and summarized in the following table Option Number Result Display Method Headings Only Display Method Heading and Summary Display Complete Method Listing Print Method Headings Only
36. ECTIVITY Peaks are separate good selectivity ACCURACY Approximately 5 of true value Mean recovery of soil spike 97 98 Tested for eleven soil spikes PRECISION REPEATABILITY One sample run in triplicate gave standard deviation of 0 231 Two duplicate samples differed by 2 18 Relative standard deviation RSD of soil spike was 14 eleven samples COMMENTS Samples below the detection limit can be concentrated and re run USE LOCATION USED G E Moreau Schenectady N Y Modified at Wide Beach N Y EPA SITE NUMBER CERCLIS NYD980528335 MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP After a week of continuous use columns and detectors have to be cleaned and reconditioned requiring one and a half days of down time 42 ANALYSIS TIME 30 minutes per sample CAPITAL COSTS 18 000 00 CALIBRATION Calibration determined by the peak heights and retention times of PCB standards Standards and method blanks are run after every tenth sample COMMENTS This method has had very limited use PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT Lisa Gatton Vidulich AFFILIATION U S EPA Region Il Monitoring Management Branch TELEPHONE 201 321 6676 PREPARED April 17 1987 BIBLIOGRAPHY A Rapid Procedure for the Determination of Polychlorinated Biphenyls in Soils Draft U S EPA Region ll 43 METHOD FM 22 PESTICIDE ANALYSIS USING A GC WITH ECD HEXANE METHANOL EXTRACTION SUMMARY Rapid determination
37. ERCLIS site number where appropriate and matrix Preparation maintenance and cleanup Calibration Analysis time z Capital costs and Source of technical information It is important to note that these fields specify the parameters that have been utilized in the development and subsequent use of the methods and not necessarily the only possible choices For example the Instrument Used field for PCB Analysis Using a Gas Chromatograph in an On Site Laboratory Hexane Extraction shows that a Hewlett Packard 5880 Gas Chromatograph with an electron capture detector was used However any GC with analogous capabilities could be used to perform this analysis Caution should however be used to assure that modifications to the method will not effect the quality of the resulting data As such it is important to consult with an analytical chemist prior to modifying any of the methods contained in this Catalog 1 2 INTENDED USERS The FSMC system has been developed for individuals who are responsible for devel oping or overseeing sampling activities at Superfund hazardous waste sites As already mentioned these individuals require information regarding analytical screening techniques which have demonstrated field utility and which complement those methods used by the CLP The FSMC addresses the need of site personnel to determine what field methods if any are most appropriate in a given situation Based on preliminary site
38. ICALS l Aromatics 4 Base kid Chlorinated Hydrocarbons BNA Gasoline Coal Tar Volatiles Hydrocarbons Polynuclear Aromatics PNAs Volatile Organics Polcyclic Aromatics Unsaturated Hydrocarbons Hydrocarbons PAHs Semi volatiles 2 Aroclors 5 Heavy metals PCB Inorganics Metals 3 Insecticides Pesticides SELECT CHEMICAL CLASS 1 5 0 to exit 0 Figure 3 4 21 3 1 4 SEARCHING BY METHOD NAME OR NUMBER The user may enter a specific method name If the full name is not known enter a character string that you know is correct The search is designed to look for an embedded character string within a method name The system will match on what the user has entered display what was found and then permit the user to select the one desired If the method number is known the user can reduce typing and search time by entering the number instead of the name See Figure 3 5 SEARCH FOR A FULL OR PARTIAL METHOD NAME ENTER METHOD NAME OR NUMBER BLANKS TO EXIT headspac Enter ALL to select ALL Methods ENTER SEARCH PARAMETERS Enter Y for each matrix desired AIR Y N SOIL Y N 1 WATER V N 1 Pi DETECTION LIMIT PP P 8 for no limit s this correct Y N 11 DISPLAY or 21 PRINT HEADING ONLY 3 DISPLAY or 41 PRINT HEADING amp SUMMARY 151 DISPLAY or 161 PRINT COMPLETE METHOD S 5 Methods found SELECT DISPLAY PRINT 1 6 8 TO EXIT Figure 3 5 22 3 1 5 S
39. IIAN 4 ON 9 4 TWOIMOLSIH 11 8 Sigi U S GOVERNMENT PRINTING OFFICE 1988 548 158 87043 20 APPENDIX C USER COMMENT FORM FIELD SCREENING METHODS CATALOG FSMC USER COMMENT FORM Your comments and suggestions are important to us Comments may relate to the software user manual or mini guide or may be a request for an addition or correc tion to the method descriptions and additional copies of the system discs Please return this form to FSMC System Coordinator Office of Emergency and Remedial Response Analytical Operations Branch WH 548 A U S Environmental Protection Agency Washington DC 20480 Please provide the following information so that we may follow up if necessary Your name Address Phone number
40. ION MAINTENANCE AND CLEANUP Precautions should be taken not to contaminate column Occasional cleaning and reconditioning of column and detector required ANALYSIS TIME 20 25 minisample CAPITAL COST 20 000 00 46 CALIBRATION Calibration determined by peak areas and retention times of pesticide standards COMMENTS A much less expensive GC ECD could be used PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT William Loy AFFILIATION EPA Region IV ESD TELEPHONE 404 546 3386 PREPARED April 15 1987 BIBLIOGRAPHY Screening Method For Extractable Organic Compounds EPA Region IV Mobile Laboratory Protocol January 1987 47 METHOD FM 24 PHENOL DETERMINATION BY LIQUID LIQUID EXTRACTION AND GC ANALYSIS SUMMARY Detection of phenols in water to 100 ug l and soil to 25 ug kg Requires field laboratory and chemist METHOD DESCRIPTION Uses liquid liquid extraction with GC analysis to determine phe nols in soil and in water The procedure for soil analysis entails taking 2 3 grams of soil and extracting with methanol The procedure for water analysis consists of taking 20 ml of water adjusting the pH to 2 and extracting with methanol Extract for both soil and water s reacted with pentafluorobenzyl bromide and potassium carbonate in presence of hexacyclooctadecane catalyst to form pentafluorobenzyl PFB phenol derivative PFB de rivative is exchanged into hexane using liquid liquid extraction An aliquot of hexa
41. K beta etc Spectra are stored on computer disc for later printout and direct identification of each element ACCURACY Four samples analyzed for lead by CLP had values of 80 180 130 and 910 mg kg The range of values for the same samples analyzed by XRF were 100 300 100 200 95 120 and 800 900 mg kg respectively PRECISION REPEATABILITY Duplicate samples show good repeatability COMMENTS XRF is non destructive samples can be stored for future reference after analysis USE LOCATION USED Sudbery MA 1985 Non CERCLA EPA SITE NUMBER CERCLIS Non CERCLA MATRIX Soil and Water PREPARATION MAINTENANCE AND CLEANUP Soil samples dried 60 mesh screened are placed directly into sample cup aqueous samples are ion exchanged by passing through a resin coated filter paper XRF spectrometer must be set up and pro grammed Maintenance of the spectrometer includes checking probe for cleanliness and dryness and checking source decay Standards are prepared using 1 000 mg kg AA standard solutions for Ag Ba Mn Ni Sn Zn Se and Pb Standards can be prepared separately or as multi element mixtures and can be used up to 5 months ANALYSIS TIME 10 30 minutes for sample preparation Analysis time is less than 10 minutes CAPITAL COSTS 80 000 00 CALIBRATION Standards required at concentrations of 1000 500 250 and 125 mg kg for soil and 2 1 0 5 and 0 25 ug l plus a blank for water samples Run all standards at beginning of
42. Levels and Il analysis As a general rule of thumb Level analysis typically result in qualitative measurements for the presence or absence of classes of contaminants typically volatile organics although specific compounds can also be measured in certain instances while Level Il analyses can provide qualitative and frequently quantitative values for both groups and specific analytes At times the same instrument can be used for both Levels and li analyses For example an OVA a flame ionization organic vapor detector can be used in the survey mode for Level analyses to measure total organic vapor In the GC mode this same instrument can be used to obtain Level II data of specific analytes 1 1 FIELD SCREENING METHODS CATALOG One of the primary reasons for Superfund as well as RCRA and other EPA pro grams contamination monitoring at potential and known hazardous waste sites is the determination of the identity concentrations and vertical and horizontal extent of chemical contamination An essential element of any monitoring effort is analytical support that provides rapid sample throughput while matching the data quality objec tives of the sampling effort Experience gained during the first five years of the Superfund program has shown that various types of field screening analytical methods are suitable and are being used during field investigations to characterize hot spots evaluate the necessity of emergency respon
43. N RECORD CAS CHEMICAL NAME 71 43 2 BENZOL 85 68 7 BENZYL BUTYL PHTHALATE 85 68 7 BENZYL N BUTYL PHTHALATE 91 94 1 BENZIDINE 3 3 DICHLORO 91 94 1 3 3 DICHLOROBENZIDINE 92 87 5 BENZIDINE 95 50 1 0 DICHLOROBENZIDINE 95 50 12 DICHLOROBENZME 98 95 3 NITROBENZENE 98 95 3 NITRBBENZOL ENTER RECORD TO SELECT CORRECT NAME Enter 0 to return to the MAIN MENU Figure 3 2 3 1 2 SEARCHING BY CHEMICAL ABSTRACT SERVICES CAS NUMBER The user must enter a Chemical Abstract Services CAS Number including the dashes and not including preceding zeros The system will respond by displaying all chemical synonyms with that CAS number so that the user can verify the entry One chemical name is then selected to continue the search See Figure 3 3 Valid CAS Numbers Invalid CAS Numbers 7440 43 9 7429905 7143 2 0057 74 9 SEARCH FOR CAS NO 100 41 4 ETHYLBENZENE ENTER SEARCH PARAMATERS Enter Y for each matrix desired R1R 1 N 2 SOIL Y M 1 WATER V N J MX P DETECTION LIMIT 8 for no limit 15 this correct Y N 1 DISPLAY or 2 PRINT HEADING ONLY 31 DISPLAY or 41 PRINT HEADING amp SUMMARY 51 DISPLAY or 6 PRINT COMPLETE METHOD S 6 Methods found SELECT DISPLAY PRINT 1 6 8 10 EXIT Figure 3 3 20 3 1 3 SEARCHING BY CHEMICAL CLASS The user may request a search by one of five chemical class These classes are shown in Figure 34 FIELD SCREENING METHODS CATALOG FSMC SEARCH BY CLASS OF CHEM
44. N USED HNU Systems PI 101 Portable Photoionizer Available probes include 9 5 ev 10 2 ev and 11 7 ev PERFORMANCE SPECIFICATION DETECTION LIMIT 100 ug for most volatile organics Linear operating range for most compounds is IOO 60 000 ug l Useful range extends to 200 000 ug l SELECTIVITY Depends on probe ACCURACY Not tested PRECISION REPEATABILITY 1 at Full Scale Deflection Duplicate samples show good agreement COMMENTS Three probes are available that vary in sensitivity to organic compounds One probe 9 5 ev detects aromatics and large molecules The 10 7 ev probe detects the above compounds plus vinyl chloride MEK TCE and other 2 4 carbon compounds The 11 7 ev probe detects the above compounds plus halocarbons methanol and other single carbon compounds USE LOCATION USED Ottadi amp Gross Kingston Steel Drum Kingston NY 1980 EPA SITE NUMBER CERCLIS NHD990717647 MATRIX Air Headspace above soil sediment and water PREPARATION MAINTENANCE AND CLEANUP Recharge battery after use Clean light source window every few weeks 16 ANALYSIS TIME Response given in less than 5 seconds COST 5 000 00 CALIBRATION Zero electronically at start of day Check periodically Use calibration gas prior to each use COMMENTS Easy to train personnel in usage Used fairly regularly PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT Or Thomas Spittler AFFILIATION U S EPA Region Laboratory TELEPHO
45. NE 617 861 6700 PREPARED April 13 1987 BIBLIOGRAPHY Becker D L and Carter M H Equipment Available for Sampling and On Site Measurements U S EPA Document Number HQ 831104 May 30 1984 17 METHOD FM 9 HEADSPACE TECHNIQUE USING A MOBILE GC FOR VOLATILE ORGANICS VOCS SUMMARY Analysis of soil water and air samples for identification and quantitation of most VOCs to 0 5 ug l range Soil results are semi quantitative Depending on GC used is portable or requires field laboratory METHOD DESCRIPTION Used to screen water air soil and sediment samples on a GC with a PID FID or ECD Method involves collecting desired sample in a 40 ml vial pre paring sample if soil or sediment and sampling and analyzing vapor headspace above aqueous solution Air screened directly by collecting sample and injecting into GC for analysis Identification and quantitation is determined by comparing peak retention times and areas of standard solution to samples APPLICATION Good for most VOCs to low concentrations halogenated methanes and ethanes chlorinated hydrocarbons aromatics etc arsine phosphine hydrogen sulfide and carbon disulfide LIMITATIONS GC and sample need to be at same temperature in an area free of or ganic vapor For reproducibility surrounding temperature must remain constant Complex samples give co eluting peaks Identifications are considered tentative for soil INSTRUMENTATION REQUIRED Photovac Mode
46. OIL GAS SAMPLING USING DIRECT INJECTION STOPPER SUMMARY Sampling of VOCs in soil gas to determine ground water contaminant plume Requires probe installation for equilibration and repeated sampling Analysis can be performed using portable GC and or field laboratory METHOD DESCRIPTION A 12 17 foot borehole is drilled using a hollow stem auger 8 O D A sample probe is inserted borehole walls are allowed to collapse as the auger is pulled The hole is sealed with a bentonite slurry plug the probe is sealed with a stopper and screw cap Samples are collected by syringe after a 2 day equilibration period and analyzed by a GC APPLICATION Delineation of extent of contamination long term sampling of true soil gas concentrations LIMITATIONS Probe installation required INSTRUMENTATION USED Auger for drilling gas tight syringes for sampling GC for analysis PERFORMANCE SPECIFICATION DETECTION LIMIT 0 2 ug l for TCE in one study SELECTIVITY Volatile organics depends on GC method used ACCURACY Results correlated well with results from other sampling methods at same locations Correlation coefficients were 0 78 direct injection auger 0 87 one liter method 0 73 headspace method 0 98 Tenax PRECISION REPEATABILITY Field variability 33 RSD for 42 samples COMMENTS Occasional leaks in stoppers increased variability Water contamination ac curately reflected however number of samples was small and correlation ma
47. TOCOL AVAILABLE Yes SOURCE CONTACT NAME Richard Chappell AFFILIATION CDM INC TELEPHONE 303 458 1311 PREPARED April 6 1987 BIBLIOGRAPHY Chappell R W Davis A O and Olsen R L Portable X Ray Fluorescence as a Screening Tool for Analysis of Heavy Metals in Soils and Mine Waste Management of Uncontrolled Hazardous Waste Sites Washington D C December 1 3 1986 Chappell R W and Olsen R L EPA Memorandum XRF Field Analysis of Smuggler Mountain Soil Samples January 13 1986 Columbia Scientific industries Corporation Operating instructions X MET 840 Portable XRF Analyzer March 1985 METHOD FM 4 AIR MONITORING FOR VOLATILE ORGANIC COMPOUNDS USING PROGRAMMED THERMAL DESORBER PTD AND GC SUMMARY Air monitoring of volatile organics as a time weighted average to ug l range Time consuming Requires field laboratory METHOD DESCRIPTION Uses a field sampling pump programmed thermal desorber and a GC to evaluate volatile organic contaminants in air samples as a time weighted average Identification and quantitation is done by comparing peak retention times and heights of peaks with standards Sample acquisition involves collecting an adequate sample usually 10 30 liters of ambient air using a Tenax or activated carbon tube at tached to a pump The sample is thermally desorbed in the PTD Two samples are with drawn from the PTD and analyzed on the GC The first sample is usually a small volume
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49. United States Office of Emergency and EPA 540 2 88 005 Environmental Protection Remedial Response Agency Washington DC 20460 September 1988 Superfund SEPA Field Screening Methods Catalog Users Guide EPA 540 2 88 005 September 1988 Field Screening Methods Catalog User s Guide 250027 Office of Emergency and Remedial Response Hazardous Site Evaluation Division U S Environmental Protection Agency VVashington DC 20460 NOTICE The information in this document has been funded wholly or in part by the United Slates Environmental Protection Agency under Contract No 66 01 6939 to CDM Federal Programs Corporation and Roy F Weston inc It has been subject to the Agency s peer and administrative review and has been approved for publication as an EPA document Mention of trade names or commercial products does not neces sarily constitute endorsement or recommendation for use EXECUTIVE SUMMARY The Field Screening Methods Catalog FSMC is a technical document produced by the United States Environmental Protection Agency s Office of Emergency and Remedial Response Analytical Operations Branch This document is a compila tion of methods that were identified as being used in EPA Regions Several methods contain no method performance information because this information was not avail able The methods are provided as submitted by the technical contact listed in the method description The Analytical Operations Branch has not eval
50. Using Mini Barrel Sampler FM 12 Soil Gas Sampling Using a One Liter Syringe FM 13 Soil Gas Sampling Using Direct Injection Stopper FM 14 Soil Gas Sampling Using a Perforated Tube FM 15 Soil Gas Sampling Using Tenax Tubes FM 16 Soil Gas Sampling for Downhole Profiling FM 17 Soil Gas Sampling Direct Injection Auger FM 18 6 Analysis Using a Gas Chromatograph in an On Site Laboratory Hexane Methanol Water Extraction FM 19 PCB Analysis Using a Gas Chromatograph in an On Site Laboratory Hexane Extraction 0 FM 20 PCB Analysis Using a Gas Chromatograph in an On Site Laboratory Hexane Methanol FM 21 PCB Analysis Using a Gas Chromatograph in an On Site Laboratory Hexane Acetone Extraction FM 22 Pesticide Analysis Using a GC with ECD Hexane Methanol Extraction EE att ilata a ote Se Q Je S we oa FM 23 Pesticide Analysis Using Isothermal GC with ECD Hexane Extraction e aos sd S he Se FM 24 Phenol Determination by Liquid Liquid Extraction and GC Analysis FM 25 PAH Analysis Using GC with Heated Column FM 26 Total PNA Analysis Using an Ultraviolet Fluorescence Spectrophotometer ae ee eee r rr eee d METHODS UNDER DEVELOPMENT FM D1 Trace Atmospheric Gas Analyzer TAGA ooa aa FM D2 Use
51. VNIVAS NOILVZIHSLOVYVHD ALIS NOILVNIIWNYSLAG dud LOSSEN YS H NOI 1V 1N3IN3 du oNlunq ONIYOLINOW N9IS3Q SNIH33NI9N3 SSAILVNYALTV 40 NOILVNIVAS NOILVZIHSLVYVHO 3115 NOLLVINGIG viy NOILLVZIUSLOVUVHO 315 939 0 100 1 OOQ 48 WD 53 8 3l1VlHdOHddV 210N A 13A31 N 14A41 III 14Az1 Il 14Ad1 I 14Az1 3SN viva VLVG Ad ST3A31 TVOLLA TVNV 3lVItidOtiddV cc 4148V1 The decision to use field anaiytical screening techniques i e Levels and ii must be made on a site specific and on a sampling event by sampling event basis Factors to be considered include data quality requirements parameters for which the analytical method is valid contaminants of concern required detection limits and the range of precision accuracy representativeness completeness and com parability PARCC required and provided by each analytical option Documentation and chain of custody considerations are also relevant and should be considered While representativeness completeness and comparability are for ail practical pur poses sampling considerations precision and accuracy encompass both sampling and analytical considerations and define the quality of the resulting data Precision measures the reproducibility of measurements under a given set of conditions Specifically it is a quantitative measure of the variability of a group of measurements compared to their average valu
52. WELXS PT T 5n 9 Z T0S Tr T 5n oss SM aVuL 9 Bund pp T bn gt T TOS 0 T 5n 007 SW D9 z T 5n 6 29 ur1ogjgouo1g 62 T 5n OLT SW DD NOLLOWELXa T9 T 5n gr Z T0S T 5n oss SW DD dt 9 Bina 99 T bn ep T TOS 81 T 5n opp SH D9 82 T bn g 29 9 20 TZ T 5n 001 5 0928 TZ T 5n 087 SW D9 9T T 5n TT 29 u zu g asu KE SQOINHOGL SULA TWNW NOIS load NOLLWULNGHONOD QOHLAN SCOHIGW SVU 412 NVHL MEUHLO SCOHLAW SANOINHOSL TWOILATWNW III 4ASI ATALVM VLVG XOVUDOOV ANY NOISIOGYd TWOIMOLSIH 1 8 Sigi 70 Ur yy 3 0 272 SWIG TZ SZ T LE HE DE 6T T 92 89 PT v9 TI T asa NOIS Lg T bu T bu 1 Ldbpn 1 T 5bn 1 1 1 T 5n 1 1 L bn T bn 202 12 01 HI 0SS 8 0 09 1 8 OLT 811 055 610 002 CR DNVS NOLLVMLN432NO2 SW D9 T9 SW 0D NOLLOVMULXA3 Z T0S SW 0D dt 9 404 04 T T0S SW D9 29 SM O9 NOILOW amp LXG 105 SW DD dt 9 2044 1 10S SW 29 PCH SNOINHOAL GOHISHW ucu3 uozoTuoouo q q wIOJOIOTUD SALATVNVY SCOHLAN SVU 410 NVHL SAOHIAW 98 1 TVOILATYNY 111 HANI b nu12uo2 pudLVM WIVG AOQWHNOOW NY NOISIOWYd TWOINOLISIH 1 9 419 1 saqATeue UO UOT eULIOFUT 2023 p 31nsuo aq pTnous qu umoop
53. analysis consists of extracting contaminants from 100 ml water sample into 1 ml methylene chloride by vortex mixing Procedure for soil analysis consists of mixing 2 3 grams of soil with 6 ml methylene chloride and separating methylene chloride Extraction step for soil and water is repeated and extracts are combined The methylene chloride is passed through a silica gel column to remove potential interferences before GC analysis Method is a modification of EPA method 610 APPLICATION Rapid identification and quantitation of polycyclic aromatic hydrocarbons LIMITATIONS Possible co eluting peaks e g phenanthrene and anthracene Method gives poor spike recovery for naphthalene Does not detect many semi volatlles INSTRUMENTATION USED Shimadzu Mini 2F or Shimadzu Mini 3 GC FID with 6 foot glass quantitation and confirmation column PERFORMANCE SPECIFICATION DETECTION LIMITS 500 1000 ug in water and 50 500 ug kg in soil for PAHs SELECTIVITY Peaks usually separate and give good selectivity Occasional co eluting peaks ACCURACY Spike recovery for 12 different compounds in soil 67 129 naphthalene excluded 14 recovery PRECISION REPEATABLLITY Relative Standard Deviation RSD for 12 different com pounds in soil 7 8 55 7 COMMENTS None USE LOCATION USED J H Baxter Washington 1986 EPA SITE NUMBER CERCLIS WAD009265521 WAD053823019 MATRIX Soil and Water PREPARATION MAINTENANCE AND CLEANUP Columns and
54. arge distances with low light loss transmission depends on the core having a higher index of refraction than the cladding Configurations include use of laser induced fluorescence absorption spectroscopy raman spectroscopy amp mul tivariate spectral analysis A fiber optical chemical sensor FOCS unit includes a chemical specific sensor amp can operate in at least three modes fluorescence absorption amp refraction A FOCS can respond to a class of compounds or a single species APPLICATION In situ real time monitoring of environmental contamination Particularly suited for inaccessible or hazardous situations e g ground water spill cleanup monitoring LIMITATIONS A different FOCS is needed for each pollutant to be monitored increasing development costs but many can be bundled n a lt l 2 package Both techniques are still developmental INSTRUMENTATION USED Optical fibers with special coatings attached to various ana lytical instruments e g a portable laser spectrometer fluroesence spectrometer etc PERFORMANCE SPECIFICATION DETECTION LIMIT RFS Low ug l range for aromatic gasoline components using laser Induced fluorescence ug l for organophosphorus pesticides A other compounds using raman spectroscopy FOCS low ug l range for chloroform SELECTIVITY RFS fluorescence spectra showed good separation of contaminants from background FOCS sensors for specific chemicals used thus selectivity is high
55. ars requires addition time Some interferences possible with hydrocarbons and chlorinated solvents lacks isomer specificity requires frequent recalibration standard QA QC procedures not compatible Analyses are performed in specially build mobile laboratory METHOD DESCRIPTION Triple quadrupole MS MS analyzes polar and non polar com pounds in ambient air using direct sampling The MS MS uses the ambient air as its chemical ionization reagent gas Chemical ionization of target compounds achieved by charge transfer hydride abstraction halide abstraction hydride halide abstraction proto nation and or adduct formation lonization is determined by the compound class being analyzed and the instrument source being used In tandem mode preselected ions are fragmented and analysed to produce characteristic mass spectra specific fragment ions can be sought In single mass analyzer mode scans all ions produced For air analyses chromatographic separation is not compatible with the existing software Some type of parallel GC sampling is recommended for compound confirmation lon signals obtained in the tandem mode can be used to directly calculate air concentration APPLICATION For air and soil gas samples instant real time screening and monitor ing of concentration changes over time eg plume tracking and characterization for polar and nonpolar compounds including amines nitrogen and sulfur containing hete rocyclic compounds oxygenated hyd
56. atomic units INSTRUMENTATION USED Automated spectrophotometer microtiter plate reader IBM compatible personal computer printer and software package PERFORMANCE SPECIFICATION DETECTION LIMIT 25 ug for pentachlorophenol without sample concentration depends upon binding strength of antibody for target compound and is compound specific SELECTIVITY Each assay is highly selective for a single compound with minor or no cross reactivity Antiboides can also be developed which exhibit broad cross reactivity with compounds of similar structure ACCURACY Not available PRECISION REPEATABILITY Not available preliminary results show 10 20 variability between samples COMMENTS Each sample must be tested in triplicate to provide statistically valid results Performance data is being compiled in conjunction with US EPA EMSL Las Vegas USE LOCATION USED Mobile laboratory and laboratory setting EPA SITE NUMBER CERCLIS N A MATRIX Water soil 62 PREPARATION MAINTENANCE AND CLEANUP Antibodies recognize and bind to spe cific chemical structures so sample cleanup amp purification may not be critical in many cases Sample preparation for soil samples requires extraction or solvent exchange into a polar solvent prior to introduction into the immunoassay Aqueous samples can usually be analyzed directly or concentrated using reverse phase adsorbtion columns ANALYSIS TIME 4 hours per plate up to 24 samples per plate s
57. atory TELEPHONE 617 861 6700 PREPARED April 7 1987 BIBLIOGRAPHY Quimby J M Cibulskis R W and Gruenfeld M Evaluation and Use of a Portable Gas Chromatograph For Monitoring Hazardous Waste Sites National Conference on Management of Uncontrolled Hazardous Waste Sites November 29 December 1 1982 Washington D C METHOD FM 8 HEADSPACE ANALYSIS USING HNU PID FOR TOTAL VOLATILE ORGANICS SUMMARY Portable instrument that gives rapid analysis of total organic vapor con centrations in water soil and sediment to 100 ug l benzene equivalent METHOD DESCRIPTION Used to screen water soil and sediment samples for total or ganic vapor concentration HNU is a portable photoionization detector that requires inter nal electronic calibration as well as calibration to a known standard After sample is collected it can be analyzed by inserting probe of HNU into headspace of jar Alternative procedures to place probe directly above soil or insert probe into a shallow hole APPLICATION Measures total organic vapor concentration Response to VOC varies with probe used Insensitive to methane May detect unsaturated hydrocarbons chlorin ated hydrocarbons aromatics nitrogen and sulfur compounds aldehydes ketones alco hols acids and others LIMITATIONS Not able to identify Individual compounds Total response reported as benzene equivalent High ambient humidity causes erratic responses usually low INSTRUMENTATIO
58. bents for the Sampling of Priority Pollutants in Wastewaters Journal of Chromatographic Science Vol 22 p 313 320 August 1984 61 METHOD FM D4 IMMUNOASSAYS FOR TRACE ORGANIC ANALYSIS METHOD UNDER DEVELOPMENT SUMMARY Alternative inexpensive and simple analytical technique incorporating mono clonal antibodies for the quantitative measurement of organic chemicals in ground water amp other media Method for individual chemicals in varying stages of development development nearly complete for pentachlorophenol Preliminary data indicates sensitivi ties equal to GS or HPLC methods METHOD DESCRIPTION Developmental stage technique which is a competitive inhibition enzyme immunoassay EIA that incorporates monoclonal antibodies produced via ceil fusion hybridoma technology The EIA steps include the addition of reagents e g anti bodies and samples standards to a microtiter plate a 3 hour incubation and spectro photometric analysis of microtiter plate A colorimetric reaction indicates the concentration of target compound by reference to a standard curve APPLICATION inexpensive rapid and high volume anlysis of organic compounds in aqueous media Solid phase or oily samples must be extracted into polar solvents prior to introduction into the assay Antibodies can distinguish stereoisomers LIMITATIONS Limited field studies to date Antibodies methods cannot detect organic compounds of molecular weight less than 100
59. cable 48 MATRIX Water and Soil PREPARATION MAINTENANCE AND CLEANUP Column cleaning and recondltloning re quired occasionally Column can be saturated easily by concentrated samples ANALYSIS TIME 20 40 min sample depending on column length CAPITAL COST 4520 Shimadzu GC with ECD CALIBRATION Standards necessary to identify and quantify compounds Calibration Is done using mixed standard solutions of known concentrations A minimum of three stan dard solutions should be used for calibration COMMENTS Interpretation of results requires a trained chemist Used occasionally in Region X PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT John Ryding AFFILIATION C C Johnson amp Malhotra TELEPHONE 303 433 6966 PREPARED April 22 1987 BIBLIOGRAPHY McGinnis Roger Screening Method for Acid Extractables Phenols in Soil and Water EPA Document No TDD R10 8601 04 September 1986 49 METHOD FM 25 PAH ANALYSIS USING GC FID WITH HEATED COLUMN SUMMARY Detects PAHs in water and in soil to ppm range GC may give overlapping peaks hindering identification Has trouble determining naphthalene METHOD DESCRIPTION Requires a field laboratory with a gas chromatograph able to heat column above ambient temperatures for polycyclic aromatic hydrocarbon PAH de termination Identification and quantitation is done by comparing peak retention times and peak areas between standards and samples Procedure for water
60. cations in New England and elsewhere EPA SITE NUMBER CERCLIS Not Available MATRIX Air PREPARATION MAINTENANCE AND CLEANUP Tubes are prepared by thermally de sorbing in PTD and cleaned to background levels less than 1 ug l If tubes are dirty or contaminated they may have to be cleaned and repacked or replaced ANALYSIS TIME 4 8 hours for sample collection 5 minutes desorbing 5 minutes analysis time CAPITAL COSTS 5 990 for Model 132A PTD 5 200 6 325 for OVA CALIBRATION Calibration determined by peak heights and retention times for stan dards Run standards as for GC or GC MS COMMENTS The Interpretation of results requires a trained chemist Method is used on average 2 3 times per year in Region 1 PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Dr Thomas Spittler AFFILIATION U S EPA Region Laboratory TELEPHONE 617 861 6700 PREPARED April 7 1987 BIBLIOGRAPHY Spittler T M Siscanaw R J and Lataille M M Correlation between Field GC Measurement of Volatile Organics and Laboratory Confirmation of Collected Field Samples Using the GC MS National Conference on Management of Uncontrolled Hazardous Waste Sites November 29 December 1 1982 Washington D C Chapman H and Clay P Field Investigation Team FIT Screening Methods and Mobile Laboratories Complementary to Contract Laboratory Program CLP TDD HQ 8507 01 October 17 1986 METHOD FM 5 VOLATILE ORGANIC COMPOUND VOC
61. check for contamination by GC analysis check soil probes by drawing air through and analyzing Teflon may be subject to carry over from high liquid or gas phase concentrations ANALYSIS TIME 40 min sample 32 CAPITAL COST Syringes 30 40 sampling pump 100 500 Both are reusable CALIBRATION N A COMMENTS One of several soil gas sampling methods each has advantages under various circumstances PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Andrew Hafferty AFFILIATION Ecology and Environment Inc TELEPHONE 206 624 9537 PREPARED May 6 1967 BIBLIOGRAPHY Chapman H and Clay P Field Investigation Team FIT Screening Methods amp Mobile Laboratories Complementary to Contract Laboratory Program CLP TDD HQ 8507 01 October 17 1986 Draft 33 METHOD FM 17 SOIL GAS SAMPLING USING DIRECT INJECTION AUGER DIA SUMMARY Rapid sampling technique for soil gas analysis to aid in ground water plume determination Repeated sampling not possible once auger is pulled Analysis can be performed using a portable GC and or field laboratory METHOD DESCRIPTION A 12 17 foot borehole is drilled using a hollow stem auger 8 O D When desired sampling depth is reached a 500 ml gas tight side port syringe is lowered and filled Syringe contents are injected directly into a GC APPLICATION Delineation of extent of contamination rapid soil gas sampling LIMITATIONS No repeated sampling Lack
62. ctober 17 1986 Draft 13 METHOD FM 7 HEADSPACE TECHNIQUE USING AN OVA FID VOLATILE ORGANIC COMPOUNDS SUMMARY Rapid analysis of total VOCs or identification of individual components in soil water or air OVA is portable Soil results are semi quantitative Field instruments give better sensitivity METHOD DESCRIPTION Used to screen water soil and sediment samples on an OVA a portable GC equipped with a flame ionization detector Method involves collect ing samples in a 40 ml vial preparing sample if it is soil or sediment and sampling the vapor headspace above the aqueous solution The vapor sample is analyzed by the OVA Air may be screened directly by injecting it into the OVA Identification and quantitation determined by comparing the peaks of standards to samples A modification of this method involves placing the probe directly above the soil sample or inserting the probe directly into a shallow bore hole APPLICATION Analysis for low molecular weight total volatile organic concentration or for identification of specific constituents with the use of proper standards LIMITATIONS Measures volatile organics only Highly volatile organics such as methane tend to skew analysis for total VOCs Light VOCs e g vinyl chloride are rapidly eluted from column and are difficult to detect Response given in methane equivalent OVA op erates at ambient temperatures therefore for reproducibility surrounding temperatures must
63. d On Site Measurements Appendices TDD HQ 8311 04 EPA Contract 68 01 6699 NUS Corporation May 30 1984 includes EPA report and company literature 57 METHOD FM D2 USE OF BONDED SORBENTS FOR PESTICIDE ANALYSIS METHOD UNDER DEVELOPMENT SUMMARY Method is faster than traditional liquid liquid extraction Determines pesticide concentration in water to ug l Requires field laboratory and trained chemist METHOD DESCRIPTION Uses bonded phase extraction column with GC and ECD to determine pesticide concentrations in water The procedure involves passing 100 ml of filtered ground water through a cyclohexyl bonded phase extraction column with 1 ml ethylacetate as the elution solvent The extract injected into GC for analysis Identification and quantitation are performed by comparing peak heights and areas to standards APPLICATION Determination of pesticide concentrations in water LIMITATIONS Possible interferences from other electron capturing species INSTRUMENTATION USED Varian Model 3700 GC equipped with a nickel electron cap ture detector and a glass capillary column PERFORMANCE SPECIFICATION DETECTION LIMITS 1 ug l for most pesticides SELECTIVITY Separate peaks compounds usually easily identified Occasional interfer ences from other electron capturing species ACCURACY Spike recoveries for 5 replicates of 9 compounds 79 105 PRECISION REPEATABILITY Coefficient of variation for 5 replicates 4 COMMENTS Pe
64. d correlation to GC MS data At higher levels there is a discrepancy between data sources by a factor of two Bias ranged from high to low with increasing concentrations PRECISION REPEATABILITY Not available COMMENTS This method was developed by Region IV and until recently was not used as a quantitative method USE LOCATION USED Not used in field EPA SITE NUMBER CERCLIS Not applicable MATRIX Air Headspace above soil sediment or water PREPARATION MAINTENANCE AND CLEANUP Column and detector cleaning and re conditioning almost nonexistent because of the nature of headspace analysis Samples must equilibrate in sampler 1 hour before analysis 10 ANALYSIS TIME 30 40 nin sample CAPITAL COST Approximately 20 000 for Perkin Elmer GC with PID and ECD Approximately 8 000 for Hewlett Packard headspace sampler CALIBRATION 3 point standard calibration curve necessary to accurately quantify com pounds detected by GC Single point calibration is adequate for semiquantitative data Standard is known quantity of organic vapor in equilibrium with air with an aqueous or ganic solution COMMENTS The interpretation of results requires a trained chemist This method has been used in Region IV laboratory but has yet to be used in the field PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT William Loy AFFILIATION U S EPA Region IV ESD TELEPHONE 404 546 3386 PREPARED April 16 1987 BIBLIOGRAPHY Screening
65. d for field personnel and provides a concise description of each method which provides field staff with the information needed to consider the range of analytical methods that might be appropriate for the site The computer program is written on dBase lll is IBM compatible and provides search capabilities according to chemical of interest class name or CAS number or method name or number The search options also prompt the user to select a matrix of Interest air soil and or water and a detection limit to match and provide an available method that will meet the need of the user as closely as possible Once a method or methods that can potentially meet the user s need is found a number of options are available to view and or print the method s These options are discussed in more detail in Section 4 0 In addition this volume provides an Introduction a computer user s guide including an appendix containing copies of the thirty one methods For ease of use and consistency a standard set of Fields or major headings have been developed to organize method specific information These information provided for each method include the following Method name and number number is specific to this Catalog Summary and method description x Application limitations and instrumentation used Performance specifications such as detection limits selectivity curacy precision and repeatability Use of the method location C
66. d method due to its size limited availability and cost However since these methods represent an available tech nology they have been retained in this Catalog in a separate section These five methods have not been segregated in the computerized data base and as such will be selected when the appropriate parameters are input in considering the applica bility of these five methods the user should be aware of the above mentioned limitations and take sufficient CWQC steps to allow an assessment of data quality to be performed For the purposes of this Catalog the term field methods is used as a catch ail phrase and includes methods which utilize hand held instrument and or instruments which can be carried with relative ease portable instruments which can be set up and used in the back of a van or field trailer and fieldable instruments which usually require a more stationary and stable environment such as a field mobile laboratory These terms are defined in more detail in Section 1 5 The methods presented in this Catalog include analyses for metals volatile and semi volatile organics phenols pesticides PCBs dioxins and polycyclic aromatic hydrocarbons In addition several soil gas sampling techniques have been included because of the expanding use of such techniques The FSMC consists of a reduced pocket guide a computerized retrieval system stored on two floppy disks and a user s guide The pocket guide was designe
67. d syringes required ANALYSIS TIME 15 30 minutes to drill borehole 1 minute for sample collection 34 CAPITAL COSTS Syringes 30 40 GC 4 100 20 000 CALIBRATION Purge syringes with nitrogen and check for contamination by injecting carrier gas samples into GC COMMENTS Sample collection relatively easy Minimal sample preparation required before analysis PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT John Ryding AFFILIATION CC Johnson amp Malhotra TELEPHONE 303 433 6966 PREPARED May 6 1967 BIBLIOGRAPHY Jowise P P Villnow J D Gorelik L I and Ryding J M Comparative Analysis of Soil Gas Sampling Techniques Management of Uncontrolled Hazardous Waste Sites Washington D C December 1 3 1986 p 193 199 35 METHOD FM 18 PCB ANALYSIS USING A GAS CHROMATOGRAPH IN AN ON SITE LABORATORY HEXANE METHANOL WATER EXTRACTION SUMMARY Rapid determination of major Aroclors to 200 ug kg in soil Accurate to 100 000 ug kg then underestimates by 60 Requires field lab Appropriate extraction solvent should be determined by laboratory testing prior to field use METHOD DESCRIPTION Requires a field laboratory with a GC and linearized electron capture detector for PCB analysis of soil samples Identification is done by comparing peak retention time with external standards Quantitation is determined by comparing peak heights and volumes of the standard and sample Sample preparation consists
68. ds Level IV significantly less information exists for the other levels of analysis including Level V Historic accuracy and precision information has been compiled and classified by media and by analytical level EPA 1987 OSWER Directive 9355 0 7A This information is excerpted and presented in Appendix B The available data base for documenting accuracy and precision as well as mini mum detection limits for Levels and Il is sparse To supplement the sparse and scattered information which exist in published and unpublished reports etc person nel who use the methods presented in the FSMC are encouraged to catalog the precision and accuracy that is obtained during his her specific use and to provide this Information to the FSMC Systems Coordinator Based on the required data quality objectives and data uses the choice to use field screening analytical methods should be made in conjunction with a confirmation program to include a rigorous QA QC program analysis of QC samples instrument calibration and Level III or IV confirmation The user is urged to consult both the Data Quality Objectives for Remedial Response Activities and the Compendium of Superfund Field Operations Methods Manuals EPA 1987 OSWER Directive 9355 0 7A and EPA 1987a OSWER Directive 9355 0 14 as part of the decision process used to define the appropriate levels of analytical support It is further recommended that based on the Intended data uses a
69. dson Feldt U S EPA Hazardous Site Control Division William Venit U S EPA Region VI Herbert Moseley U S EPA Systems Coordination Section P K Chattapadhyay Ecology and Environment Inc 1 0 INTRODUCTION AND BACKGROUND The United States Environmental Protection Agency EPA awarded the first two major hazardous waste contracts in 1979 Since that time the scope and nature of hazardous waste Investigations have grown and matured The culmination of this maturation process is the present day Super fund Program as amended by the Superfund Amendments and Reauthorization Act of 1988 SARA Throughout this period of maturation the basic initial yet complex premise of field investigations has remained the same to determine the chemical constitue its identity and quantitation in environmental media air soil water as well as source media such as sludges and materials from containers including drums and tanks An additional complexity which became evident as field investigations were initiated was the frequent need for rapid turnaround of sample analysis results This was critical for example to evaluate if emergency response was necessary The Contract Laboratory Program CLP was established by EPA to provide analyti cal support for the massive amount of data that was being generated by the nu merous hazardous waste sites throughout the country This program provides a range of analytical chemistry services of kno
70. e Precision is usually stated in terms of standard deviation but other estimates such as coefficient of variation relative standard de viation range maximum value minus minimum value and relative range are also common Since precision defines the scatter of results about a mean value a lower standard deviation means less scatter The overall precision of measurement data is a mixture of sampling and analytical factors Analysis of field and laboratory replicates provides a measure of overall precision Accuracy measures the bias in a measurement system Sources of error are the sampling process field contamination preservation handling sample matrix sample preparation and analysis techniques Sampling accuracy can be assessed by measuring the concentration of contaminants in field trip blanks while analytical accuracy may be assessed through use of known and unknown QC samples and matrix spikes Accuracy is most frequently reported as percent recovery or percent bias A 100 recovery indicates a completely accurate measurement the greater the deviation e under or over is from IOO the less accurate the measurement Percent bias reports the difference of the result from the true value A completely accurate measurement would have zero percent bias the lower the percent bias the more accurate the measurement While historical accuracy and precision information which is classified by media are available for CLP analytical metho
71. e Searching by CAS Number Searching by Chemical Class Searching by Method Name vi 18 19 20 21 22 LISTING OF METHODS PRIMARY METHODS 2 4 5 6 FM 7 FM 8 FM 9 FM 10 FM 11 FM 12 FM 13 FM 14 FM 1 5 FM 16 FM 17 FM 18 FM 19 FM 20 FM 21 FM 22 FM 23 FM 24 FM 25 FM 26 Field Atomic Absorption Analysis lt s s t t t eee X Ray Fluorescence in Laboratory for Heavy Metals X Ray Fluorescence for Heavy Metals On site Air Monitoring for Volatile Organic Compounds Using Programmed Thermal Desorption and GC Volatile Organic Compound Analysis Using GC with Automated Headspace Sampler a a Headspace Technique Using an lon Detector for VOC Analysis Headspace Technique Using an OVA for VOCs Headspace Analysis Using HNU for Total Volatile Organics Headspace Technique Using a Mobile GC for VOCs Passive Soil Gas Sampling Using Industrial Hygiene Samplers Soil Gas Sampling Using Mini Barrel Sampler Soil Gas Sampling Using a One Liter Syringe Soil Gas Sampling Using Direct Injection Stopper Soil Gas Sampling Using a Perforated Tube Soil Gas Sampling Using Tenax Tubes gt t t Soil Gas Sampling for Downhole Profiling Soil Gas Sampling Direct Injection Auger PCB Analysis Us
72. e column can easily be saturated by concentrated samples resulting in an inoperable unit Used routinely PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Dr Thomas Spittier AFFILIATION U S EPA Region Laboratory TELEPHONE 617 861 6700 PREPARED April 7 1987 BIBLIOGRAPHY Chapman H and Clay P Field investigation Team FIT Screening Methods and Mobile Laboratories Complementary to Contract Laboratory Program CLP TDD HQ 8507 01 October 17 1986 Draft Clark A E Latailie M and Taylor E L The Use of a Portable PID Gas Chromatograph for Rapid Screening of Samples for Purgeable Organic Compounds in the Field and in the Lab U S EPA Region Laboratory June 29 1983 Morin S O Development and Application of an Analytical Screening Program to Superfund Activities Management of Uncontrolled Hazardous Waste Sites Washington D C November 4 6 1985 19 METHOD FM 10 PASSIVE SOIL GAS SAMPLING USING INDUSTRIAL HYGIENE SAMPLERS SUMMARY Passive sampling for volatile organics as a way to detect and estimate ground water contamination Concentrations obtained by calculation Site conditions affect results Field laboratory or off site analysis possible METHOD DESCRIPTION Passive sampling using open inverted Louart metal cans con taining an activated carbon organic vapor monitor are buried at one foot depths in area to be sampled exposed for a time determined by sampling rate for
73. eA ay ainseam p sn uorsr5 i4 70 q3 S UT3 OT SS T SEM SrTU3 S SVI 1501 UI 3TuTT ie U 10 3s 3a qut Jo ATeuc ai JO suoT3ei3u ouoo DAOU U3TA setdues pue sasXjTeue 2 01 sem 3u z d aberaae ue se paquasaad Adeinoow O139Z aAOge ST NTLA ey soUEPTJUOD 66 YIM pue peinseau ued yey oue sqns e JO uorqe qu ouoo WNUTUTM m ST STU UO p 3sTT se IAN 3TUT1 UorT452 43 q SHION TQETT AV JON VN q ATuo 104 pb T 5H T WN VN T 9LE Wda SepTF TNs 0606 LPM 2070 Z ST 210 201 58 2756 Vaz s prueXo 0106 2000 0 0 9 6 0 SZT 18 Sb Wda AUNOWAWN sTe3 y 0171 T W Co 10070 WN WN 002 va d9 SSITAWW1I 51929 S T2 S 000L S 10 0 WN WN 002 va satzes 000L HWV STe2 H TSN SL E T qsu 6 TZ WN L 00Z dWOI Steen 8 T 5u 5 oanos BIEN pou3 y 1 qumN 70 DOTStOa1d eed SCOHLIN 9p8 MS III THAT p nurquoo MALVM VIVG ADWHNDOW ANV NOISIOSYd TVOTMOLS H CR ERIC Kat DC 62 62 Le yc 6z yc y 21 91 21 TT YT LT T 81 6T TT 21 61 T 21 LE ET 02 95 4054 5 NOISIOgud gt VN 2
74. each day and run a set every fourth hour of analysis or after all samples have been analyzed whichever is more frequent Additional standards must be prepared and used to cover the entire working range of required analyses COMMENTS Spectrum displayed on video screen and stored in computer disk Used routinely in Region 1 Sample quantity needed for analysis is 1g of soil or 40 ml for water PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Dr Thomas Spittler AFFILIATION U S EPA Region Laboratory TELEPHONE 617 861 6700 PREPARED April 7 1987 BIBLIOGRAPHY Furst G A Spittler T and Tillinghust V Screening For Metals at Hazardous Waste Sites A Rapid Cost Effective Technique Using X Ray Fluorescence Management of Uncontrolled Hazardous Waste Sites Washington D C November 4 6 1985 METHOD FM 3 X RAY FLUORESCENCE XRF FOR HEAVY METALS ON SITE SUMMARY Good for on site screening of some metals in soil to minimum of 15 mg kg Sample matrix may cause accuracy problems Uses portable XRF analyzer METHOD DESCRIPTION Uses flux of high energy X rays to bombard sample causing elements in sample to emit energy at characteristic wavelengths Instrument separates wavelengths produced into a spectrum that contains energy peaks characteristic of ele ments present Concentration of each element present Is directly proportional to the in tensity of energy produced for that element This technique has been used to screen
75. ementary to Contract Laboratory Program CLP TDD HQ 8507 01 October 17 1986 Draft 41 METHOD FM 21 PCB ANALYSIS USING A GAS CHROMATOGRAPH IN AN ON SITE LABORATORY HEXANE ACETONE EXTRACTION SUMMARY Rapid determination of major Aroclors down to 2 000 ug kg in soil Requires field laboratory Method was not tested for all PCBs Appropriate extraction solvent should be determined by laboratory testing prior to field use METHOD DESCRIPTION Requires field laboratory with a gas chromatograph GC and linearized electron capture detector ECD for PCB analysis of soil samples Identification is done by comparing peak retention times with external standards Quantitation is deter mined by comparing the peak heights and volumes of the standard and sample Sample preparation consists of mixing 10 15 grams of soil with a UV grade 1 1 hexane acetone solution followed by extraction Florisil SepPak used to adsorb interferences from so lution Extract from SepPak then screened by GC analysis APPLICATION Simple and rapid determination of polychlorinated biphenyls Aroclor 1232 1242 1248 1254 and 1260 LIMITATIONS Method was not tested for all PCBs INSTRUMENTATION USED Hewlett Packard HP Model 5840 A Gas Chromatograph with one glass column or HP Model 5880 A Gas Chromatograph with one glass column with AID 511 or Shimadzu Mini 2 with Electron Capture Detector PERFORMANCE SPECIFICATION DETECTION LIMIT 2 000 ug kg SEL
76. es DQOs recognize and promote the concept that In the course of a typical Superfund reme dial investigation samples are taken with various objectives and that these various objectives require different data quality In other words not all objectives require for example CLP quality data While DQOs present a framework for identifying and achieving site specific data quality objectives through the appropriate sampling and analytical techniques the Compendium focuses primarily on Sampling techniques and methods used during the fieldwork phase of a remedial investigation DQOs define five levels of analytical support which are available for sample analysis These levels are based on numerous factors Including and foremost data quality requirements These five levels of analytical support are defined as Levels through V and range from hand held equipment and screening techniques to sophisticated GUMS instrumentation and analysis Specific discussions of these analytical levels their applicability and limitations as well as specific directions for use are contained in both the Compendium of Superfund Field Operations Methods and in the Data Quality Objectives for Remedial Response Activities EPA 1987a OSWER Directive 9355 0 14 1987 OSWER Directive 9355 0 7A In addition a brief overview of these five analytical levels is Included in Sections 1 4 and 1 5 It should be noted that no clear delineation exist especially between
77. everal plates may be run concurrently CAPITAL COSTS 22 000 for complete system including spectrophotometer computer can purchase without software printer plate washer micropipetters CALIBRATION Prepare a standard curve amp controls along with samples The standard curve is developed using known concentrations of the target compound amp occupies 18 wells on the plate COMMENTS Immunoassays are simple to perform Highly trained operators not needed Methods under development for dioxin 2 3 7 8 TCDD pesticides PCBs benzene phenol etc Studies to compare method to other methods will be performed PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Joseph Paladino Product Manager AFFILIATION Westinghouse Bio Analytic Systems Company TELEPHONE 4 12 722 5602 PREPARED May 19 1987 BIBLIOGRAPHY Technical Product Description Corporate Literature personal conversation 63 METHOD FM D5 USE OF FIBER OPTIC SENSORS IN ENVIRONMENTAL MONITORING METHOD UNDER DEVELOPMENT SUMMARY n situ monitoring technique for various contaminants to ug l concentrations in ground water air amp soil Few fully developed applications but appears to offer signifi cant advantages over conventional sampling techniques METHOD DESCRIPTION Optical fibers are used either as a light tube in remote fiber spectroscopy mode RFS or as a sensor in fiber optical chemical sensing mode RFS provides light transmission over l
78. f GC MS results which is considered acceptable for screening 52 USE LOCATION USED Southern Maryland Wood Treating Plant Summer 1986 EPA SITE NUMBER CERCLIS MDD980704852 MATRIX Soil and water PREPARATION MAINTENANCE AND CLEANUP UV Fluorescence cells should be cleaned occasionally ANALYSIS TIME 20 30 samples day CAPITAL COST 16 300 00 CALIBRATION Standards were made of seven commonly occurring PNAs Calibration curve was from 0 01 g l to 0 1 g l and 0 1 g l to 1 0 g l with four points for each curve COMMENTS Can be operated by trained technician PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT Stacie Popp AFFILIATION Roy F Weston Inc TELEPHONE 215 692 3030 PREPARED April 10 1987 BIBLIOGRAPHY Motwani J N Popp S A Johnson G M and Mindock R A Field Screening Techniques Developed Under the Superfund Program Management of Uncontrolled Hazardous Waste Sites Washington D C December 1 3 1986 53 METHOD FM DI TRACE ATMOSPHERIC GAS ANALYZER TAGA METHOD UNDER DEVELOPMENT SUMMARY Quick characterization and monitoring of many organic compounds using MS MS Capable of analyzing direct air samples for most organics at the ppb level and performing rapid GS MS MS analyses of soils Capable of real time screening of ambient air for target compounds l 2 order of magnitude accuracy but the quantitative data reduction increase of accuracy to include the calculation of error b
79. floppy disk drive and at least one hard drive The floppy disk drive on the hard disk system is used to copy all programs and data files to the hard drive usually C it is not used to run the system once all programs and data files have been copied to the hard drive It is assumed that the computer used has already been turned on and loaded with MS DOS version 2 0 or higher Consult your computer s operating manual for these procedures Some users will have to change the CONFIG SYS file to properly run the compiled dBASE Ill code The CONFIG SYS file should have the following two lines BUFFERS 25 FILES 20 To list the file enter C gt TYPE CONFIG SYS If the two values are equal to or larger than listed above then no changes are needed If the values are less than those listed above or if the lines are missing the file will have to be edited Please consult your MS DOS manual for instructlons on editing this file 2 1 INSTALLATION ON A TWO DISK DRIVE COMPUTER SYSTEM Users with a dual floppy disk drive system may use FSMC The following procedures should be followed the first time the system is used so that the FSMC will recognize which disk drives will be used The user should make a copy of the two system diskettes and return the originals to the manual for any future installations 1 Insert FSMC disk A into drive A and disk B into drive B 2 Ifthe A drive is not the current drive enter B gt A RETURN ENTER
80. he instrument separates the elements wavelengths into a spectrum Concentration of elements present is directly proportional to energies being produced Technique used to screen soil and water samples Soil sample preparation includes drying sample and grinding to a fine powder Aqueous sample preparation includes concentrating the metallic cations by filtering through strong acid ion exchange paper Sample pH must be below 2 to ensure that metal lons are in cationic form When anionic forms such as arsenate etc are present base ion exchange is required Region VIII method uses portable XRF analyzer which offers less sensitivity and detects fewer metals than this method APPLICATION Rapid screening in laboratory for chromium barium cobalt silver ar senic antimony selenium thallium mercury tin cadium lead copper nickel zinc manganese iron and vanadium LIMITATIONS Does not have sensitivity or precision of atomic absorption or other con ventional methods Lithium beryllium aluminum and boron not detected using this method INSTRUMENTATION USED Kevex 7000 X Ray Fluorescence Spectrometer PERFORMANCE SPECIFICATION DETECTION LIMIT Is element specific For critical elements such as lead it is 20 mg kg in soil and 600 ug in water For 18 elements tested the range was from 20 to 50 mg kg in soil and 100 to 600 ug l in water SELECTIVITY Elements may be identified by looking at various emission x rays e K alpha
81. ibrated for each target compound at least twice daily In addition for many target compounds e g tetrachloroethyiene chlorinated aromatics and oxygenated solvents the calibrations should be periodically checked throughout the day COMMENTS Requires high level of expertise and experience on the part of the analyst Calibration is simple and method is relatively fast cost effective and applicable to many compounds Calibration accuracy depends on accuracy of literature value of vapor pressure vs temperature and on setting of flow rates Use of ambient air as reagent gas means that as air changes calibrations change PROTOCOL AVAILABLE Available upon request for TCDD Air protocols currently under revision to incorporate ERT developed software and ERT NYDEC developed QA QC procedures Onsite consultation available from ERT SOURCE TECHNCIAL CONTACT Tom Pritchett Dr S H MO AFFILIATION EPA ERT NYDEC TELEPHONE 201 321 6738 518 457 7454 PREPARED April 29 1987 BIBLIOGRAPHY Engels J W Kerfoot H B and Arnold D F Survey of Mobile Laboratory Capabillities and Configurations EPA 600 X 84 170 U S Environmental Protection Agency July 1984 56 Ben Hur D Smith J S and Urban M J Application of Mobile MS MS to Hazardous Waste Site Investigation 5th National Conference on Management of Uncontrolled Hazardous Waste Sites November 7 9 1984 Becker D L Carter M L Equipment Available for Sample Screening an
82. ikes of 13 compounds recovery 26 200 PRECISION REPEATABILITY Relative Standard Deviation RSD of 13 compounds in water in triplicate RSD 1 5 34 2 13 compounds in soil in triplicate RSD 7 6 54 9 COMMENTS Recoveries are given before and after acidification USE LOCATION USED Beaver Creek Oregon 1985 EPA SITE NUMBER CERCLIS ORD095016887 MATRIX Soil and Water PREPARATION MAINTENANCE AND CLEANUP Column should be at thermal equilib rium before running Column and detector require occasional cleaning and reconditioning 44 ANALYSIS TIME 30 45 min sample CAPITAL COST AID 511 with ECD 7 245 00 Shimadzu Mini 2E with ECD 4 520 00 CALIBRATION Calibration determined by peak retention times and areas of PCB stan dards Standards and method blank should be run every tenth sample COMMENTS Used fairly regularly in Region X PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Hunt Chapman AFFILIATION Ecology and Environment Inc TELEPHONE 703 522 6065 PREPARED April 15 1987 BIBLIOGRAPHY Chapman M and Clay P Field Investigation Team FIT Screening Methods and Mobile Laboratories Complementary to Contract Laboratory Program CLP TDD HQ 8507 01 October 17 1986 Draft 45 METHOD FM 23 PESTICIDE ANALYSIS USING ISOTHERMAL GC WITH ECD HEXANE EXTRACTION SUMMARY Rapid determination of pesticides to 5 ug l in water and 500 ug kg in soil Requires field lab Many other co
83. information such as types of contaminants the user can identify field analytical screening meth ods that have been developed and applied at other similar sites and therefore may be of use for site characterization and other screening analytical requirements 1 3 SYSTEM UPDATES Documentation and system revisions will be made to the pocket guide user docu mentation and computer retrieval system The documentation updates will focus on the user documentation and the method descriptions to ensure accuracy and com pleteness of available methods and additions of new methods on a periodic basis 1 4 TECHNICAL CONSIDERATIONS The appropriate type of sampling and analysis at a given site depends on numerous factors the foremost of which are the intended end use of the data and associated data quality requirements Data quality as stated in the Data Quality Objectives for Remedial Response Activities EPA 1987 OSWER Directive 9355 0 7A is defined by the level of analytical support appropriate to various data uses As such five levels of analytical support Levels l V are defined below and are appropriate to a number of overlapping data uses as shown on Tables 2 1 and 2 2 LEVEL I Field Screening or analyses using portable instruments Results are often not compound specific and not quantitative but results are available in real time It is typically the least costly of the analytical options LEVEL l Field analyses using more soph
84. ing a Gas Chromatograph in an On Site Laboratory Hexane Methano VVaterExtractlon PC6 Analysis Using a Gas Chromatograph In an On Site Laboratory Hexane Extraction lt lt t tt t t eee PCS Analysis Using a Gas Chmatograph in an On Site Laboratory Hexanel Methanol PCB Analysis Using a Gas Chromatograph in an On Site Laboratory Hexane Acetone Extraction s 0 00 Pesticide Analysis Using a GC with ECD Hexane Methanol Extraction 52000 m Pesticide Analysis Using Isothermal GC with ECD Hexane Extraction r r aran iz s i s tl Phenol Determination by Liquid Liquid Extraction and GC Analysis PAH Analysis Using GC with Heated Column Total PNA Analysis Using an Ultraviolet Fluorescence Spectrophotometer ee vil 37 39 41 43 45 47 49 51 METHODS UNDER DEVELOPMENT FM D1 Trace Atmospheric Gas Analyzer TAGA 53 FM D2 Use of Bonded Sorbents for Pesticide Analysis 57 FM D3 Use of Bonded Sorbents for Semi Volatlle Analysis 59 FM D4 Immunoassays for Trace Organic Analysis 61 FM D5 Use of Fiber Optic Sensors in Environmental Monitoring 63 Viii ACKNOWLEDGMENTS This document was developed for the Office of Emergency and Remedial Response OSWER Hazardous Site Evaluation Division with assistance from the following individuals Carla Dempsey U S EPA Hazardous Site Evaluation
85. inssv ioj paiedeid 0 L906 IIN aseud 30114 WHNY SpoyjeW Jusweinsesy p sn q u yunoy uo ezea s j5ueuioji q pue UOT eULIOJUI 3yeiq a0In0g e 9 E 678 ew bn 10 8 VV 44Y13 0 9 8 eu bn 9 0 dav 0G M32 pest WN 1619 qdd gt TAUTA WN L E qdd pg VN Ty qdd ce u uq3 ojoTuOr4rL MN IT S wdd got u nTor VN TZ u 5n ep VN TT ul 5n g L SW 25 XVNAL CN T S qdd 6 WN qdd er 29 aV4L 1 auazueg SNI s aS CW SNOINHOGL 2 GOHLAN SHIX TVNV SGOHLAM 5 410 NVHL SCOHLAW SAN GINHOAL TVOILXTVNV III THAT pUIWV WLWO GNW NOISIOWYd TWOIMOLSIH 01 8 Faw 19 saqXTeue TenPTATPUT UO 103 p aTnsuo aq pTnous qu umoop stu 9961 9 29 3u m Bbeuey soueinssy AaTTen 103 p ied id 60 806 114 eseud 30T14d WHOM spouqsW 3U m inse n p sn ATauTJNoY uo eed pue UOT eEWIOJUI wNTpuseduOD zeia aDINOS e GS TT 5y bu 02 0 z by bu s bpnTs PTTOS 8 0 L E by bu SL re OT 6y 5u oe 3S M PTTOS 02 22 Boy bur g z a21 0T T E or 23SeM TIO 0109 pee SVIS asa HONVM WNIGaW ANOINHDSL AOWHNDOW NOISIO4Hud GOHLAN ALAIVNV 54 1 SVU 412 NVHL MSHLO SGOHISW SHNOINHOSL TVOLLATVNV III 78 41 A
86. isticated field portable analyti cal instruments In some cases the instruments can be set up in a mobile laboratory on site There is a wide range in the quality of data that can be generated from qualitative to quantitative LEVEL III Laboratory analysis using methods other than the CLP RAS This level is used primarily in support of engineering studies using stan dard EPA approved procedures Some procedures may be equivalent to CLP RAS but without the CLP requirements for documentation LEVEL IV CLP Routine Analytical Services RAS This level is characterized by rigorous QA QC protocols and documentation and pro vides qualitative and quantitative analytical data Some Regions have obtained similar support via their own regional laboratories university laboratories or other commercial laboratories LEVEL V Non standard methods Analyses which may require method modification and or development CLP Special Analytical Services SAS are considered Level V Whereas the quality of data generally increases from Level through Level V as shown above this can only be stated in a general way and in certain instances and with the appropriate QA QC procedures the quality of Level II and III data can parallel that achieved by Level IV and V data Consider for example a Level II analysis for volatile organics using a GC in a field laboratory in this situation the quality of the data may be higher than that achieved i
87. l 10AIO equipped with PID and 4 foot SE 30 column AID 511 equipped with FID or ECD and 3 foot SE 30 column Shimadzu GC Mini 2 and GC Mini 3 with FID and 6 foot SP 1000 and AT 1000 column HNU Model GC 301 with PID or FID and Standard SE column PERFORMANCE SPECIFICATION DETECTION LIMIT 1 ug l for aromatics 40 ug l for some chlorinated hydrocarbons SELECTIVITY Peaks are separate good selectivity ACCURACY 27 32 RPD Standard Deviation 70 TCE and PCE samples PRECISION REPEATABILITY Duplicate samples show very good agreement COMMENTS Results given for Photovac the most common GC used Others give simi liar results USE LOCATION USED Norwalk Harbor Conn Winter 1981 EPA SITE NUMBER CERCLIS Non CERCLA MATRIX Air and headspace above soil sediment and water PREPARATION MAINTENANCE AND CLEANUP Optional backflush valve allows for flushing of contaminants from column Column conditioning done every third month by heating to 100 and flushing with helium ANALYSIS TIME 10 20 minutes CAPITAL COSTS Photovac 14 000 00 AID 511 5 020 00 Shimadzu 4 100 00 5 200 00 HNU 301 6 350 00 CALIBRATION Standard necessary to identify and quantify compounds detected by GC Standard is a known quantity of organic vapor in equilibrium with air or an aqueous or organic solution Standards run before screening field samples and after every 5 samples COMMENTS The interpretation of results requires a trained chemist Th
88. mpounds detected with pesticides on GC METHOD DESCRIPTION Requires field laboratory with GC and linearized ECD for pesti cide analysis in soil and water Identification and quantitation is determined by compar ing peak retention times and peak areas of the standard and sample Sample preparation for water consists of mixing 15 ml of water with 1 5 ml hexane and separat ing hexane layer Sample preparation for soil consists of mixing 2 grams soil with 2 grams sodium sulfate To this 10 ml hexane is added mixed with an ultrasonic probe and hexane layer separated The hexane layer is ready for analysis APPLICATION Simple and rapid determination of pesticides Also detects PCBs LIMITATIONS Results are semi quantitative Has not been used in the field Detects phosphorus nitrogen sulfur and oxygen compounds along with pesticides INTRUMENTATION USED Hewlett Packard Model 5880 with ECD PERFORMANCE SPECIFICATION DETECTION LIMIT 5 ug l in water and 500 ug kg in soil SELECTIVITY Compounds give separate peaks many compounds detected usually good selectivity ACCURACY Not available PRECISION REPEATABILITY Not available COMMENTS This method was developed by Region IV to provide tentative identification of compounds and semiquantitative data Until recently not used as a quantitative method USE LOCATION USED Field Mobile Laboratory in Florida EPA SITE NUMBER CERCLIS Not Applicable MATRIX Soil and water PREPARAT
89. ms of physical configuration size weight power requirements and the level of accuracy and precision achievable Based on the mobility of the equipment three terms are typically used to describe the mobility of the equipment Portable Requires no external power requirements hand held devices which can be easily carried by one person Typically includes photoionization detec tion PID and flame ionization detection FID to measure the total amount of ionizable materials mostly volatile organic compounds Also includes suitcase sized gas chromatographs GC with assorted detectors and capabilities and X Ray fluorescence devices Fieldable Particularly rugged limited external power required Easily transported in a van pick up or four wheel drive Mobile Small enough to carry in a mobile lab Includes most analytical instru ments Power considerations may limit the use of many instruments in mobile laboratories As outlined in this brief discussion of Level and II analytical methods numerous factors must be considered when determining which method should be implemented at a site Data quality objective for the sampling event in question and the ultimate end use of the data developed should also be considered 13 2 0 INSTALLING THE SYSTEM The first time the FSMC system is run an installation menu will appear and request information about your computer This system will run on a computer with two floppy disk drives or one
90. n an offsite laboratory Level III IV or V due to sample handling considerations Similarly Level II and III analyses can at times provide lower detection limits than those required by Level IV require ments and as such the quality of data is higher based on the data quality objectives It is important to note that in most situations the exact quality of an analysis cannot be specified or determined prior to the analysis and as such sufficient QA QC steps have to be taken e g documentation of blank injections calibration standard runs runs of qualitative standards between samples and analysis of duplicates and spikes to be able to assess the quality achieved As such one of the major benefits of Level IV analysis is that it provides sufficient documentation to allow qualified personnel to review and evaluate data quality In other words while the quality of Level IV data may not be higher as defined by the precision and accuracy than those achieved by other levels of analysis it does provide data of known quality 21310349 0 13 SNOYADSIY All1VnO NMWONN 40 1 SI 1VOS SNOYODIY 5531 d 19 OL YVIIWIS SAONVY NI 0314 ATIVOIdA L VLVG 031014 3 54315 0 NO IN40N4d40 NOILVNINVLNOD 40 NOILVOIGNI 3AOHd NYO 1 031344431 VLVd ON qalvugl1vO SLNANNYLSNI al Viva AWIL
91. n of soil water air and waste locations which have a high likelihood of showing contamination through subsequent analysis Real time data to be used for health and safety considerations during site investigations Qualitative data relative to a primary calibration standard if the contami nants being measured are unknown Quantitative data if a contaminant is known and the instrument is call brated to that substance and Presence or absence of contamination Level Il analytical support is designed to provide real time data for ongoing field activities or when initial data will provide the basis for seeking laboratory analytical support As such Level Il analytical methods can be effectively utilized when a phased approach Is used for field sampling There have also been a significant number of instances where data derived from Level II support have been used to make decisions about site dispositlon Field analysis using Level II analytical options can provide data from the analysis of air water soil and waste materials for many Target Compound List TCL organic compounds including volatiles base neutral acid BNA extractable organics and pesticides PCBs Inorganic analysis can also be conducted using field atomic ad sorption AA and other instruments Level Il analyses are used for on site real time baseline data development extent of contamination and remedial activities and generally provide rapidly available data for a va
92. nd associated data quality requirements the data obtained through field analysis screening be confirmed by CLP analysis 1 5 OVERVIEW OF LEVELS AND II ANALYSES Level and Il analyses are defined as field screening analytical methods which utillze equipment amenable to the rigors of field conditions and are located at or near the sampling site Level analytical support Is typically defined as field screening with the objective of generating data which will generally be used for example during Phase 1 Investiga tions In refining sampling plans and determining the extent of contamination A second objective of Level analyses is to conserve other analytical support resources Level analyses are generally effective for total vapor readings using portable pho toionization or flame lonization detectors PID or FID which respond to a variety of organic and Inorganic volatile compounds Detection is typically limited to volatile compounds These types of analyses provide data for on site real time total vapor measurements evaluation of existing conditions sample location optimization extent of contamination and health and safety evaluations Data generated from Level analyses are considered qualitative in nature although semi quantitative and or quantitative data can be generated for example by using the GC option of a FID with sufficient calibration Data generated from Level analyses provide the following Identificatio
93. ne solu tion is injected Into GC for analysis Identification and quantitation by comparison of retention time and peak height and volume to standard response factor determination required Method is a modification of EPA method 604 APPLICATION Determination of phenol concentrations in soil and water 2 4 dimethyl phenol phenol 2 chlorophenol 2 nitrophenol 2 4 dichlorophenol 4 chloro 3 methylphenol 2 4 6 trichlorophenol and pentachlorophenol LIMITATIONS Liquid Liquid extraction procedure is a difficult process and can best be performed by a trained chemist INSTRUMENTATION USED Shimadzu GC Mini 2 Gas Chromatograph with ECD and Shimadzu Chromatopac C RSA Data Processor PERFORMANCE SPECIFICATION DETECTION LIMITS Detection limit for pentachlorophenol in water 100 ug l and in soil 25 ug kg SELECTIVITY Separate peaks easily identifiable Other compounds may appear on chromatograph ACCURACY Spike recoveries In soil 6 replicates of 8 compounds 102 127 Spike recoveries in water 6 replicates of 8 compounds 1 096 8896 PRECISION REPEATABLLITY Relative Standard Deviation RSD for 6 replicates of 8 compounds in soil 15 3 44 4 RSD for 6 replicates of 8 compounds in water 19 6 to 56 2 COMMENTS Recoveries for water samples were acceptable for pentachlorophenol 88 CLP limits 9 103 and phenol 25 8 CLP limits 12 89 USE LOCATION USED Not Available EPA SITE NUMBER CERCLIS Not Appli
94. ng portable GC or field laboratory METHOD DESCRIPTION A Teflon collection hose with attached collection chamber low ered into a borehole and a sample is withdrawn by pumping for analysis Gas tight syringe is used to take sample from a septum fitting on the pump Grab or composite samples can be taken APPLICATIONS Used to determine vertical contamination gradient identify hot spots predict emission rates and assess migration pathways as determined by soil type and stratigraphy LIMITATIONS Uncontrolled variables include soil temperature influenced by heat gener ated by the auger and surface area of the soils INSTRUMENTATION USED Custom fabricated downhole Isolation flux chamber Teflon line gas tight syringe PERFORMANCE SPECIFICATION DETECTION LIMITS Function of injection volume and detector sensitivity 0 2 ug l for TCE in one study SELECTIVITY Volatile organics ACCURACY Not Known PRECISION REPEATABILITY Not Known COMMENTS Sensitivity depends on GC used Clay layers and horizons with lt 5 air filled porosity reduce effectiveness of soil gas sampling Precision and ground water cor relation must be demonstrated at each site Compare with other sampling methods to determine applicability to the site USE LOCATION USED Not Available EPA SITE NUMBER CERCLIS Not Available MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Equipment decontamination required purge syringes with nitrogen gas and
95. nter ing a Y after each matrix name Enter the detection limit to constrain the search to only those methods capable of analyzing below or equal to this limit for each matrix selected Enter 0 0 if no limit is desired The default units of measure may be changed Valid units of measure for the detection limit are PPM parts per million and PPB parts per billion The system will respond by informing the user how many methods were found in this search If there was at least one a display print menu will display the options of viewing the method descriptions FIELD SCREENING METHODS CATALOG 5 USER RETRIEVAL SYSTEM wee SEARCH OPTIONS menee 11 CLASS OF CHEMICALS 2 COMPOUND CHENICAL NAME 131 CAS NUMBER 4 METHOD NAME OR NUMBER 81 EXIT S UTILITIES INSTALL REINDEX SELECT OPTION 8 5 J Tuesday October 27 1987 Figure 3 1 18 3 1 1 SEARCHING BY CHEMICAL NAME The user may enter a specific chemical name If the full name is not available enter what you know is correct The search is designed to look for an embedded character string within a chemical or method name The system will match on what the user has entered if that character string is found anywhere in the name display what was found and then permit the user to select the one desired See Figure 3 2 EE A TE EE E GSR ert SEARCH FOR A CHEMICAL NAME ENTER CHEMICAL NAME BLANKS TO EXIT NOTE THE RECORD s FOR NAME CONFIRMATIO
96. of mixing 0 8 gram of soil with with a 1 4 5 ratio of distilled water methanol hexane An optional step Is to dry and grind sample before extraction Agitate sample and let sit allowing hexane layer to separate Transfer hexane layer to a test tube containing sul furic acid and mix This step is optional as it is used to eliminate matrix interferences Withdraw sample from hexane layer for GC analysis APPLICATION Simple and rapid determination of polychlorinated biphenyls Method most appropriate for Aroclors 1242 1248 1254 and 1260 but good for 1016 1221 and 1232 LIMITATIONS Above 100 000 ug kg concentrations are underestimated by 60 Results are approximations INSTRUMENTATION USED Analytical instrument Development Corp AID Model 511 06 GC equipped with ECD and a 4 foot SE 30 stainless column PERFORMANCE SPECIFICATION DETECTION LIMIT 200 ug kg SELECTIVITY Compounds give characteristic multiple peaks good selectivity ACCURACY Recovery of Aroclor 1242 spike 80 105 Based on results of 300 samples accuracy Is equivalent to CLP below 100 000 ug kg determination above 100 000 ug kg are biased low about 40 of the CLP determined value PRECISION REPEATIBILITY Relative Standard Deviation RSD of 4 samples 10 12 COMMENTS USE LOCATION USED Extensively used sites include Washburn ME Norwood MA EPA SITE NUMBER CERCLIS Not Available MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Care sho
97. of control of sampling environment INSTRUMENTATION USED Auger for drilling and 500 ml gas tight side port syringe for sampling GC for analysis PERFORMANCE SPECIFICATION DETECTION LIMIT Heat generated by drilling raises sampled concentration of contami nants however fewer DIA samples found contaminant possibly indicating less sensitivity than other soil sampling methods 0 2 ug l for TCE in one study based on capability of GC used for analysis SELECTIVITY Volatile organics depends on GC method used ACCURACY Results correlated well with results from other sampling methods at same locations Correlation coefficients were 0 68 for one liter method 0 72 headspace method 0 78 direct injection stopper 0 80 Tenax PRECISION REPEATABILITY Not Known COMMENTS May not accurately reflect ground vvater conditions due to quick nature of sampling GC used will affect detection limits Clay layers and horizons with lt 5 air filled porosity reduce effectiveness of soil gas sampling Compare method to other sam pling techniques to determine its applicability to a particular site USE LOCATION USED Puget Sound WA 1986 EPA SITE NUMBER CERCLIS Not Available MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Determine appropriate drilling depth by use of test holes need to drill below surface soils to bypass competing adsorption sinks or by combined experience and assessment of site factors Decontamination of auger an
98. of the standard and sample Sample preparation for water consists of adding 1 5 ml hexane to 15 ml of water mixing and separating hexane layer Sample prepara tion for soil consists of mixing 2 grams of soil with 2 grams sodium sulfate Then 10 ml of hexane is added to sample mixed with an ultrasonic probe and hexane layer sepa rated The hexane layer is ready for GC analysis APPLICATION Simple and rapid determinations of polychlorinated biphenyls PCBs Also determines pesticides Testing based on Aroclor 1260 LIMITATIONS Results are semi quantitative Has not been used in the field INSTRUMENTATION USED Hewlett Packard 5880 with ECD PERFORMANCE SPECIFICATION DETECTION LIMITS 25 ug l in water and 2 500 ug kg in soil SELECTIVITY Compounds give characteristic multiple peaks good selectivity ACCURACY Not available PRECISION REPEATABILITY Not available COMMENTS This method was developed by Region IV to provide semiquantitative data Until recently not used as a quantitative method USE LOCATION USED Field Mobile Laboratory in Florida EPA SITE NUMBER CERCLIS N A MATRIX Soil and Water PREPARATION MAINTENANCE AND CLEANUP Precautions should be taken not to 77 column Occasional cleaning and reconditioning of column and detector ANALYSIS TIME 20 25 min sample CAPITAL COST 20 000 00 38 CALIBRATION Calibration determined by peak area and retention time of PCB standard COMMENTS A much less expensi
99. ol dor 1OdeA Dro dol 4 1 d l do1 421 4 1 4 1 41 INHOGL 51108 AXOVUDDOV GNV NO S OSUd TWOIMOLSIH 8 TIWL Surz UTL KE AirO1a s uv5uey umtseubey peay uoir a ddoo unruoruo WNTITeD umTupeo umu TUN TW 48 LEI SALA TYNW SGOHISW 54 412 SENOINHOGL TVOLLATVNV AI TSAR 16 TQETTEAV ON VN P suoT eoTZ Sads qu umiqsur uoTsTo id pue A3TAT31SU S o ST A T u3oq 3e p sn aq Aen s3u um3suT T 1 A S uorqaeqau umiqsur pue s nbtuu II T A T pue I T A T M2 Q 03 YINOJIP St 31 q s u umagzsu s vq3 JO qu u siaopu ue 3n3T3suo JOU s op sT pou 6 Jo uorqu Ww Git ss run sTenucu Si inaoeynuey oinos e uorqezr u zu g uoro3oud 29 p WN wdd 10070 MN 2 1 f l ULYJ N UOT3EZTUOI uleT4 p YN sueyjew wdd 1 0 wdd 0002 170 OTL qIV soTuebio u zu g UOT3EZTUOTO201u4 Te S TTNJ 431 u zu g wdd ro wdd 0002 170 TOT Id TNH sotuebio ucu3 y UOT3EZTUOI WETA p WN aueujen wdd 170 wdd 0001 10 821 Ainquag soTueb o NOISIOMHMa XAL ALLISN4S FONT SNOINHOAL SULA TYNY ANAHTMISNI LNAWMLLSNI ANANTDDILSNI ANZNDMLSNI ADWUNDIW GNV 910 TVOTMOLS H 8 8 419 1 qo INO INOHAL ONIN4GGMOS 1414 I TART 17 qJuawasiopua
100. oundwater EPA Project I D CR811018010 October 10 1984 29 METHOD FM 15 SOIL GAS SAMPLING USING TENAX TUBES SUMMARY Sampling long term and time averaged of soil gas for on site analysis to determine volatile organic contaminant plume Requires use of sampling probe and pre conditioning of Tenax tubes Analysis can be performed in a field laboratory or offsite laboratory METHOD DESCRIPTION Stainless steel desorption tubes packed with Tenax are suspended inside a stoppered sampling probe and connected to a pump Three liters of soil gas are drawn through each tube concentrating the contaminant on the adsorbing material In a field laboratory contaminants are driven off thermally and analyzed using a GC APPLICATION Soil sampling to aid in contaminant plume delineation especially where very low concentrations expected LIMITATIONS Sampling probe installation necessary Tenax tubes must be precondi tioned Sampling requires lengthy pumping Pre packed Tenax tubes often contaminated recommend packing own tubes but requires laboratory and chemist INSTRUMENTATION USED Tenax filled desorption tubes calibrated air pump thermal desorber gas tight syringe PERFORMANCE SPECIFICATION DETECTION LIMIT Sensitivity improved over other sampling techniques by sample con centration calculated 0 02 ug l for TCE 10x below detection limit of GC used SELECTIVITY Volatile organic contaminants depends on GC method used for analy
101. pends on GC used concentrating techniques overcome some field GC limitations Clay layers and horizons with lt 5 air filled porosity reduce effec tiveness of soil gas sampling Method should be tested at each site by comparing to results of other sampling techniques USE LOCATION USED Puget Sound WA 1986 EPA SITE NUMBER CERCLIS Not Available MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Syringes and tubing must be cleaned e g using vacuum heated syringe cleaner following sample injection nitrogen gas flushing Decontamination of auger amp syringes required for reuse 24 ANALYSIS TIME Drilling borehole 15 30 min sample collection 1 min GC analysis 30 minutes CAPITAL COSTS Syringe 30 40 pump lOO 500 Both are reusable GC 4 100 20 000 CALIBRATION N A COMMENTS Simple sample collection May perform better than Direct Injection Auger sampling when most appropriate analytical equipment used Allows adjustment of sam pling area for further investigation based on immediate results PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT John Ryding AFFILIATION C C Johnson amp Malhotra TELEPHONE 303 433 6966 PREPARED May 6 1987 BIBLIOGRAPHY Jowise P P Villnow J D Gorelik L I Ryding J M Comparative Analysis of Soil Gas Sampling Techniques Management of Uncontrolled Hazardous Waste Sites Washington D C December 1 3 1986 p 193 199 25 METHOD FM 13 S
102. r ail samples Two distinct developments within EPA address this concern first the increasing use of field screening analytical methods and second the issuance of the Data Quality Objectives for Remedial Response Activities EPA 1987 OSWER Directive 9355 0 7A The development of field analytical methods was initiated early in the hazardous waste program history The FITs developed and used field analytical techniques first for health and safety related air monitoring and subsequently for sample screening and analyses of increasing complexity This use of field methods was frequently performed in conjunction with EPA laboratories and the Environmental Response Teams ERTs As such initial use of Instruments such as the Foxboro Organic Vapor Analyzer OVA and the HNu Systems HNu 101 were limited to air monitoring to determine levels of safety protection This initial use of field instrumentation made the FITS and ERTs familiar with the capability of these and other instruments and paved the way for their use as analytical tools in the Superfund Program The second development while discussed for many years was initiated and codified in 1986 with the issuance of a number of EPA sponsored documents the foremost of which were the Data Quality Objectives for Remedial Response Activities EPA 1987 OSWER Directive 9355 0 7A and A Compendium of Superfund Field Operations Methods EPA 1987a OSWER Directive 9355 0 14 Data Quality Objectiv
103. remain constant INSTRUMENTATION USED Century Systems Foxboro Organic Vapor Analyzer Model 128 PERFORMANCE SPECIFICATION DETECTION LIMIT 500 ug l for most volatile organics SELECTIVITY Early peaks tend to overlap Later peaks easily identifiable ACCURACY Calibration error for benzene ranged from 25 of value at detection limit 0 74 mg kg to 14 at higher concentrations 165 mg kg PRECISION REPEATABILITY Coefficient of variance l 4 for five standard samples of benzene and carbon tetrachloride Duplicate samples show good agreement COMMENT Performance specifications are for air results for soil sediment semi quantitative USE LOCATION USED Ottadi amp Gross Kingston Steel Drum Kingston NY 1980 EPA SITE NUMBER CERCLIS NHD990717647 MATRIX Air Headspace above soil sediment and water 14 PREPARATION MAINTENANCE AND CLEANUP Columns must be cleaned every 3 months Recharge batteries after use ANALYSIS TIME 20 samples per hour CAPITAL COSTS 7 000 CALIBRATION Standards necessary to identify and quantify compounds detected by GC The standards are run before screening field samples COMMENTS The interpretation of results requires a trained chemist The column can easily be saturated by concentrated samples resulting in an inoperable unit Method Is routinely used in Region 1 PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Dr Thomas Spittler AFFILIATION U S EPA Region Labor
104. rformance data are available for recovery as a function of solvent column flow rate and type of water USE LOCATION USE Not Available EPA SITE NUMBER CERCLIS Not Applicable MATRIX Water PREPARATION MAINTENANCE AND CLEANUP Columns are disposable Columns are conditioned prior to use with methanol followed by water or buffer After the sample has been added interferences are washed off the column with distilled water and the sample eluted by a solvent ANALYSIS TIME Sample preparation 10 15 min analysis 20 30 minutes CAPITAL COST 4 000 00 20 000 00 for GC CALIBRATION Standards were made of high purity solvents with various concentrations of seven pesticides This is used to spike water samples The spikes were used for identification and quantitation 58 COMMENTS Interpretation of results requires a trained chemist Columns must not be allowed to dry out prior to adding sample PROTOCOL AVAILABLE No SOURCE TECHNICAL CONTACT Patricia Gardner AFFILIATION Analytlchem International TELEPHONE 800 42 1 2825 PREPARED April 22 1987 BIBLIOGRAPHY Andrews J S and Good T J Trace Enrichment of Pesticides Using Bonded Phase Sorbents American Laboratory April 1982 59 METHOD FM D3 USE OF BONDED SORBENTS FOR SEMI VOLATILE ANALYSIS METHOD UNDER DEVELOPMENT SUMMARY Method is faster than traditional liquid liquid extraction Determines most PAHs and phenols in water to 20 ug l Poor
105. riety of activities including hydrological investigations establish depth concentration profiles extent of contaminant determination including special activi ties such as vadose zone sampling cleanup operations determine extent of con taminated soil excavation and health and safety considerations Typically a gas chromatograph and more sophisticated instruments operated in the field provide the bulk of the analytical support at this level The ability to assess the data quality accuracy and precision is dependent upon the QA QC steps taken in the process including documentation of blank injections calibration standard runs and runs of standards between samples The level of precision and accuracy that can be achieved by a specific Level or II analysis varies as a function of numerous factors including the matrix and contami nant being sampled and perhaps most importantly the skill of the analyst doing the work As summarized in the Data Quality Objectives for Remedial Response Activities EPA 1987 OSWER Directive 9355 0 7A because the procedures for Level Il are not formalized a great deal of improvisation usually takes place The inherent variability of the procedures themselves would make the development of a centralized quality assurance data base tenuous The same reasoning would apply to making uncertainty predictions based on a centralized data base On the other hand Level l analyses based in a mobile laborato
106. rocarbons halogenated hydrocarbons aromatics C5 and larger hydrocarbons and sulfur containing hydrocarbons Also capable of quanti tation but more analytical control and data reduction time needed For soil analyses capable of dilute and shoot GC MS MS analyses for any GC compatible compound present in mg kg concentrations e g PCBs and chlorinated pesticides and rapid cleanup and shoot GC MS MS analyzes for any compound present in ug kg concentra tions e g TCDD LIMITATIONS Lacks isomer specificity for air analyses Hydrocarbons and chlorinated solvents can yield ions of equal mass and similar structures resulting in cross interfer ences Dirty samples can yield spectra with fragments from more than one parent struc ture Not as stable as normal GC MS 2 to 3 fold drift in sensitivity over a day is possible The sampling system is not totally compatible with classical QA QC procedures direct sampling of audit cyclinders and replicate analyses but TAGA specific QA QC procedures are currently being developed and refined by the ERT and NYDEC Difference in ionization and the use of an initial mass filtering will result in MS MS spectra being different than the MS spectra contained in standard EPA NIH standard spectral libraries The use of the sample matrix as the chemical ionization reagent gas can result in poten tial matrix affects The current instrument software does not support QA QC criteria being applied to quan
107. rous other locations EPA SITE NUMBER CERCLIS Non CERCLA MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Solvent desorption required before GC analysis 20 ANALYSIS TIME Sample collection time varies depending on analytical sensitivity ex pected concentration of contaminant etc Sample processing involves solvent desorption 1 2 hour and GC analysis 15 30 min sample CAPITAL COST Not available CALIBRATION Check validity of method under site conditions COMMENTS One of several soil gas sampling methods that may be applicable under various circumstances Clay layers and horizons with 5 air filled porosity can reduce efficiency of soil gas sampling PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Henry 6 Kerfoot AFFILIATION Lockheed Engineering and Management Services Co Inc TELEPHONE 702 734 3217 PREPARED May 6 1987 BIBLIOGRAPHY Kerfoot H B amp Mayer CL The Use of Industrial Hygiene Samplers for Soil Gas Surveying Ground Water Monitoring Review Fall 1986 74 78 21 METHOD FM 11 SOIL GAS SAMPLING USING MINI BARREL SAMPLER SUMMARY Method to collect soil gas samples when low concentration expected Soil aliquots are directly removed and prepared Headspace gas is withdrawn and injected into GC Analysis can be performed using portable GC field and or off site laboratories METHOD DESCRIPTION A coring tool is used along with an auger or backhoe to collect the sample Samples
108. ry setting and using state of the art sophisticated instrumentation can allow mobile laboratory capabilities to approach the analytical range and performance accuracy sensitivity and precision achieved in off site analytical facilities Based on the undocumented data quality of most Level and II analyses data generated in the field are typically confirmed by submitting duplicate samples to the CLP Although no statistical methods are available to determine the exact number of samples to submit for confirmation numerous factors have to be considered includ ing Objective of sampling Le data quality objectives Data uses and Method of analysis used and the level of accuracy and precision achieved In general confirmation samples should include a subset or all of designated critical samples a subset of samples covering the entire range of identified con centrations and a subset of samples near the action level and near the 0 con centration or not detectable range An additional factor to consider is the measured precision of the field instrument in use When high precision is measured less samples need to be confirmed if how ever a low precision Is calculated It is recommended that based on the data quality objectives defined for the site the analysts be suspended until a qualified chemist determines the reason for the low precision The equipment utilized for Level and Il analyses can vary greatly in ter
109. s added to soil samples and is used as an absorbent for water extract samples to clean up the sample Acetonitrile is used for soil extraction and hexane for water extraction Quantitation is done by a seven point calibration curve APPLICATION Simple and rapid determination of total PNAs LIMITATIONS Does not identify individual PNA compounds Must be validated for each site due to potential matrix interferences INSTRUMENTATION USED Perkin Elmer Model LS 5 Fluorescence spectrometer with chart recorder PERFORMANCE SPECIFICATION DETECTION LIMIT 10 0 ug l in water 1 000 ug kg in soil SELECTIVITY Dependent upon matrix interference Where used only PNAs were detected ACCURACY Spike recoveries for napthalene acenapthene for soil 10 samples and water 6 samples were 63 100 and 81 101 respectively Spike recoveries for phenanthrene for soil 10 samples and water 6 samples were 66 130 and 93 111 respectively PRECISION REPEATABILITY Relative Standard Deviation RSD for phenanthrene for water 6 samples and soil 10 samples were 0 6 11 and 0 6 13 respectively RSD for napthalene acenaphthene for water 6 samples and soil 10 samples were 1 2 10 and 096 2 7 respectively COMMENTS Specifications shown based on data from two sites Calibration curves ex trapolated to non linear response regions will give high concentrations gt 100 recover ies of spikes Results were within an order of magnitude o
110. sTYL 9861 Arenuer zzeIS JuoWebeueW oucinssv Arten waa 103 p red id 0 L80E IIN aseyd 20TTd WIN spou3 M 3u m inse y p sn ATauT JnNoy uo ezea pue uMTpuedmOD 3 eiq c oznog e T E 6T T 5n pez Maul 22 Ee 1 6 or Z 6EZ 6 T L 9 T 5n SOT VV IWW LT 6 S 1 6 21 T 6EZ S T 5bn Cp ddI TE 15n zy i U007X T 5n ei SW D9 S yc T 5n er 0928 2 2 68 T 5n 092 SW D9 gt tSn pre 729 1 T bn et SW 29 0T 6T T 5n sz 0728 TE T 5n 009 SW D9 ST 61 T bn er 29 u nTor 92 zs T 5n 89 SW D9 LT 8L T bn CC 29 u TAu3 v 9 17 4094 GONE SMOINHOAL NOISIDJYAd NOLLVMELN392NO O SGOHLAN SWU 410 NVHL 4 1 SCOHIGW SAD INHO L TVOLLATVNV III 3AZ1 p nuT3uoo MALMM VLVU AOVMDOOV ANV NOISIOGYd T G Sigi AseTT1deo suoq eoospAH Z 0 0 6721 E L 911 8L 978 MS Otem IweTONUATOE 0128 WN WN VN S TT36TOATN S SW DD 0909 uum TOD yy 6 0 GPT 02 TP S TT3ETOATN S 0928 6 9 91 82 6 LOT 56 978 MS soTue540 TT35TOA 0928 002 1 0 VN VN 9y8 MS p eurzoTuo 0ST8 0 S 170 6761 E S L 0ZT S 9S 978 MS s proT3s q snozoydsoydoueb10 OPT8 T 0 0 92 OT 66
111. se define general site conditions assist in well placement and screen Setting aid in the selection of sampling locations compare off and on site conditions estimate potential population exposures determine the completeness of cleanup actions such as excavations and establish long term monitoring Presently field screening analytical techniques are routinely being used throughout the Superfund program However because of the decentralized nature of the pro gram knowledge and skills gained in one region or state or even at one site are not necessarily transferred to others Many personnel responsible for developing overseeing site sampling efforts need to have timely and accurate information re garding the availability of appropriate analytical methods To meet this need and to facilitate transfer of information about methods for measuring and screening chemi cals in the field the United States Environmental Protection Agency has developed the Field Screening Methods Catalog FSMC To date thirty one methods have been compiled and documented in the Catalog Of the thirty one methods contained in this Catalog four are in the developmental stage Use of Bonded Sorbents for Pesticide Analysis Use of Bonded Sorbents for Semi Volatile Analysis immunoassays for Trace Organic Analysis and Use of Fiber Optic Sensors in Environmental Monitoring and one Trace Atmospheric Gas Analyzer TAGA cannot truly be considered a viable fiel
112. single step extraction extract dilution and flash chromatography dilute and shoot Water analyses consist of extraction and flash chromatography of the extract Air analyses typically consist of sampling the air directly from a 1 5 2 liter second sample stream ANALYSIS TIME Dioxin 15 20 minutes for non isomer specific analyses 30 45 minutes for TCDD complete screening of chemical classes in air 30 minutes complete set of air analyses for a set of target compounds 1 10 seconds depending on the number of compounds CAPITAL COSTS 500 000 for MS MS 800 000 in fully outfitted van CALIBRATION For GC MS MS analyses uses conventional GC calibration methods For air analyses two different calibration techniques are used 1 A motorized syringe drive expels headspace vapor from syringe containing solid or liquid Vapor from syringe is mixed with air at 2 liters minute in the temperature controlled 1OOoC mixing tee Relative concentration in the stream is calculated based on vapor pressure and flow rates Overall calibration accuracy is 30 2 Certified gas standard cylinders 25 50 ppm v can also be serially diluted directly into the sampled air stream to generate cali bration concentrations in the range of 5 100 ppb v This method has an overall calibra tion accuracy of 10 but is limited only for compounds which can be maintained at stable concentrations in gas cylinders For air analyses the instrument should be cal
113. sis ACCURACY High correlation with other sampling techniques direct injection auger 0 80 headspace sampler 0 84 one liter technique 0 90 direct in jection stopper 0 98 Also high correlation with concentrations in water 0 80 amp 0 99 In two sample groups Percent recovery is unknown PRECISION REPEATABILITY RSD 24 for 10 samples from a single location over a 4 week period For three sets of triplicate samples from different locations RSDs were 5 1096 and 44 varying inversely with concentration COMMENTS Variation in results is mainly due to the nature of soil gas sampling rather than the subsequent analysis unless contaminant concentrations are very low Correlation with ground water contaminant concentrations may be misleading Sensitivity depends on GC used concentrating method overcomes some limitations of field GC Clay horizons with lt 5 air filled porosity reduce effectiveness of soil gas sampling Should be com pared with other sampling techniques to determine its applicability at a particular site USE LOCATION USED Puget Sound WA 1986 EPA SITE NUMBER CERCLIS Not Available 30 MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Preconditioning and assembly of Tenax tubes necessary solvent extraction with methanol then hexane heating in N at mosphere Cleanup required for reuse ANALYSIS TIME Drilling borehole 15 30 minutes installing sampling probe 10 min utes sample collection
114. soil and sediment samples for concentrations of lead zinc copper arsenic iron and chro mium Sample preparation includes drying a 5 gram sample and grinding it to a fine powder The XRF analyzer must be programmed and calibrated before samples are screened APPLICATION Rapid on site screening for lead zinc copper arsenic iron and chromium LIMITATIONS Method does not have the sensitivity or precision of atomic absorption or other conventional methods Cadmium manganese barium and mercury may be de tected but only at high concentrations due to spectral overlap of other elements Sample matrix effect may cause significant accuracy problems and can never be elimi nated fully Matrix effects include non homogeneity surface conditions and spectral interferences INSTRUMENTATION USED XRF 840 analyzer electronic unit HEPS sample probe either Cm 244 or Am 241 radioisotope or both PERFORMANCE SPECIFICATION DETECTION LIMIT 15 mg kg for arsenic to 140 mg kg for iron but dependent on site specific matrix and calibration techniques SELECTIVITY Elements may be identified by looking at various emission X rays i e K alpha K beta ACCURACY Student s t test and Wilcoxin s test show agreement between XRF and CLP data at a 95 confidence level for As Cu Pb Zn and Fe Number of samples ranged from 26 45 PRECISION REPEATABILITY Coefficient of variation 20 at detection limit and 5 at higher values for
115. target chemical and anticipated soil concentrations of target chemical 8 hours to 1 month followed by sol vent desorption in off site or field laboratory and GC analysis with ECD PID or FID Soil gas concentration of chemical by volume is calculated using results of analysis sample exposure time and sampling rate for chemical of interest APPLICATION Assessment of VOC ground water contamination plume by soil gas sampling LIMITATIONS Does not provide ground water contaminant concentrations directly is an indirect method Site conditions affect method INSTRUMENTATION USED Activated carbon organic vapor monitors 3500 3M St Paul MN Various GCs and column configurations have been successfully used includ ing the HP 5710 GC ECD the AID GC ECD and the HNu 301 GC FID PID PERFORMANCE SPECIFICATION DETECTION LIMIT Depends on GC used local conditions and exposure time SELECTIVITY Volatile organics depends on GC method used ACCURACY Correlation of 0 93 between this technique and grab samples obtained ear lier correlation of 0 79 with ground water monitoring results PRECISION REPEATABILITY Based on closely spaced samples 12 RSD over 27 COMMENTS Need to demonstrate precision and correlation with ground water contamination at each site Test precision using closely spaced samplers and evaluate correlation with ground water data by regression analysis USE LOCATION USED Pittman Lateral Henderson NV Nume
116. te for Aroclor 1232 1242 1248 1254 1260 LIMITATIONS Results are approximations INSTRUMENTATION USED Analytical Instrument Development Corp AID Model 51 1 06 with ECD and 4 ft SE 30 column or Shimadzu Mini 2 with ECD and 4 ft OV 1 column PERFORMANCE SPECIFICATION DETECTION LIMIT 200 ug in water 100 ug kg in soil SELECTIVITY Compounds give characteristic multiple peaks good selectivity ACCURACY Average Percent Recovery 104 Range 65 193 PRECISION REPEATABILITY Average Relative Standard Deviation 14 range 5 0 42 COMMENTS The percent recovery decreases as PCB concentration increases USE LOCATION USED Beaver Creek Oregon 1985 EPA SITE NUMBER CERCLIS Not Available MATRIX Soil and Water PREPARATION MAINTENANCE AND CLEANUP Care should be taken not to contami nate column Column should be at thermal equilibrium before running ANALYSIS TIME 5 10 samples hr 40 CAPITAL COST AID 51 1 7 245 00 Shimadzu Mini 2 4520 00 CALIBRATION Calibration determined by peak heights and retention times of PCB stan dards Standards and blanks should be run every tenth sample COMMENTS Used regularly in Region X PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Hunt Chapman AFFILIATION Ecology and Environment Inc TELEPHONE 703 522 6065 PREPARED April 9 1987 BIBLIOGRAPHY Chapman H and Clay P Field Investigation Team FIT Screening Methods and Mobile Laboratories Compl
117. tion limits are obtained by taking 3 times the standard deviation from 14 determinations on a standard Selectivity Zeeman technique used to reduce background interference Accuracy Not generally available Whenever possible comparative results are presented in the user s Application Manual Precision Repeatability In general better than 10 Measurements are based on 14 determinations of a metal standard which lies in the middle of the linear working range For example the RSD for 8 ng ml copper was 3 for 1 0 ng ml of cadmium was 8 and for 20 ng ml lead was 7 Comments Portable generator can be used for power Argon gas is used for cooling the furnace eliminating need for water and as a purge gas Argon hydrogen and helium are also used as purge gases based on specific applications For each ele ment being analyzed a specific cathode lamp is required USE Location Used Field experience mainly related to mining beginning to be used in haz ardous waste work EPA Site Number CERCLIS Not Applicable Matrix Water and Soil Preparation Maintenance and Cleanup Monochromator adjustment required to analyze for each element Filament replacement in the furnace required after hundreds of firings Argon gas used for flushing 75 kg tank replacement in about 200 hours Analysis Time 2 minutes sample after sample preparation Capital Cost 20 000 30 000 Calibration Three 3 standard solutions covering the en
118. tire working concentration range of the element being analyzed are used and prepared fresh daily The standard solu tions and a blank is run at the start of each day and one standard is used to verify calibration three times a day Comments Easily set up for field work in mobile or stationary field laboratory Zeeman correction compensates somewhat for design compromise in optics and furnace re quired for portability Hazardous waste site experience is limited Protocol Available Yes SOURCE Technical Contact Dr John D Kinrade Affiliation Scintrex Limited Telephone 416 669 2280 Prepared 09 29 87 BIBLIOGRAPHY Becker D L and Carter M H Equipment Available for Sample Screening and On Site Measurements Appendices TDD HO831 1 04 U S EPA May 30 1984 Draft Kinrade J D et al Applications Manual for the Scintrex AAZ 2 Zeeman Modulated Absorption Spectrophotometer Scintrex Limited Concord Ontario Canada October 1986 METHOD FM 2 X RAY FLUORESCENCE XRF IN LABORATORY FOR HEAVY METALS SUMMARY Rapid screening of most metals 46 in soil and water in field laboratory to minimum of 20 mg kg in soil Conventional methods have better sensitivity and preci sion Simultaneous detection of the 18 elements analyzed for is one of the greatest advantages of the system METHOD DESCRIPTION Uses a flux of high energy x rays to bombard sample causing elements in sample to emit characteristic wavelengths T
119. titative results obtained during air analyses Quantitative software utilizing QA QC criteria is currently being developed by the ERT and by NYDEC Similar 54 software development is also being proposed by Battelle and by Sciex the instrument manufacturer For all analyses because of its cryogenic vacuum pump the instrument can only be used for a maximum of sixteen hours a day However typical analysis days rarely exceed fourteen hours INSTRUMENTATION USED TAGA 6000E Triple Quadrupole Mass Spectrometer Mass Spectrometer three quadrupoles are RF coupled sources in use are Atmospheric Pressure Chemical lonization APCI and Low Pressure Chemical lonization LPCI PERFORMANCE SPECIFICATION DETECTION LIMIT 1 10 ug l for most non polar organics in air 0 02 1 7 ug kg for dioxins in soil 0 02 ug kg for 2 3 7 8 TCDD 25 ug l for phenols and other such polar compounds in air 1 mg kg for PCB and chlorinated pesticides In soil without cleanup SELECTIVITY Compounds may be identified by comparing spectral peaks but lacks isomer specificity in air analyses Also during air analyses certain non isomeric com pounds will form isomers upon ionization e g isopropanol and acetone 1 2 dichloroethane and vinyl chloride and methylene chloride and chloroform ACCURACY Variation of less than 20 between spiked PCB and TCDD samples in different soil types PRECISION REPEATABILITY Standard deviation of 0 68 with a mean of 5 5 ug l dioxin
120. uated the meth ods contained in this document but has simply compiled existing methods The methods presented in this Catalog should not be viewed as Standard Operating Procedures SOP but rather as a compilation of available technologies which have been successfully utilized on a site specific basis Prior to the application of any of these methods the user is urged to consult with the technical contact listed for each method and an analytical chemist familiar with both the instrumentation method and the specific conditions inherent to the site under consideration It is also critical that an assessment be made of these site specific conditions and how they may effect the utility of the method and the resulting data quality The FSMC is available to users particularly those individuals responsible for devel oping and overseeing sampling activities at Superfund hazardous waste sites e g Regional Project Managers RPMs and contractor Site Managers SMs The Catalog currently consists of a User s Manual Including a listing of all methods a pocket guide a field screening methods data base and a computerized informa tion retrieval system contained on two floppy discs The discs are not included with this Users Guide but will be distributed separately to EPA Regional Offices for further distribution as the Region sees fit Information on how to acquire copies of the discs is available from the EPA Headquarters FSMC Systems Coordinator
121. uce effectiveness of soil gas sampling Precision and ground water correlation must be demonstrated for each site Determine applicability to each site by comparing to other sampling techniques USE LOCATION USED Tucson International Airport EPA SITE NUMBER CERCLIS CR811018010 MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Flushing of sampling equipment with nitrogen gas is effective in preventing contamination Inject carrier gas samples into GC to check for contamination Draw air through soil gas probes and inject into GC to check for contamination Teflon may be subject to carry over from high liquid or gas phase concentrations 28 ANALYSIS TIME NA CAPITAL COST Sampling probes 100 each syringes 30 40 Sampling pump 100 500 All are reusable GC 4 100 20 000 CALIBRATION Pump should be calibrated if used for composite samples COMMENTS One of several soil gas sampling methods that may be applicable under various circumstances PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Andrew Hafferty AFFILIATION Ecology and Environment Inc TELEPHONE 206 624 9537 PREPARED May 6 1987 BIBLIOGRAPHY Chapman H and Clay P Field Investigation Team FIT Screening Methods and Laboratories Complementary to Contract Laboratory Program TDD HQ 8507 01 October 17 1986 Draft Marrin D L Thompson G M Investigation of Volatile Contaminants in the Unsaturated Zone Above TCE Polluted Gr
122. uld be taken not to contami nate column Before run column should be at thermal equilibrium 36 ANALYSIS TIME 5 10 samples hr CAPITAL COST 7 245 00 CALIBRATION Calibration determined by peak heights and retention times of PCB stan dards Standards and blanks should be run every tenth sample COMMENTS This method has been used often in Region I PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT Dr Thomas Spittler AFFLILIATION U S EPA Region Laboratory TELEPHONE 617 861 6700 PREPARED 4 9 67 BIBLIOGRAPHY Spittler T M Field Measurement of PCBs in Soil and Sediment Using a Portable Gas Chromatograph Proceedings of 4th National Conference on Management of Hazardous Waste Sites Washington DC October 31 November 2 1963 Fowler B A and Bennett J T Screening For Characterization of PCB Containing Soils and Sediment 37 METHOD FM 19 PCB Analysis Using a Gas Chromatograph in an On site Laboratory Hexane Extraction SUMMARY Rapid determination of major Aroclors to 25 ug l in water and 2 500 ug kg in soil Requires field laboratory Appropriate extraction solvent should be determined by laboratory testing prior to field use METHOD DESCRIPTION Requires field laboratory with GC and linearized ECD for PCB analysis of water and soil samples Identification is done by comparing peak retention times with external standards Quantitation is determined by comparing peak heights and volumes
123. ve GC ECD could be used PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT William Loy AFFILIATION EPA Region IV ESD TELEPHONE 404 546 3386 PREPARED April 15 1987 BIBLIOGRAPHY Screening Method For Extractable Organic Compounds EPA Region IV Mobile Laboratory Protocol January 1987 39 METHOD FM 20 PCB ANALYSIS USING A GAS CHROMATOGRAPH IN AN ON SITE LABORATORY HEXANE METHANOL SUMMARY Rapid determination of major Aroclors to 200 ug kg in soil and 200 ug l in water Requires field laboratory Appropriate extraction solvent should be determined by laboratory testing prior to field use METHOD DESCRIPTION Requires a field laboratory with GC and linearized electron cap ture detector for PCB analysis of soil samples Identification is done by comparing peak retention times with external standards Quantitation is determined by comparing peak heights and volumes of the standard and sample Sample preparation for water consists of adding 1 ml hexane to 100 ml of water mixing sample and separating hexane layer This step Is repeated once Add 1 ml sulfuric acid to hexane extract and mix Sample is ready for GC analysis Sample preparation for soil consists of mixing 1 to 2 grams soil 2 ml methanol and 10 ml hexane Separate hexane layer add 1 ml sulfuric acid to ex tract and mix Hexane extract is ready for GC analysis APPLICATION Simple and rapid determination of polychlorinated biphenyls Method most appropria
124. wn quality on a high volume cost effective basis The central and overriding assumption governing the structure and function of the CLP is the basic requirement to provide legally defensible analytical results for use in supporting Agency actions As of early 1987 the CLP was able to provide over 6 000 sample analyses per month through its Routine and Specialized Analytical Services RAS and SAS Programs Based on the central and overriding assumption to provide legally defensible analytical results CLP data deliverable packages are accompanied by very specific documentation containing information which includes initial and continuing calibration GC MS tuning surrogate percent recovery matrix spike duplicate results GC chromatograms Furnace AA analysis digestion distillation logs ICP interference and serial dilution analysis and spectra for every sample and every blank standard or spike run with a particular set of samples Data delivery for this complete data package takes approximately 3540 days after submission An additional 30 days for Regional review of each data pack age is also required Faster turn around times can be achieved through the SAS and through expedited review by the Regions It is now recognized in the scientific regulatory community that frequently the ap proximately 65 70 day turn around in sample analyses is unacceptable and that the quality of data provided by the CLP is not required fo
125. y be misleading Sensitivity depends on GC used Clay layers and horizons with lt 5 air filled porosity reduce effectiveness of soil gas sampling Compare to other sampling methods to assess applicability to a particular site USE LOCATION USED Puget Sound WA 1986 EPA SITE NUMBER CERCLIS Not Available MATRIX Soil PREPARATION MAINTENANCE AND CLEANUP Determine appropriate drilling depth by use of test holes need to drill below surface soils to bypass competing adsorption sinks or by combined experience and assessment of site factors Auger and syringe decontamination required Periodic direct mixing of probe contents needed before sam pling to provide equilibrium conditions along probe length Minimal sample preparation required before analysis 26 ANALYSIS TIME 15 30 minutes to drill boreholes 2 days for sample probe equilibration 1 minute to collect sample CAPITAL COST Syringes 30 40 probes 100 plus drilling equipment GC 4 100 20 000 CALIBRATION Purge syringes with nitrogen and check for contamination by injecting carrier gas samples Into GC Periodic mixing of probe contents COMMENTS Long term changes in soil gas concentration will not be evident without mixlng of probe contents PROTOCOL AVAILABLE Yes SOURCE TECHNICAL CONTACT John Ryding AFFILIATION C C Johnson amp Malholtra TELEPHONE 303 433 6966 PREPARED May 6 1987 BIBLIOGRAPHY Jowise P P Villnow J D Gorelik L I and

Field Screening Methods Catalog: User`s Guide (U.S. EPA

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