Attachment_1_-_BPA-TO_15_SOW.pdf

EPA Region 2 and Region 3

TO-15 AIR ANALYSIS

REQUEST for ANALYTICAL SERVICES

I. General Information:

EPA Region 2 and Region 3 requires the analysis of TO-15 air samples collected in 6 Liter Summa Canisters. Samples are collected from Superfund sites located in New York, New Jersey, Pennsylvania, Maryland, Delaware, Virginia, West Virginia, Washington D.C., Puerto Rico and the US Virgin Islands, though the majority will be for sites in New York and New Jersey. For the purpose of this Statement of Work (SOW), suspected site contaminants would be Volatile Organic Compounds (VOCs). It should be noted that since these samples are being collected at Superfund sites, there is the potential for higher concentrations of contaminants. This SOW is separate from any Region 3 contract SOWs for TO-15 work. Awards under the RFQ for this SOW will primarily be utilized for Region 2 work but will allow Region 3 the ability to place call orders under the BPAs should the need arise.

A. To maintain consistency with data submitted through other laboratory programs, each project assigned under this SOW should be identified, on all deliverables, using the Regional Tracking (Case) number provided with each request (YY- XXXX) and the Sample Delivery Group (SDG) number as defined below in Section C of this SOW. Both SDG Cover Sheets and Invoices should also contain the Regional Tracking and associated SDG numbers.

B. The EPA will usually need 10 to 40 canisters per event, but at times may require up to 100 canisters over a one-week period. Ideally, the Contractor should be able to provide the number of canisters and flow controllers required for projects submitted by the Region. EPA Region 2, will try to provide as much advanced notice as possible for all sampling events (usually one – two weeks prior to the need for delivery of canisters) however, there may be emergency circumstances in which the Region may require canisters with less than a week notice prior to the sampling event.

C. Region 2 utilizes 6-liter summa canisters for sample collection and needs air samples analyzed via EPA Method TO-15 and per the specifications of this SOW, when possible. Specific details and needs for each project will be provided in individual requests submitted for each case. A maximum of 600 samples per year, are expected to be collected and analyzed by the EPA.

D. For planning purposes, sampling is generally heavier during the heating season, October to April. During this time, EPA Region 2 can be expected to request the majority of the analyses. From May to September the sample volume is much lower.

II. Period of Performance

The period of performance for this BPA is five years.

III. Contact Information

A. Organization:

US EPA Region II Division of Environmental Science and Assessment (DESA)

HWSS MS-215

2890 Woodbridge Ave.

Edison, NJ 08837 Fax: (732) 321-6622

B. Project Officer (PO) and Sampling Contact: Jennifer Feranda Phone: (732) 321-6687 E-mail: Feranda.jennifer@epa.gov

C. Alternate Project Officer: Kim Brandon-Bazile Phone: (732) 321-6711 E-mail: Brandon-Bazile.kim@epa.gov

D. Document Control Coordinator EPA Region 2: Adly Michael Phone: (732) 906-6161 E-mail: Michael.Adly@epa.gov

Document Control Coordinator EPA Region 3: Jarmael Burman Phone: (410)-305-2743 E-mail: Burman.Jarmael@epa.gov

E. Data Delivery Recipient EPA Region 2: Adly Michael

Data Delivery Address:

U.S. EPA Region 2 Document Control Room (DCR) Building 205 2890 Woodbridge Ave.

Edison, NJ 08837 mailto:Feranda.jennifer@epa.gov mailto:Michael.Adly@epa.gov mailto:burman.jarmael@epa.gov

Data Delivery Recipient EPA Region 3:

Data Delivery Address:

USEPA Region 3 Environmental Science Center

OASQA/EAID/TSB (3EA22)

701 Mapes Road Fort Meade, Maryland 20755-5350 Attention: Jamal Burman

Summary of Process and Requirements:

A. Requests for Services

a. Request for each individual project (Case) will be issued by the Contracting Officer via a call order against the BPA. The request will be submitted ideally, one to two weeks prior to the sampling start date.

However, there may be emergency circumstances in which the sampling team may require canisters with less than a week notice prior to the sampling event. The EPA will make every effort to give the lab as much advanced notice as possible prior to the start of a project.

b. The call order sent (via e-mail) will contain the following information:

i. Project specific case number (refer to I.A above)

ii. Sampling period (start date and end date)

iii. Number of canisters and flow controllers required

iv. Number of T-valves (for duplicate samples) if required

v. Required compounds and detection limits (per Table 1)

vi. Trip Blank (if required for analysis)

vii. Date canisters required to be delivered to sampling team

viii. Address canisters to be shipped to

ix. As necessary, sampler contact information. In the absence of this information the contact will default to the PO as listed above in II.B.

x. Any project specific information for the individual case.

B. Canister Preparation and Shipment

a. When possible, the laboratory may be asked to provide the following:

i. For each sample requested, 6 Liter Summa Canisters, shall be equipped with a pressure/vacuum gauge which indicates the amount of vacuum in the canister upon receipt at the site.

ii. Twenty-four (24) hour, constant flow rate orifices, at one per canister.

iii. T –valves for collecting duplicate samples may be requested to be provided by the laboratory at the number specified with each request (usually one or two per project).

iv. All canisters and potentially flow rate orifices shall be individually certified clean at or less than the detection limit concentrations required for the SCAN and/or Trace analysis levels, as specified for each compound per the individual project analysis requests.

a. Copies of clean canister certifications, which include the analytical results of the certification(s), shall be included with the canisters when shipped to the sampling contact prior to the start of the sampling event.

b. Canisters shall be provided by the Contractor and shipped to the sampling contact at the address provided and by the date designated in each individual project request.

c. If the project requires canisters for both SCAN and Trace analysis:

canisters for Trace analysis and canisters for SCAN analysis shall be shipped in separate boxes. Each canister shall contain a sample label to reflect the appropriate detection level certifications, i.e., which canisters have been certified clean for the requested reporting limits (Trace or Scan).

d. The Contractor shall seal all shipping containers to ensure the integrity of the chain of custody of the canisters. The Contractor shall seal the shipping containers with an appropriately numbered custody-sealing device and record the sealing device number on the Chain of Custody form. The Contractor shall, ensure that the appropriate containers are present for each analysis requested.

e. The Contractor shall provide canisters in an appropriate shipping container. The shipping container shall securely hold the canisters and any supporting equipment (i.e., flow controller, pressure gauge, etc.) and shall meet the shipping requirements of the USDOT and overnight common carrier.

f. The Contractor shall provide a mechanism to ship empty canisters to the designated sampling contact person by an overnight common carrier. The Contractor shall ship canisters only to official Government Offices, warehouses or work sites as designated in the individual project requirements.

C. Canister Receipt and Sample Delivery Group(s)

a. Once samples have been collected, all canisters (used and unused) as well as all associated equipment will be returned to the Contractor. EPA or their designated representative will be responsible for the shipping costs associated with the return of the canisters and supporting equipment to the Contractor.

b. Each sample received by the Contractor shall be labeled with an EPA Sample Number, and accompanied by a Traffic Report/Chain of Custody (TR/COC) bearing the sample number and descriptive information regarding the sample.

c. Once the canisters are received, they shall be grouped into Sample Delivery Groups.

d. A case consists of one or more SDG(s). An SDG is defined by the following, whichever is more frequent:

i. Each Case of field samples received; or

ii. Each 20 field samples within a case; or

iii. Each 7 calendar day period during which field samples in a Case are received (said period beginning with receipt of the first sample in the SDG).

e. For EPA Region 2 & Region 3 reporting purposes, the SDG name shall be designated by the first EPA sample number ID in the SDG. For example, if the laboratory receives 10 samples and the first sample number in the SDG is B0001, the SDG name/designation will be “SDG B0001”.

f. For sample tracking purposes, within three (3) days of completion of an SDG, the laboratory shall forward to the EPA Region 2 PO, via e-mail, the completed “Region 2 Delivery of Analytical Services (DAS) Sample Delivery Group (SDG) Cover Sheet” (Attachment #1)

D. Analytical Methods and Requested Compound List:

a. Depending on the project requirements, the Contractor will be asked to provide either; the analysis of samples for a more comprehensive TO-15 compound list which would entail the entire list provided in Table 1 or a smaller subset of the Table 1 compound list. For some projects, additional compounds, which are not found in Table 1, may be requested based on the specific needs for that Case. Analysis shall be performed by the TO- 15 method and additional requirements as prescribed in this Statement of Work (SOW). The required analyte list will be designated, by the EPA, at the time of each individual project request.

b. The reporting limits listed in Table 1 are the EPA Region 2 requirements for analysis by both the TO-15 SCAN method and those compounds which require analysis for Trace levels (SIM/lower CRQLs) by Gas Chromatography/Mass Spectrometry (GC/MS) SIM or equivalent methodology. The SIM equivalent (Trace level) methodology shall able to achieve the required reporting limits defined in the “Required Reporting Limits for Trace Analysis” column of Table 1. It is anticipated that approximately 50 – 75% of all samples analyzed will request analysis for Trace levels as specified in Table 1. It should be noted that some projects may require analysis solely by the SCAN method, solely for Trace levels (SIM) or a combination and/or subset of both.

c. The laboratory will perform the analysis of samples per “EPA Method TO-15: Determination of Volatile Organic Compounds (VOCs) in Air Collected in Specially-Prepared Canisters and Analyzed by Gas Chromatography/Mass Spectrometry (GC/MS). (January, 1999)” or any subsequent revision of this method; the requirements of this Statement of Work; and project specific requirements as defined in the individual call orders.

Table 1:

. Region 2 TO-15 BPA Target Compound List and Standard Reporting Limits

CAS No. Compound Required Reporting Limit for

SCAN

Analysis (ppbv)

Required Reporting Limit for

SCAN

Analysis (ug/m3)

Required Reporting Limit for Trace/SIM

Analysis (ppbv)

Required Reporting Limit for Trace/SIM

Analysis (ug/m3)

67-64-1 Acetone 5.0 11.88 ----- ----- 107-05-1 Allyl Chloride 0.5 1.57 0.08 0.25 71-43-2 Benzene 0.2 0.64 0.04 0.13 100-44-7 Benzyl chloride 0.2 1.04 ----- ----- 75-27-4 Bromodichloromethane 0.2 1.34 0.04 0.27 75-25-2 Bromoform 0.2 2.07 0.04 0.41 74-83-9 Bromomethane 0.2 0.78 0.08 0.31

78-93-3 2-Butanone (Methyl Ethyl Ketone) 0.5 1.47 ----- -----

75-15-0 Carbon disulfide 0.5 1.56 ----- ----- 56-23-5 Carbon tetrachloride 0.2 1.26 0.04 0.25 108-90-7 Chlorobenzene 0.2 0.92 ----- -----

Reporting Limit for

SCAN

Analysis (ppbv)

Required Reporting Limit for

SCAN

Analysis (ug/m3)

Required Reporting Limit for Trace/SIM

Analysis (ppbv)

Required Reporting Limit for Trace/SIM

Analysis (ug/m3)

75-00-3 Chloroethane 0.5 1.32 0.08 0.21 67-66-3 Chloroform 0.2 0.98 0.04 0.19 74-87-3 Chloromethane 0.5 1.03 ----- ------ 124-48-1 Dibromochloromethane 0.2 1.70 0.04 0.34 106-93-4 1,2-Dibromoethane 0.2 1.42 0.04 0.28 95-50-1 1,2-Dichlorobenzene 0.2 1.20 ----- ----- 541-73-1 1,3-Dichlorobenzene 0.2 1.20 ----- ----- 106-46-7 1,4-Dichlorobenzene 0.2 1.20 ----- ----- 75-71-8 Dichlorodifluoromethane 0.5 2.10 0.04 0.17 75-34-3 1,1-Dichloroethane 0.2 0.81 0.02 0.08 107-06-2 1,2-Dichloroethane 0.2 0.81 0.04 0.16 75-35-4 1,1-Dichloroethene 0.2 0.79 0.04 0.16 156-59-2 cis-1,2-Dichloroethene 0.2 0.79 0.04 0.16

156-60-5 trans-1,2- Dichloroethene

0.2 0.79 0.04 0.16

75-09-2 Dichloromethane 0.5 0.69 ----- ----- 78-87-5 1,2-Dichloropropane 0.2 0.92 0.08 0.37 10061-01- 5 cis-1,3-Dichloropropene

0.2 0.91 0.04 0.18

1006-02-6 trans-1,3- Dichloropropene

0.2 0.91 0.04 0.18

123-91-1 1,4-Dioxane 5.0 18.02 ----- ----- 100-41-4 Ethylbenzene 0.2 0.87 0.04 0.17 622-96-8 4-Ethyltoluene 0.2 0.98 0.04 0.20 76-13-1 Freon 113 0.2 1.53 ----- ----- 76-14-2 Freon 114 0.2 1.4 0.04 0.28 142-82-5 n-Heptane 0.2 0.82 0.04 0.16 87-68-3 Hexachlorobutadiene 0.2 2.13 ----- ----- 591-78-6 2-Hexanone 0.5 2.05 ----- ----- 108-10-1 Methyl Isobutyl Ketone 0.5 2.34 ----- ----- 80-62-6 Methyl methacrylate 0.5 2.05 ----- ----- 1634-04-4 Methyl tert butyl ether 0.2 0.72 0.04 0.14 91-20-3 Naphthalene 0.5 2.62 ----- ----- 100-42-5 Styrene 0.2 0.85 ----- -----

79-34-5 1,1,2,2- Tetrachloroethane

0.2 1.37 0.04 0.27

127-18-4 Tetrachloroethene 0.2 1.36 0.04 0.27 108-88-3 Toluene 0.2 0.75 0.04 0.15 120-82-1 1,2,4-Trichlorobenzene 0.5 3.71 ----- ----- 71-55-6 1,1,1 -Trichloroethane 0.2 1.09 0.04 0.22

Reporting Limit for

SCAN

Analysis (ppbv)

Required Reporting Limit for

SCAN

Analysis (ug/m3)

Required Reporting Limit for Trace/SIM

Analysis (ppbv)

Required Reporting Limit for Trace/SIM

Analysis (ug/m3)

79-00-5 1,1,2-Trichloroethane 0.2 1.09 0.04 0.22 79-01-6 Trichloroethene 0.2 1.07 0.04 0.21 75-69-4 Trichlorofluoromethane 0.2 1.12 0.04 0.22 95-63-6 1,2,4-Trimethylbenzene 0.2 0.98 ----- ----- 108-67-8 1,3,5-Trimethylbenzene 0.2 0.98 0.08 0.39 108-05-4 Vinyl acetate 5.0 1.76 ----- ----- 75-01-4 Vinyl chloride 0.2 0.51 0.04 0.21

108-38-3 m & p-Xylene 0.5 0.87 0.08 0.38

95-47-6 o-Xylene 0.2 0.87 0.04 0.17

E. Additional Analytical Requirements

a. Equipment Requirements:

i. The Contractor shall comply with all the GC/MS tuning requirements set forth in the instrument operator’s manual and USEPA Method TO-15 and the Contractor’s approved laboratory Standard Operating Procedures (SOP). Post-acquisition manipulation of the ion abundances using computer software to achieve tuning criteria is acceptable. Any sample analyzed in conjunction with a failed tune performance check requires re-analysis and shall be performed at the Contractor’s expense.

ii. The Contractor shall maintain a GC/MS equipped with a computerized MS library search system capable of providing reverse searching for targeted analytes and forward searching for non-targeted analytes. The Contractor shall use the most recent NIST/EPA/MSDC or the most recent Wiley mass spectral library for searches of targeted analytes. The system shall also be capable of removing background signals from the suspect chemical pollutant spectrum (background subtraction capability).

b. Tentatively Identified Compounds (TICs)

i. Analysis of TICs is not a standard requirement of this SOW but may be requested on a project by project basis.

ii. A library search shall be executed for non-target sample components for the purpose of tentative identification. The Contractor shall use the most recent NIST/EPA/MSDC or Wiley mas

iii. s spectral library as the reference library.

iv. All organic compounds that have not been positively identified as volatile target analytes shall be tentatively identified via a forward search of the NIST, Wiley, or equivalent mass spectral library. Only after visual comparison of sample spectra with the nearest library searches will the mass spectral interpretation specialist assign alternative identification. Computer-generated library search routines shall not use normalizations which would misrepresent the library or unknown spectra when compared to each other.

v. Up to 10 non-alkane Tentatively Identified Compounds (TICs) of greatest apparent concentration shall be reported. Peaks that are tentatively identified as straight-chain, branched, or cyclic alkanes, and are alone or part of an alkane series, shall be reported as "total alkanes". An alkane is defined as any hydrocarbon with the generic formula CnH2n+2 (straight-chain or branched) or CnH2n (cyclic) that contains only C-H and C-C single bonds. The concentrations of each of the alkanes shall be summed and reported as a single result for the "total alkanes".

Documentation for the tentative identification of each alkane shall be supplied in the hard copy deliverable packages. The alkanes are not to be counted as part of the 10 compounds individually reported as TICs. Carbon dioxide and compounds with responses less than 10% of the internal standard in which they are to be quantified (as determined by inspection of the peak areas or height) shall not to be reported (nor are they to be counted as part of the 10 compounds that are to be reported).

c. Electronic Media Storage for Data

i. Data storage devices shall be suitable for long-term, off-line storage of data.

ii. The laboratory shall store all raw data and processed electronic analytical data in the appropriate instrument manufacturer’s format, uncompressed and with no security codes. The electronically stored data shall include all data needed to completely reconstruct a hard copy and electronic deliverable. The electronic data files shall include, but are not limited to, blanks, spikes, tunes, calibrations, quality control samples, proficiency testing samples and check samples. The electronic data files shall also include all laboratory generated spectral libraries and quantitation reports as well as the associated raw data files if those files contain data or instrument parameters related to analytical results.

iii. If a request is made by the USEPA for the electronic data files, the files shall be sent within ten (10) days from receipt of the written (email) request.

d. Pressure of Canisters

If a sample of air is received and the pressure in the canister is less than -10 inches of Mercury (-10, -15, -20, etc.), the EPA Region 2 PO shall be contacted for guidance on how to proceed. If directed by EPA, the Contractor may proceed with dilution and analysis of the sample as specified in TO-15. (Note: It is understood that a sample should never be received at zero negative pressure or at pressure equal to atmospheric pressure. If this occurs, the Contractor shall contact the EPA Region 2 PO immediately). The humidified ultra pure zero air or humidified ultra pure nitrogen that is added to canister to bring the sample up to the method specified pressure shall be from the same source as the method blank air.

e. Leak Tests

Perform a leak test on each canister by evacuating the canister to approximately –

29.5 Hg.

f. Method Detection Limits

The minimum MDL reported for each target analyte shall be less than or equal to the clean canister certification specified in Method TO-15 for each appropriate analysis (SCAN or Trace/SIM). The contractor shall provide the USEPA their most recent MDLs within 7 days from receipt of a written (email) request.

F. Additional QA/QC Requirements

a. TRIP BLANKS:

The Contractor may need to analyze a Trip Blank sample on a project specific basis. The need for a Trip Blank will be stated in the project request as well as provided on the Chain of Custody Record. The Contractor will receive the un-opened canister with the same negative pressure as the initial delivery. The Contractor shall treat the sample as a Method Blank and shall follow the same requirements as stated in Method TO-15 Section 10.7 regarding method blanks.

b. METHOD BLANKS:

i. The laboratory shall follow the requirements of Method TO-15 Section 10.7 regarding method blanks. Any method blank that deviates from the preparation and technical acceptance requirements specified in the method will not be acceptable and will be rejected by the Region. Any analysis that is related to a failed method blank will also be rejected.

ii. The serial number of the method blank canister shall be noted on all the clean canister logs and instrument run logs.

iii. A canister that has been designated as a canister that is being certified clean as part of the batch certification process shall not be designated as a method blank.

c. . INSTRUMENT BLANKS:

i. If the laboratory determines during the analytical sequence that an instrument blank needs to be analyzed for any reason within an analytical sequence, the instrument blank shall meet the requirements of Method TO-15 Section 10.7 to be acceptable. The sample shall be labeled as an instrument blank and the reason for analyzing the blank documented (e.g. testing for carryover) in the case narrative and the instrument run log.

ii. The serial number of the instrument blank canister shall be noted on all applicable instrument run logs.

iii. A canister that has been designated as a canister that is being certified clean as part of the batch certification process shall not be designated as an instrument blank.

iv. The instrument blank that demonstrates that there was no carryover from the previous sample is to be reported. The laboratory can also report the instrument blank that demonstrates that the system is clean. Instrument blanks analyzed during the instrument decontamination process that exceed the requirements listed in this section do not need to be reported.

d. LABORATORY CONTROL SAMPLES:

i. The Contractor shall analyze one Laboratory Control Samples (LCS) and one Laboratory Duplicate each time a Method Blank is analyzed.

ii. The LCS shall be prepared in the same manner as the Method Blank (Method Section

10.7) with the only difference being that the canister is spiked with all compounds at the mid-point concentration of the calibration curve for both the SCAN and Trace level analyses. The LCS shall be spiked with all highlighted compounds in Table 1.

iii. The LCS shall meet the same internal standards and retention time technical requirements as a method blank as provided for in Method section 10.7.5.

iv. The percent recovery for each of the compounds in the RLLCS should be within 70- 130 % of the known value for 90 % of the compounds for the LCS to be considered acceptable. If less than 90% of the LCS recoveries are within the control limits, then all the compounds (detected and non-detected compounds) in the associated sample should be qualified and a statement must be added to the case narrative stating that all the data in the associated samples are qualified. The EPA may choose to reject all affected data based on the severity of the failure. If greater than 90% of the LCS recoveries are within control limits, then only the affected compounds in the associated samples are to be qualified and listed in the case narrative of the required analytical data package

e. INTERNAL STANDARDS:

i. During the course of sample analysis, the Contractor may determine that the internal standard area response is outside the control limits as established by Method TO-15, Section10.8.6.1. When this occurs, the Contractor shall comply with the corrective action procedures specified in the method and reanalyze the sample as required. The laboratory shall report data for both the initial analysis and the reanalysis. The laboratory shall not submit more than two sets of data. If upon reanalysis of the sample, after corrective action, the internal standard area responses are within the control limits established by the method, the problem is determined to be within the control of the laboratory and the laboratory will be paid for only one analysis. If upon reanalysis of the samples, the internal standard area responses are outside of the control limits established by the method, a matrix effect is occurring. This matrix effect is outside the control of the laboratory. Therefore, laboratory will be paid for two analyses.

f. ANALYTICAL SEQUENCE FOR SAMPLES ANALYSIS:

Method TO-15 specifies the analytical sequence for the sample analysis. The only addition to this sequence is the analysis of the two (2) Laboratory Control Samples after the analysis of the Method Blank and after the completion of the initial calibration sequence or daily calibration. Method TO-15 Sections 10.4-

10.8 all have reference to the analytical sequence required for the initial and daily calibration requirements. The Contractor shall meet both the method and contractual requirements for the initial and daily calibrations.

g. GC/MS INSTRUMENT PERFORMANCE TUNE CHECK STANDARD

REQUIREMENTS:

The GC/MS Instrument Performance Tune Check Standard shall contain Bromofluorobenzene (BFB) and should not be combined with any calibration standard to create an injection consisting of a calibration standard and the tune solution. The BFB Tune Check Solution is the first injection in any 24-hour sequence. The BFB tune shall meet the requirements of Method Sections 10.4.3 and 10.4.4 to be considered acceptable.

h. SAMPLE DILUTIONS

NOTE: Dilution for the purposes of the following discussion is defined as the process of adding a diluent gas to a sample in order to reduce the sample concentration so that it is within the calibration range of this method. For laboratories performing automatic canister pressurizations to slightly above one atmosphere, a sample will be considered diluted if an additional volume of makeup gas is added to that volume of makeup gas routinely employed.

As part of the routine analysis, canisters will be received by the laboratory that will require dilutions to be conducted so that sample results will be within the calibration range of the instrument. As part of the process, this method requires the laboratory to incorporate the following procedures when diluting samples from canisters. The laboratory shall describe which of the following dilution procedures that they intend to use for this method in their Case Narrative and SOP.

Automatically adding humidified ultra-pure air or humidified ultra- pure nitrogen to the canisters may not necessarily be considered a dilution for purposes of the discussion below. If the laboratory must add additional make up air to the sample for a dilution (for the purpose of generating data within the initial calibration range of the method) then the air source shall be the same as the air source that is used for the preparation of the method blanks, that being humidified ultra-pure zero air or humidified ultra-pure nitrogen.

i. All dilutions shall be made immediately prior to GC/MS analysis of the sample.

ii. The dilution procedures shall be documented in the Case Narrative of the analytical data package.

iii. If all sample target analyte results are at or below the required reporting limits, then the sample shall be analyzed without adding additional makeup air.

iv. If any target analyte results are less than the high calibration standard in the sample, then the sample shall be analyzed without adding additional makeup air.

v. If dilutions are required due to concentrations in the samples that exceed the upper calibration of the instrument, then the volume drawn from the canister may be reduced and/or ultra-pure humidified zero air or ultra-pure humidified nitrogen may be used as a diluent gas. All sample data shall be reported with the dilutions factored in and the all the reporting limits shall be adjusted for the required dilutions.

vi. Both the undiluted and diluted sample data shall be reported on separate data summary reporting forms with all the accompanying documentation.

vii. The laboratory shall choose a sample specific dilution factor that is required to keep the concentration of the largest peak for a target compound in the upper half of the initial calibration range.

viii. Any screening data shall be provided in the analytical data packages.

ix. If the screening results indicate that the peak response for any target compound in any sample does not exceed the peak response in the highest standard in the initial calibration, then the sample shall be analyzed without adding additional makeup air.

x. If the screening results indicate that the peak response for any target compound in any sample does exceed the peak response in the highest standard in the initial calibration, then the laboratory shall choose one of two options.

1. The laboratory can analyze the sample as undiluted and then analyze the sample at the correct dilution level. The laboratory can use the results of the original analysis to determine the approximate dilution factor to get the largest analyte peak within calibration range. The laboratory may not submit more than two sets of data. The laboratory shall submit both sets of data separately. Both sets of data shall meet the requirements of the method.

2. The laboratory shall choose the dilution level that will allow the sample to be analyzed at the most concentrated dilution and meet the requirements of the method. The laboratory shall demonstrate that it has chosen the appropriate level by analyzing the sample at one further dilution. The laboratory may not submit more than two sets of data. The laboratory shall submit both sets of data separately. Both sets of data shall meet the requirements of the method.

ii. There are various options available for the dilution of the samples depending on the analytical systems used by the laboratory. The laboratory must provide in their Case Narrative and SOP which options they will be using in sample analysis. The options can include the following:

1. Injection of a volume of sample into another certified clean canister and induction of ultra pure humidified zero air.

2. Dilutions conducted directly on the instrument.

3. Tedlar Bags can be used. When tedlar bags are used, absorption and contribution issues shall be determined prior to their use. Tedlar bag blanks shall be analyzed as part of the analytical sequence. These blanks are in addition to the required method blanks and must be clearly identified in the sequence. The blanks shall be analyzed after the method blank and prior to the sample.

4. The laboratory can propose other options for the dilution of the samples. However, approval must be obtained from EPA Region 2 prior to their use.

G. Data Turnaround Time:

i. Preliminary Electronic File/EDD – 7 to 14 calendar days per individual project requirements.

j. Final Hard Copy – As the standard, 14 calendar days unless otherwise specified in the individual project call order.

k. Data turnaround time is determined per SDG (see Section C above) based on the Verified Time of Sample Receipt (VTSR) of the last sample in the

SDG.

G. Data Deliverables:

a. The Contractor shall submit both a hard copy and PDF electronic copy of the data package including all analytical results. Each delivery package shall be comprised of CLP forms 1-8 or equivalent (forms) that convey the following:

i. Reporting of all data should be done by Regional Tracking (Case) Number

(Section I A above) and SDG number as defined in Section IV. C above.

ii. All results shall be reported in ppbv and ug/m3.

iii. Hard copy data packages shall contain a CLP DC-1 equivalent form that contains information regarding the canister conditions and pressure upon receipt at the lab.

This form shall also contain the canister ID number and the corresponding field sample number.

iv. Hard copy data packages shall contain a Table of contents or CLP equivalent DC-2

Form. Data package should be paginated for easy cross reference between the table of contents and relevant portions of the data. Data packages shall be submitted, per the CLP DC-2 form, with data grouped together per sample (i.e., related forms, raw data, etc), with additional information, such as canister certifications, included toward the end of the package.

v. SDG/Case Narrative must be provided with each data package. The SDG narrative shall contain all relevant canister and analysis quality issues and actions taken. The narrative shall also include a statement and supporting information as to the relevance and appropriateness of any manual integrations.

vi. Target analytes analyzed for by the method, the CAS number for each analyte, the concentration and concentration units for each analyte (e.g. ppbv), the reporting limit for each “non-detect” analyte, a qualifier for each analyte (e.g. an E qualifier indicates concentration is an estimate. Qualifiers shall be defined in each order), EPA sample identification number, Laboratory specific sample identification number, Laboratory name, Contract Number, Date sample received, Date sample analyzed, Case number, Sample Delivery Group Number (SDG), Instrument Identification number, Sample size analyzed, and level of dilution, if applicable.

vii. Summa Canister Final Pressure Check Record. This includes sample lab ID, canister serial number and initial pressure Hg, final pressure Hg. A table shall be submitted containing the following information:

1. Canister ID

2. Date/Time of initial vacuum

3. Value of initial vacuum (“Hg)

4. Date/Time of vacuum after at least 24 hours has elapsed

5. Value for 24 hour vacuum (“Hg)

6. Difference between two vacuum values

viii. Results of canisters and orifice/sample train certification for each individual canister. Results for all compounds shall include actual detection limits found in certification, not simply a “non-detect”. Cross reference should be provided between canisters and orifice/sample train certification number and individual sample number. GC/MS documentation (i.e., ion chromatograms, quantitation reports, etc.) for clean canister and orifice/sample train certifications shall also be included in the final data packages.

ix. Results of initial calibration analyses as specified in the analytical method. Results shall include name of each calibration analyte standard, the concentration and concentration units for each calibration analyte, the relative response factor or calibration factor determined for each calibration analyte, the statistical evaluation of each calibration analyte for each concentration level ( usually five calibration levels are specified in each method) that shows degree of linearity or acceptability of the “calibration curve” (usually as a %RSD), the acceptable criteria for the initial calibration analyses as described by the formal analytical method and laboratory SOP, Laboratory name, Contract number, Case and SDG number, Instrument Identification number, and Calibration dates for each calibration level.

x. A run log shall be provided. The run log states the order of the run in the following sequence: BFB tuning, ICAL/CCV, Method Blank, LCS, LCSD, followed by the samples. BFB, CCV, MB, LSC, LCSD must be run every 24 hours of sample analysis per instrument.

xi. Data shall be tabulated and presented per run log order.

xii. Results of Mass Spectra tuning (BFB) for each tuning performed

xiii. Results of all daily or continuing calibration analyses as specified in the analytical method. Results shall include name of each calibration analyte standard, the concentration and concentration units for each calibration analyte, the relative response factor or calibration factor determined for each calibration analyte, the statistical evaluation of each calibration analyte with respect to the initial calibration analysis (usually as a %Difference from the initial calibration analyses for each analyte), the acceptable criteria for the continuing calibration analyses as described by the formal analytical method and laboratory SOP, Laboratory name, Contract number, Case and SDG number, Instrument Identification number, and Calibration date.

xiv. Results of Mass Spectrometer tuning analyses where samples have been analyzed by GC/MS (as specified in the formal analytical method). Laboratory name, Contract number, Instrument Identification number, date of tuning analyses, acceptance criteria as listed by the formal method for the tuning analysis, and samples that are associated with the tuning analysis.

xv. The mass spectra for all GS/MS performance check, BFB, shall be shown.

xvi. Results of all blank analyses pertinent to a set of data or SDG. Results of blank analyses may be submitted using forms used to report sample analyses as per instructions in item (1) above.

xvii. Each sample and method blank shall include a data summary report, quantitation report, mass spectra and reference mass spectra for all positive compounds of interest.

xviii. Results of all Quality Control/Assurance samples pertinent to an SDG. This may include matrix spike and duplicate analysis (spike of a field sample), or a Laboratory Control Sample (LCS).

xix. LCS/LCSD shall include the quantitation report. Mass Spectra are not required.

xx. Internal Standard Area and RT summary forms. A table containing the following information shall be submitted in the data package:

1. Col 1: 24 hour Standard, Upper Limit, Lower Limit, EPA Samples

2. Col 2: Area count for Internal Standard (IS) #1

3. RT of IS #1

4. Area count for Internal Standard (IS) # 2

5. RT for IS #2

6. Same as Col 2 & 3 if there is a 3rd IS

7. If needed, additional columns may be created. Place an asterisk next to the area count(s) that do not meet the + 40 % criteria.

xxi. All canisters shall be leak tested prior to sampling use. The initial gauge pressure shall be approximately 30 psi with zero air. The canister pressure test must not vary by more than +/- 2psi over a 24 hour period. This data is to be presented in a summary form for all canisters and shall include the canister serial number, initial pressure, final pressure and times.

b. The following is a summary of required deliverables:

Note: The applicable CLP Forms can be used to report the information below as long as they include, at a minimum, all items listed in i, ii, iii, and iv.

i. QC Summary

1. Lab Control Sample/Lab Control sample Duplicate Recovery Summary Form

2. Method Blank Summary Form

3. GC/MS Instrument Performance Check, List all associated samples

4. Internal Standard Area, RT and Recovery Summary Form List all associated samples including standards and LCS/LCSD

ii. Sample Data

1. T0-15 Results – Volatile Analysis Data Summary Form (Form 1)

2. For each sample, blank and LCS/LCSD:

a. Reconstruction total ion chromatograms (RIC)

b. Quantitation reports

c. Raw spectra, background-subtracted mass spectra and reference spectra of target compounds identified

iii. Standards Data (All Instruments)

Initial and Continuing Calibration Verification (CCV) Data RIC and Quantitation reports for all standards (mass spectra not required)

iv. Raw/Quality (QC) Data

1. BFB

2. Blank Data

3. LCS/LCSD Data

4. Leak Test Data Table

5. Clean Canister Verification Documentation

H. Electronic (EDD) Reporting Requirements

1. Electronic data shall be submitted in the Modified Region 2 Electronic

Data Deliverables (EDD) format. See attached documentation for EDD requirements.

2. Preliminary results should be provided in electronic EDD format and sent to:

Region 2:

Jennifer Feranda at Feranda.jennifer@epa.gov;

Kim Brandon-Bazile at Brandon-Bazile.kim@epa.gov Agustin Aoanan at Aoanan.agustin@epa.gov Cheng-Chang Chen at Cheng-Chang.Chen@epa.gov

Region 3:

Jay Burman at Burman.jarmael@epa.gov

3. Preliminary results shall be provided within 7 -14 calendar days from the Verified Time of Sample Receipt (VTSR) of the last sample in an SDG (see section C above) as specified in each individual call order.

4. Hard Copies of the data and EDDs s shall be provided in the time frames specified in Section H above.

5. A CD with both the PDF data package and EDD shall be provided with the submission of the hard copy data package.

mailto:Brandon-Bazile.kim@epa.gov mailto:Aoanan.agustin@epa.gov mailto:Burman.jarmael@epa.gov

Attachment # 1

REGION 2 DELIVERY OF ANALYTICAL SERVICES (DAS)

SAMPLE DELIVERY GROUP (SDG)

COVER SHEET

Laboratory Name: ________________________ Laboratory Code: _________________

Regional Case No.: ________________________

SDG No./First Sample in SDG: ____________ Sample Receipt Date: _______________ (Lowest EPA Sample Number in first shipment MM/DD/YYYY received under SDG.)

Last Sample in SDG: ___________ Sample Receipt Date: _______________ (Highest EPA Sample Number in last shipment MM/DD/YYYY of samples received under SDG.)

EPA Sample Numbers in the SDG (List in alphanumeric order):

1. _________________________________ 11. _______________________________

2. _________________________________ 12. _______________________________

3. _________________________________ 13. ______________________________

4. _________________________________ 14. _______________________________

5. _________________________________ 15. _______________________________

6. _________________________________ 16. _______________________________

7. _________________________________ 17. _______________________________

8. _________________________________ 18. _______________________________

9. _________________________________ 19. _______________________________

10. ________________________________ 20. _______________________________

Note: There are a maximum of 20 field samples in an SDG.

Comments: ___________________________________________________________________________________

Signature Title

Print Name Date

Please make copies of this form and complete one form per SDG. E-mail the completed form within 3 days of receipt of the last sample received for each SDG to:

Jennifer Feranda, TO-15 COR: Feranda.jennifer@epa.gov Kim Brandon-Bazile, TO-15 Alternate COR: Brandon-bazile.kim@epa.gov