BPM004422 Solicitation Scope of Work Exhibits.pdf

EXHIBITS TO THE SCOPE OF WORK

Exhibit 1 - 0154.000 Addressing Spike and Surrogate Recovery as They Relate to Matrix Effects in Water, Air, Sludge and Soil Matrices Policy

Exhibit 2 - 0170.000 Implementation of EPA Method 5035 - Soil Preparation for EPA Methods 8015B, 8021B and 8260B

Exhibit 3 - Arizona Data Qualifiers – Revision 4.0

Exhibit 4 - ADEQ Temperature/Preservation Guidance Policy

Exhibit 5 – Evaluation of Contractor Performance

Exhibit 1

0154.000 ADDRESSING SPIKE AND SURROGATE RECOVERY AS THEY RELATE TO MATRIX

EFFECTS IN WATER, AIR, SLUDGE AND SOIL MATRICES POLICY

Level One Arizona Department of Environmental Quality

Originator: Kenyon C. Carlson, Manager

Quality Assurance/Quality Control (QA\QC) Unit

Issue Date: October 23, 1998

PURPOSE

The Arizona Department of Health Services (ADHS) has not established a comprehensive policy on the issue of matrix spike or surrogate recoveries because they do not have the authority to establish criteria by which ADEQ will either accept or reject data.

This policy will assure that all data submitted to ADEQ meets regulatory requirements and are legally defensible by establishing alternative criteria for when the established method recovery acceptance criteria for matrix spikes and/or surrogates are exceeded.

ADEQ is concerned with the assumption that if spike and/or surrogate recoveries exceed method acceptance criteria and that if those results can be duplicated without re-extracting the sample, the failure of that quality control criteria is a result of matrix effects. Duplication of out-of-range results can be the result of influences other than matrix effects and could be indicative of the method or instrument being out-of-control.

The ADEQ QA/QC Unit believes a more accurate and reliable assessment of possible matrix effects can be established using either a (1) dilution technique, (2) the method of standard additions, or (3) analyzing a laboratory fortified blank (LFB) or a laboratory control sample (LCS). Because ADEQ is a regulatory agency, compliance results must be able to meet all legal constraints and uphold all analytical method requirements.

AUTHORITY

A.A.C. R18-4-106 and R9-14-608.

DEFINITIONS

Data: For the purposes of this policy, data is defined as ‘raw data’ (examples include but are not limited to calibration curves, chromatograms, spectras, sample preparation and injection logs etc.) and does not include laboratory reports.

(Contact the QA unit for further information.)

Laboratory Fortified Blank (LFB): (aka blank spike)An aliquot of organic free reagent water to which known quantities of the method analytes are added in the laboratory. The LFB is analyzed exactly like a sample, and its purpose is to determine whether the methodology (analytical process) is in control, and whether the laboratory is capable of making accurate and precise measurements at the required method detection limit.

Laboratory Fortified Blank Duplicate (LFBD): (aka blank spike duplicate) A duplicate sample of the aliquot of reagent water to which known quantities of the method analytes are added in the laboratory. The LFBD is analyzed exactly like a sample, and its purpose is to determine whether the methodology (analytical process) is in control, and whether the laboratory is capable of making accurate and precise measurements at the required method detection limit.

Laboratory Control Sample (LCS): A sample of clean dirt or sand to which known quantities of the method analytes are added in the laboratory. The LCS is extracted and analyzed exactly like a sample, and its purpose is to determine whether the methodology (sample preparation and analytical process) is in control, and whether the laboratory is capable of making accurate and precise measurements at the required method detection limit.

Laboratory Control Sample Duplicate (LCSD): A duplicate sample of clean dirt or sand to which known quantities of the method analytes are added in the laboratory. The LCSD is extracted and analyzed exactly like a sample, and its purpose is to determine whether the methodology (sample preparation and analytical process) is in control, and whether the laboratory is capable of making accurate and precise measurements at the required method detection limit.

Laboratory Fortified Sample Matrix (LFM): (aka matrix spike) An aliquot of an environmental sample to which known quantities of the method analytes are added in the laboratory. The LFM is analyzed exactly like a sample, and its purpose is to determine whether the sample matrix contributes bias to the analytical results and therefore determines to what degree the method is successful in analyzing the target analytes. The background concentrations of the analytes in the sample matrix must be determined in a separate aliquot and the measured values in the LFM corrected for background concentrations.

Laboratory Fortified Sample Matrix Duplicate (LFMD): (aka matrix spike duplicate) A duplicate sample of the aliquot of an environmental sample to which known quantities of the method analytes are added in the laboratory. The LFMD is analyzed exactly like a sample, and its purpose is to determine whether the sample matrix contributes bias to the analytical results and therefore determines to what degree the method is successful in analyzing the target analytes. The background concentrations of the analytes in the sample matrix must be determined in a separate aliquot and the measured values in the LFMD corrected for background concentrations.

Matrix: The predominant material, component or substrate which contains the analyte of interest. Matrix is not necessarily synonymous with phase (liquid or solid).

Matrix Interference: Also referred to as matrix effects. Matrix spike interference are those chemical and/or physical interferences that impede the analytical instrumentation in detecting the true value concentration of a target analyte within a sample. One possible source of matrix interferences may be caused by contaminants that are co-extracted from the sample and result in a positive or negative bias. The extent of matrix interferences will vary considerably from source to source, depending upon the nature and diversity of the sample matrix.

Method of Standard Additions: A technique used most commonly in metals analysis by atomic absorption; however, it can be applied in many areas of the laboratory. It serves to correct for matrix effects in the sample. Aliquots of a sample are spiked with at least three different concentrations of a standard.

Surrogate: A pure analyte, which is extremely unlikely to be found in any sample, and which is added to a sample aliquot in known amounts before extraction and is measured with the same procedures used to measure other sample components. A surrogate behaves similarly to the target analyte and its use is most often used with organic analytical procedures. The purpose of a surrogate analyte is to monitor method performance with each sample.

POLICY

ADEQ will not accept test results for regulatory purposes when the LFM and/or surrogate recovery exceed the acceptance criteria unless the laboratory has demonstrated that the sample itself is responsible for the QC results exceeding the methods acceptance criteria.

RESPONSIBILITY

The ADEQ Program staff will be responsible for reviewing the final report or the quality control summary sheets which accompany the final results of the laboratory analysis to verify that matrix spikes and/or surrogate recoveries were within the acceptance criteria. If the program staff are uncertain as to how to evaluate the final report, or if required information is missing, it shall be the responsibility of the program staff to forward the information to the ADEQ QA/QC Unit for review and recommendations.

The ADEQ QA/QC Unit will review data referred by program staff to ensure that the procedures outlined in Attachment A of this policy were followed by the laboratory and to report their findings to the appropriate ADEQ program staff.

APPLICABILITY

This policy is applicable to all types of water, air, sludge, and soil matrices regardless of the method of analysis.

PROCEDURES

The ADEQ program staff shall review the final report or the quality control (QC) summary sheet which accompanies the final report. ADEQ program staff shall assess the results of the LFM and LFMB on the QC Summary sheet to determine if the recoveries are within the acceptance range. If the LFM or LFMB results exceed the established recovery criteria, ADEQ program staff will assess the recovery criteria for those out of range analytes in either the LFB/LFBD or LCS/LCSD. If the required information is not included with the final report or program staff are uncertain as how to evaluate the final report, they shall notify the QA/QC Unit so the QA/QC staff can perform a more thorough evaluation of the results.

The ADEQ QA/QC staff, if necessary, shall request a laboratory data package to review the raw data, determine the validity of the results and compliance with the ADEQ data reporting policy. The QA/QC Unit shall also submit in writing, to the program staff, the data validation findings and the ADEQ QA/QC Unit’s recommendations.

ATTACHMENT A (PART of EXHIBIT 1)

LABORATORY PROCEDURES

The ADEQ policy for addressing spike and surrogate recovery as they relate to matrix effects in water, air, sludge and soil matrices suggests three different techniques (analysis of an LFB/LFBD or LCS/LCSD pair, dilution procedure, or the standard additions technique) which may adequately explain the out-of-range QC results of samples. These three techniques do not represent an all inclusive list for demonstrating matrix effects within a sample and laboratories may have alternate and valid techniques to demonstrate matrix interference. These alternate techniques should be discussed with and approved by the ADEQ QA Unit prior to analysis to avoid the rejection of data.

ADEQ also requires the analyses of either an LFB/LFBD, LCS/LCSD or LFM/LFMD pair to satisfy the precision requirements for drinking water methods. More useful information can be obtained regarding precision when comparing samples containing target analytes. Very little useful precision information is obtained when comparing the instrument precision using two samples that are non detect. Whenever included in the analytical batch, the laboratory must report the results of the LFB/LFBD or LCS/LCSD in addition to the LFM/LFMD to ADEQ and shall include the numerical values established by the laboratory for the QC acceptance criteria whenever the method has not provided any.

While the method would require a re-extraction of that sample, to confirm matrix interference, if the LFM and/or the LFMB fall outside the method's acceptance criteria, ADEQ will accept the results of the LFB/LFBD or LCS/LCSD which demonstrate that the analytical process is in control. The LFB/LFBD and LCS/LCSD provide an interference free matrix such that if the surrogates and/or matrix spike analytes are within the method's acceptance criteria, then there is compelling data that an instrument is operating properly, the extraction procedure provided no bias, and the method is in control. The LFB/LFBD must be analyzed with the same batch as the LFM/LFMD for ADEQ to accept the LFB/LFBD results. The LCS/LCSD samples must be extracted and analyzed with the same batch as the LFM/LFMD samples for ADEQ to accept the results of the LCS/LCSD samples. The laboratory shall include the numerical values established by the laboratory for the QC acceptance criteria whenever the method has not provided any.

Another option is the dilution technique. The dilution technique is particularly well suited for demonstrating matrix effects in the LFM samples for analyses that don't require extraction procedures. Laboratories performing analytical work for ADEQ that suspect matrix interference in LFM samples may dilute that sample such that all suspected matrix effects are diluted out as well prior to spiking. Once the matrix effects have been diluted out, recovery of the matrix spikes and surrogates should fall within the acceptable recovery criteria established by the method, or the lab if none are given in the method. The dilution of samples suspected of having matrix interference such that interference is no longer a factor strongly suggests that there may have been matrix effects in the sample and the recovery of the spiked analytes within the acceptance range demonstrates the instrumentation and method are in control. ADEQ will accept use of the dilution technique to demonstrate matrix effects in LFM and LFMD samples because not every sample is matrix spiked and it cannot be assumed that the matrix effects observed in one sample are representative of the entire sample batch.

Because the dilution technique raises the reporting level of an analyte, it may not be a suitable technique to demonstrate matrix interference if the resulting reporting level exceeds the regulatory (trigger) or action level. The method of standard additions would be a preferred technique to help correct for positive or negative bias in the samples because this technique is unlikely to raise the reporting level of regulated contaminants that may be present in the sample. The method of standard additions usually employs aliquots of a digested or extracted sample which are spiked with at least three different concentrations of a standard. The standard additions are chosen to bracket the unknown sample concentration and the response of the instrument must be linear.

Those samples whose matrix spikes or surrogate recoveries continue to fall outside the acceptance criteria after any of the above three techniques, or an alternate method pre-approved by the ADEQ QA Unit have been employed, shall be reviewed by ADEQ on a case-by-case basis. Any results reported which are affected by matrix interference shall be lagged as an estimated quantitation.

Exhibit 2

0170.000 IMPLEMENTATION OF EPA METHOD 5035 - SOIL PREPARATION FOR

EPA METHODS 8015B, 8021B AND 8260B.

LEVEL TWO Arizona Department of Environmental Quality

Originator: David Esposito, Director

ADEQ Waste Programs Division

Issue Date: April 19, 2000

Next Scheduled Review Date: 2 years from issuance

Authority: Arizona Revised Statutes (A.R.S.) §49-104(A)

I. PURPOSE

The EPA Office of Solid Waste promulgated Method 5035, Closed- System Purge-and-Trap Extraction for Volatile Organics in Soil and Waste Samples (Attachment 1), in June 1997 in SW-846, Update III. The Arizona Department of Health Services (ADHS) Office of Laboratory Licensure, Certification and Training adopted Method 5035 in May 1998 and Method 5035 became enforceable on March 1, 1999 in Arizona. The collection and analytical procedures for the approved method are flexible and, without further guidance, could result in multiple interpretations.

This policy establishes the sampling options and the preservation holding time requirements for individual programs within the ADEQ’s Waste Programs Division. This policy is necessary to provide an understanding of the options set forth by the method and the limitations imposed on specific field sampling requirements. This policy does not eliminate the need to read and understand EPA Method 5035. The method, in conjunction with this policy, will provide a technically defensible and consistent approach to sampling for Volatile Organic Compounds (VOCs) in soils.

II. DEFINITIONS: (FOR PURPOSES OF EPA METHOD 5035 ONLY) -

1. Sample Preservation: The addition of methanol or sodium bisulfate to an unpreserved sample in the field or in the laboratory.

2. Sample Extraction: The addition of methanol to an unpreserved sample in the laboratory. After extraction, the methanol is transferred to a vial and can be stored at 4ºC (+ 2ºC) until analysis.

3. Hermetically Sealed: For the purposes of this policy a hermetically sealed container shall be defined as a sample storage device that consistently shows less than 10% loss from volatilization over the intended storage holding time (usually 14 days) or a minimum of 48 hours for the compounds of concern at a given site.

4. Sample Freezing: A preservation technique in which the sample is frozen and stored at 0ºC (32ºF), or lower upon receipt at the laboratory.

Blue ice is unacceptable.

5. Calcareous Soil: A soil whose content of carbonate is sufficient to cause effervescence when tested with hydrochloric acid.

(Reference: Bates R. L. and Jackson J. A.. (1987).

Glossary of Geology. (3rd ed.)

Alexandria: American Geological Institute.)

III. POLICY

Method 5035 is structured as a 2-tier approach for low and high concentration sampling0F

1. Preservation is recommended

1Refer to EPA Method 5035 (Attachment 1) and Regional Interim for both low and high contaminant concentrations as stated in the Method. Based upon program requirements, preservation can be conducted in the field or subsampled in an EnCore Sampler and the sample preserved in accordance with sample handling.

A. Sample collection options for low reporting limits (<200 μg/kg):

I. Methanol Preservation-

EPA has permitted the use of methanol preservation for low level analysis if the target analyte(s) can be quantitated below 200μg/kg. As a result, laboratories must demonstrate their ability to detect below 200 μg/kg to the client and ADHS. Samples preserved in the field with methanol using a 40 ml glass VOA vial with a plastic screw cap and a Teflon septa must be analyzed within 14 days from the time of sample collection.

ii. EnCore Sampler-

Policy for Determination of Volatile Organic Compound (VOC) Concentrations in Soil and Solid Matrices, June 23, 1999 (Attachment 2).

The sample can be collected using either a 5-gram or 25-gram EnCore Sampler. The sample must be stored at 4ºC (±2ºC) and preserved or extracted within 48 hours if not preserved. Approved preservatives include either methanol or sodium bisulfate. Once preserved, the sample must be analyzed within 14 days from the time of sample collection. The EnCore Sampler 48-hour preservation hold time as required in the method applies only to the EnCore Sampler option and is based on manufacturers’ studies. Freezing the unpreserved sample in the EnCore Sampling device can extend the holding time up to seven days (e.g., 48 hours unfrozen and 5 days frozen.)

iii. Sodium Bisulfate Preservation-

Samples preserved in the field with sodium bisulfate must be analyzed 14 days from the time of sample collection. This technique should be used if detection limits in the range of 2 - 5 μg/kg are desired.

Calcareous samples, however, may effervesce upon contact with the sodium bisulfate preservative solution (thereby liberating the volatile gases) and compromise the integrity of the sample. In these instances, sodium bisulfate preservative solution cannot be utilized to attain the lower reporting levels and one of three alternative sample collection methods must be employed.

a) The sample can be collected in a VOA vial containing 10 ml of reagent grade water, sealed with a plastic screw cap containing a Teflon septa and stored at 4ºC (±2ºC.) This sample must be analyzed within 48 hours from the time of sampling using a closed system purge and trap.

b) The sample can be collected in a dry VOA vial, sealed with a plastic screw cap containing a Teflon septa and stored at 4ºC (±2ºC.) Once at the lab, water must be introduced through the septa and analyzed by closed purge and trap within 48 hours from the time of sample collection. Freezing the unpreserved sample can extend the holding time an additional 5 days for a total of 7 days from the time of sample collection.

c) The sample can be collected in an EnCore Sampler, stored at 4ºC (±2ºC) and analyzed within 48 hours from the time of sample collection. Freezing the unpreserved sample can extend the holding time up to seven days.

iv. Bulk Sampling-

The rationale for the collection of bulk samples must be clearly documented and approved by the appropriate program in a work or sampling plan or other written communication with ADEQ. If samples are not preserved in the field, the reasons for not preserving must be clearly documented and approved by the relevant program.

ADHS rules require laboratories to flag data generated from samples that have not been preserved in the field or have not been collected in recommended containers if the reporting levels are below 200 μg/kg.

B. Sample collection options for high reporting limits (>200μg/kg):

I. Methanol Preservation-

This technique may be used if the reporting limits are above 200 μg/kg. Samples preserved in the field with methanol using a 40 ml glass VOA vial with a plastic screw cap and a Teflon septa must be analyzed within 14 days from the time of sample collection.

ii. EnCore Sampler-

The sample can be collected using an EnCore Sampler. Methanol must be added within the 48-hour period immediately following sample collection.

The EnCore Sampler 48-hour preservation hold time as required in the method is applicable specifically only to the EnCore subcoring device and is based on the manufacturers’ studies. After collection the sample must be stored on ice at 4ºC (±2ºC) until analyzed. Freezing the unpreserved sample in the EnCore Sampling device can extend the holding time up to seven days (e.g., 48 hours unfrozen and 5 days frozen.) Once the sample is preserved, it must be analyzed within 14 days from the time of sample collection.

iii. Bulk Sampling-

The rationale for collection of bulk samples must be clearly documented and approved by the appropriate program in a work or sampling plan or other written communication with ADEQ. If samples are not preserved in the field or subsampled in EnCoreTM Samplers, the reasons for not preserving must be clearly documented and approved by the relevant program.

Significant volatile loss occurs when samples are collected in glass jars and transported to a laboratory for analysis1F

2. Therefore, glass jars with Teflon -lined lids containing no

2Siegrist, R.L., and P.D. Jennsen, 1990. Evaluation of Sampling Method Effects of Volatile Organic Compound Measurements in Contaminated Soil, Environmental Science and Technology, Vol.24, pp. 1387-1392.

preservative ARE NOT ACCEPTABLE for the collection of soil for VOC analysis, unless otherwise specified in this policy (Program Specific Requirements) or prior approval has been received from the relevant program.

III. Program Specific Requirements2F

3:

1. WQARF, Hazardous Waste Compliance, Solid Waste Programs

3For specific programs, a sample collected in a brass/steel sleeve is acceptable under the conditions noted in Section IV. The brass or steel sleeves must have each end covered with a sheet of Teflon, aluminum foil (aluminum is optional, but preferred) and sealed with a plastic cap. The plastic caps must be secured and the capped sleeve should be placed in a plastic ziplock bag which is then taped to ensure the caps are secure. The use of tape to bind the cap to the end of the sleeve is discouraged. The length of time a sample can be held in this container is finite and subject to specific program requirements set forth in Section V.

When utilizing the field preservation option of the 5035 method, samples must be preserved immediately after collection with minimal handling to be considered reliable compliance samples. Samples maybe collected and held on ice at 4ºC (±2ºC) for a maximum of 2 hours before preserving or analyzing the sample. This option of holding samples on ice for up to 2 hours is accepted, but not encouraged, due to the known volatile loss over time.

Samples collected and preserved or analyzed after 2 hours will be considered bulk samples and not suitable for compliance purposes. Data generated from samples collected and transported to a laboratory in this manner has limited compliance value and may not be accepted by the above referenced programs.

2. Hazardous Waste Inspections and Emergency Response

Programs

For planned field sampling events, samples must be preserved immediately after collection, with minimal handling, to be considered compliance samples. The sample may be held on ice at 4ºC (±2ºC) for a maximum of 2 hours before preserving or analyzing the sample.

For unanticipated sampling events, where significant difficulties exist for preserving samples onsite, bulk soil samples may be collected and stored at 4ºC (±2ºC) but must be preserved within 72 hours with the approval of the program.

3. UST Program

When site-specific sampling conditions prevent the use of appropriate sample collection and preservation techniques as defined in Section I or Section II, samples may be submitted in properly sealed brass sleeve containers maintained at 4ºC (±2ºC) for laboratory analysis of VOCs. The laboratory must document sample holding time and flag the associated analytical results if sample preservation or extraction exceeds 48 hours, regardless of the reporting limit.

Reasons for lack of field preservation within the 48 hour period and submittal of bulk samples for laboratory analysis must be clearly documented.

IV. Quality Control for unpreserved samples:

Unpreserved samples submitted to the laboratory should have matrix spikes and surrogates added directly to an aliquot of the sample before extraction. The laboratory should be requested to provide a narrative describing the procedures for sample spiking and flag all data in which the matrix was not directly spiked prior to extraction.

V. Example of Holding Time Calculations for Frozen

Samples:

Example 1 Sample is placed in a vial without chemical preservative in the field and stored at 4ºC (±2ºC).

The sample must be analyzed within 48 hours of collection.

Example 2 The sample is collected in a hermetically sealed subcoring and storage device in the field, stored at 4ºC (±2ºC) and transferred into a vial without chemical preservative in the laboratory.

The sample must be analyzed within 48 hours of collection.

Example 3 The sample is collected in a hermetically sealed sub-coring and storage device, transported/stored at 4ºC (±2ºC), frozen at the laboratory 18 hours after collection, thawed (at ambient temperature) after 4 days and transferred into a vial without a chemical preservative in the laboratory.

The sample must be analyzed within 30 hours from the time the sample is defrosted to 4ºC (±2ºC).

48 hours allowed before analysis - 18 hours before freezing = 30 hours allowed from thawing (at ambient temperature) to analysis.

Freezing can only extend the holding times for unpreserved samples. Freezing is an alternative to preserving samples in the field. Freezing can never extend the holding times of samples beyond the analytical methods required holding time. (Ex. Freezing cannot extend the holding time from 14 days to 19 days).

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SERVICES\SOLICITATION\EXHIBITS\EXHIBIT 2.DOC April 20, 2000 9

VI. RESPONSIBILITY

All staff in the respective Waste Programs Division programs are responsible for knowledge and implementation of this policy. Supervisors are responsible for ensuring that the information contained in this policy is consistently and equitably applied by all staff. It is the responsibility of the sampler to inform the laboratory receiving personnel which program requirements are appropriate for the sample.

APPROVED BY:

The Policy Review Committee has posted, reviewed and accepted this policy by motion as of April 19, 2000.

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Exhibit 3

Arizona Data Qualifiers

Revision 4.0 9/5/12

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Arizona Data Qualifiers Revision 4.0

9/5/12

Developed by the Sub-committee of the Arizona Environmental Laboratory Advisory Committee This is an updated list of the Rev. 3.0 Arizona Data Qualifiers dated 9/20/2007, with some new qualifiers added, some obsolete ones deleted and some modified. The new qualifiers are designated in red font. If there was a minor modification to the existing qualifier, it has been highlighted in blue.

Using the following Arizona Data Qualifiers does not automatically denote acceptability to the Regulatory Agency. Arizona Department of Environmental Quality expects that data reported utilizing the following qualifiers, unless stated otherwise, is useable, scientifically valid and defensible. In the laboratory’s judgment if the data should not be used for compliance, the T6 qualifier must be used. Other general guidelines for use and application of the following data qualifiers can be found as an attachment to this document

(ATTACHMENT A).

Note: Please note that as of 10/28/08, AZ Drinking Water Data Qualifiers have been discontinued, please use Arizona Data Qualifiers Revision 4.0 dated 9/5/12.

Microbiology:

A1 = Too numerous to count.

A2 = Sample incubation period exceeded method requirement.

A3 = Sample incubation period was shorter than method requirement.

A4 = Target organism detected in associated method blank.

A5 = Incubator/water bath temperature was outside method requirements.

A6 = Target organism not detected in associated positive control.

A7 = Micro sample received without adequate headspace.

A8 = Plate count was outside the method’s reporting range. Reported value is estimated.

Method/calibration/Trip blank:

B1 = Target analyte detected in method blank at or above the method reporting limit.

B2 = Non-target analyte detected in method blank and sample, producing interference.

B3 = Target analyte detected in calibration blank at or above the method reporting limit.

B4 = Target analyte detected in blank at or above method acceptance criteria.

B5 = Target analyte detected in method blank at or above the method reporting limit, but below trigger level or MCL.

B6 = Target analyte detected in calibration blank at or above the method reporting limit, but below trigger level or MCL.

B7 = Target analyte detected in method blank at or above method reporting limit.

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Concentration found in the sample was 10 times above the concentration found in the method blank.

B8 = Analyte found in both the travel blank and sample.

Confirmation:

C1 = Confirmatory analysis not performed as required by the method.

C2 = deleted C3 = Qualitative confirmation performed.

C4 = Confirmatory analysis was past holding time.

C5 = Confirmatory analysis was past holding time. Original result not confirmed.

C6 = deleted C7 = deleted C8 = Sample RPD between the primary and confirmatory analysis exceeded 40%. Per EPA Method 8000C, the lower value was reported as there was no evidence of chromatographic problems.

Dilution:

D1 = Sample required dilution due to matrix.

D2 = Sample required dilution due to high concentration of target analyte.

D3 = deleted.

D4 = Minimum Reporting Limit (MRL) adjusted to reflect sample amount received and analyzed.

D5 = Minimum Reporting Limit (MRL) adjusted due to sample dilution; analyte was nondetect in the sample.

D6 = Minimum Reporting Limit (MRL) adjusted due to an automatic 10X dilution performed on this sample for the purpose of reporting traditional drinking water analytes for wastewater requirements.

D7= Minimum Reporting Limit adjusted to reflect sample dilution.

Estimated concentration:

E1 = Concentration estimated. Analyte exceeded calibration range. Reanalysis not possible due to insufficient sample.

E2 = Concentration estimated. Analyte exceeded calibration range. Reanalysis not performed due to sample matrix.

E3 = Concentration estimated. Analyte exceeded calibration range. Reanalysis not performed due to holding time requirements.

E4 = Concentration estimated. Analyte was detected below laboratory minimum reporting limit (MRL) but above MDL.

E5 = Concentration estimated. Analyte was detected below laboratory minimum reporting limit (MRL), but not confirmed by alternate analysis.

E6 = Concentration estimated. Internal standard recoveries did not meet method acceptance criteria.

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E7 = Concentration estimated. Internal standard recoveries did not meet laboratory acceptance criteria.

E8 = Analyte reported to MDL per project specification. Target analyte was not detected in the sample.

Hold time:

H1 = Sample analysis performed past holding time.

H2 = Initial analysis within holding time. Reanalysis for the required dilution was past holding time.

H3 = Sample was received and/ or analysis requested past holding time.

H4 = Sample was extracted past required extraction holding time, but analyzed within analysis holding time.

H5 = This test is specified to be performed in the field within 15 minutes of sampling;

sample was received and analyzed past the regulatory holding time.

H6 = The filtration was not done within the required 15 minutes of sampling, the sample was filtered in the laboratory.

BOD/CBOD:

K1 = The sample dilutions set-up for the BOD/CBOD analysis did not meet the oxygen depletion criteria of at least 2 mg/L. Any reported result is an estimated value.

K2 = The sample dilutions set up for the BOD/CBOD analysis did not meet the criteria of a residual dissolved oxygen of at least 1 mg/L. Any reported result is an estimated value.

K3 = deleted.

K4 = deleted.

K5 = The dilution water D.O. depletion was > 0.2 mg/L.

K6 = Glucose/glutamic acid BOD/CBOD was below method acceptance criteria.

K7 = A discrepancy between the BOD and COD results has been verified by reanalysis of the sample for COD.

K8 = Glucose/glutamic acid BOD/CBOD was above method acceptance levels.

K9=Test replicates show more than 30% difference between high and low values.

K10=Seed control samples do not deplete at least 2.0 mg/L, with a retention of at least 1.0 mg/L DO criteria in all samples.

K11=Minimum DO is less than 1.0 mg/L in all dilutions.

Laboratory fortified blank/blank spike:

L1 = The associated blank spike recovery was above laboratory acceptance limits L2 = The associated blank spike recovery was below laboratory acceptance limits.

L3 = The associated blank spike recovery was above method acceptance limits.

L4 = The associated blank spike recovery was below method acceptance limits.

L5 = The associated blank spike recovery was above laboratory/method acceptance limits.

This analyte was not detected in the sample.

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Matrix spike:

M1 = Matrix spike recovery was high; the associated blank spike recovery was acceptable.

M2 = Matrix spike recovery was low; the associated blank spike recovery was acceptable.

M3 = The spike recovery value is unusable since the analyte concentration in the sample is disproportionate to the spike level. The associated blank spike recovery was acceptable.

M4 = The analysis of the spiked sample required a dilution such that the spike recovery calculation does not provide useful information. The associated blank spike recovery was acceptable.

M5 = Analyte concentration was determined by the method of standard addition (MSA).

M6 = Matrix spike recovery was high. Data reported per ADEQ policy 0154.000. Matrix Interference was confirmed.

M7 = Matrix spike recovery was low. Data reported per ADEQ policy 0154.000. Matrix Interference was confirmed.

General:

N1 = See case narrative.

N2 = See corrective action report.

N3 = deleted.

N4 = The Minimum Reporting Limit (MRL) verification check did not meet the laboratory acceptance limit.

N5 = The Minimum Reporting Limit (MRL) verification check did not meet the method acceptance limit.

N6 = Data suspect due to quality control failure, reported per data user’s request.

N7= Additional analysis was not performed based on the “Total” result which was below the requested analyte’s MCL/Action level/Trigger level.

Sample quality:

Q1 = Sample integrity was not maintained. See case narrative.

Q2 = Sample received with head space.

Q3 = Sample received with improper chemical preservation.

Q4 = Sample received and analyzed without chemical preservation.

Q5 = Sample received with inadequate chemical preservation, but preserved by the laboratory.

Q6 = Sample was received above recommended temperature.

Q7 = Sample inadequately dechlorinated.

Q8 = Insufficient sample received to meet method QC requirements. Batch QC requirements satisfy ADEQ policy 0154.000.

Q9 = Insufficient sample received to meet method QC requirements.

Q10 = Sample received in inappropriate sample container.

Q11 = Sample is heterogeneous. Sample homogeneity could not be readily achieved using routine laboratory practices.

Duplicates:

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R1 = RPD/RSD exceeded the method acceptance limit. See case narrative.

R2 = RPD/RSD exceeded the laboratory acceptance limit. See case narrative.

R3 = deleted.

R4 = MS/MSD RPD exceeded the method acceptance limit. Recovery met acceptance criteria.

R5 = MS/MSD RPD exceeded the laboratory acceptance limit. Recovery met acceptance criteria.

R6 = LFB/LFBD RPD exceeded the method acceptance limit. Recovery met acceptance criteria.

R7 = LFB/LFBD RPD exceeded the laboratory acceptance limit. Recovery met acceptance criteria.

R8 = Sample RPD exceeded the method acceptance limit.

R9 = Sample RPD exceeded the laboratory acceptance limit.

R10 = deleted.

R11 = The RPD calculation for MS/MSD does not provide useful information due to the varying sample weights when Encore samplers/methanol field preserved samples are used.

R12 - RPD/RSD exceeded the method acceptance limit. Result less than 5 times the PQL.

R13 = MS/MSD RPD exceeded method acceptance limit. Matrix spike recovery was outside acceptance criteria. Batch precision and accuracy were demonstrated.

Surrogate:

S1 = Surrogate recovery was above laboratory acceptance limits, but within method acceptance limits.

S2 = deleted.

S3 = Surrogate recovery was above laboratory acceptance limits, but within method acceptance limits. No target analytes were detected in the sample.

S4 = Surrogate recovery was above laboratory and method acceptance limits. No target analytes were detected in the sample.

S5 = Surrogate recovery was below laboratory acceptance limits, but within method acceptance limits.

S6 = Surrogate recovery was below laboratory and method acceptance limits. Reextraction and/or reanalysis confirms low recovery caused by matrix effect.

S7 = Surrogate recovery was below laboratory and method acceptance limits. Unable to confirm matrix effect.

S8 = The analysis of the sample required a dilution such that the surrogate recovery calculation does not provide useful information. The associated blank spike recovery was acceptable.

S9 = deleted.

S10 = Surrogate recovery was above laboratory and method acceptance limits. See case narrative.

S11 = Surrogate recovery was high. Data reported per ADEQ policy 0154.000.

S12 = Surrogate recovery was low. Data reported per ADEQ policy 0154.000.

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Method/analyte discrepancies:

T1 = Method approved by EPA, but not yet licensed by ADHS.

T2 = Cited ADHS licensed method does not contain this analyte as part of method compound list.

T3 = Method not promulgated either by EPA or ADHS.

T4 = Tentatively identified compound. Concentration is estimated and based on the closest internal standard.

T5 = Laboratory not licensed for this parameter.

T6 = The reported result cannot be used for compliance purposes.

T7 = Incubator/Oven temperatures were not monitored as required during all days of use.

T8= Method used not listed in 40 CFR 136; alternate method chosen as acceptable per permit.

T9 = Less than the prescribed sample amount was available to perform the leachate extraction. The volume of extraction fluid was adjusted proportionately based on the method prescribed ratio of extraction fluid to sample weight.

Calibration verification:

V1 = CCV recovery was above method acceptance limits. This target analyte was not detected in the sample.

V2 = CCV recovery was above method acceptance limits. This target analyte was detected in the sample. The sample could not be reanalyzed due to insufficient sample.

V3 = CCV recovery was above method acceptance limits. This target analyte was detected in the sample, but the sample was not reanalyzed. See case narrative.

V4 = deleted.

V5 = CCV recovery after a group of samples was above acceptance limits. This target analyte was not detected in the sample; acceptable per EPA Method 8000C.

V6 = Data reported from one-point calibration criteria.

V7 = deleted.

V8 = deleted.

V9 = CCV recovery was below method acceptance limits.

Calibration:

W1= deleted.

W2= deleted.

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ATTACHMENT A

“Guidance on the Usage of Data Qualifiers”

These standardized data qualifiers are for use in qualifying analytical results for compliance samples in Arizona to represent events that occurred during analysis.

The technical subcommittee has endeavored to develop qualifiers that are succinct and narrow in scope to eliminate broad or multiple interpretations when assessing the impact on data. It must also be noted that due to the specialized nature of the individual qualifiers, it is likely that more than one qualifier may be needed in order to accurately represent the data.

Note: 1. Using the Arizona Data Qualifiers does not automatically denote acceptability to the

Regulatory Agency.

2. As specified in the Arizona Adopted Rules, R9-14-615.C.9, for each parameter tested at the laboratory for which quality control acceptance criteria are not specified in the approved method or by EPA or ADEQ,:

a. Use default limits provided in Exhibit II; or

b. Statistically develop limits from historical data

The laboratory has an option of using ADHS Default Limits which can be accessed at http://www.azdhs.gov/lab/license/tech/altdefaultlimit.pdf

Microbiology:

None.

Method/calibration blank:

Apply appropriate qualifier to affected analyte in the blank if target analyte is not detected at > RL in the samples. If analytes are detected, then all corresponding analytes for the associated samples should also be qualified.

Confirmation:

For methods that require qualitative confirmation. C3 applies to methods that require quantitative confirmation.

Dilution:

If all analytes are reported from the diluted sample, apply qualifier to the entire sample.

Otherwise apply qualifier to each analyte that required dilution.

Estimated concentration:

Appropriate qualifier must be used for any analyte result reported outside the calibration range. Affects data reported outside the calibration range or down to the MDL. E8 is only required if additional clarification is necessary.

http://www.azdhs.gov/lab/license/tech/altdefaultlimit.pdf

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Hold time:

Qualify samples appropriately when method extraction and/ or analysis holding time have been exceeded.

BOD/CBOD:

Qualifiers K5, K6, & K8 indicate situations that may impact all results in an analytical run and should be used to qualify all affected samples as well as any affected quality control samples when reported. K3 was deleted because if the seed depletion was out, then the situation must be explained in the case narrative. Criteria for qualifiers K9, K10, K11 taken from Standard Methods 5210 B, 2001 Revision.

Laboratory fortified blank/blank spike:

Appropriate qualifier must be applied to the affected analytes in the Laboratory fortified blank/blank spike and to all corresponding analytes in the associated samples.

Matrix spike:

Appropriate qualifier must be applied to the affected analytes in the matrix spike and should also be added to all corresponding analytes in the associated spiked sample. If a batch spike recovery is outside of the acceptable range, it is permissible to only flag the sample that was spiked and not the other samples in the batch. As required in the Arizona Adopted Rules A.A.C. R9-14-617.8.d, clients must always be informed if the batch QC result is unacceptable whether one of their samples was spiked or not. The laboratory can choose how the unacceptable QC is reported to the client (e.g., cover letter or flag).

The ADEQ policy 0154.000 can be accessed at http://www.azdeq.gov/function/programs/download/spike8.pdf

General:

For example, qualifier N7 refers to total cyanide vs. free or amendable cyanide, total nitrate/nitrite vs. nitrite, total metals vs. TCLP metals, total PCB’s vs. individual aroclors, and total chromium vs. hexavalent chromium.

Sample quality:

Flag samples with appropriate qualifier when sample quality may be potentially impacted or when method requirements were not met.

The ADEQ policy 0154.000 can be accessed at http://www.azdeq.gov/function/programs/download/spike8.pdf

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Duplicates:

For use with sample, matrix spike, LFB and LFB/blank spike duplicates. Qualify all affected analytes. For MS/MSD or sample duplicates qualify only the original source sample.

Surrogate:

Qualify surrogates appropriately when they do not meet criteria. Surrogate failures in quality control samples will most likely require additional narration. S11 & S12 are used to qualify sample surrogates and only in cases where the Laboratory Fortified Blank/ blank spike has acceptable surrogate recoveries.

Method/analyte discrepancies:

For use with methods or analytes that are not currently approved under the Environmental Laboratory Licensure Rules or for which the lab is not licensed.

Calibration verification:

Appropriate qualifier must be applied to all affected analytes in any samples associated with the calibration verification.

Calibration:

None.

Exhibit 4

ARIZONA DEPARTMENT OF ENVIRONMENTAL

QUALITY

DATE: January 24, 2002

ADEQ TEMPERATURE/PRESERVATION GUIDANCE POLICY

To help assure the validity and documentation of data generated for use by ADEQ, the QA Unit requires that the elements listed below be fulfilled. If the requirements listed below are not fulfilled, the data may be considered unacceptable for compliance or enforcement purposes.

Temperature Documentation Requirements

The documentation of the presence of "wet" ice with samples is not a substitute for measuring temperature. At a minimum, the temperature of a temperature blank must be recorded for each cooler upon sample receipt. The preferred procedure for documenting sample temperature is to record the temperature on the chain of custody.

It is, however, recommended that the temperature of each sample be recorded upon sample receipt. The measurement of a temperature blank is not required if each sample temperature is documented.

The sole use of "blue" ice is strongly discouraged for use by laboratories generating data that will be submitted to ADEQ. "If 'blue' ice is used, it should be frozen at the time of sampling, the sample should be chilled before packing, and special notice must be taken at sample receipt to be certain the required temperature (4C) has been maintained." Manual for the Certification of Laboratories Analyzing Drinking Water, page IV-3, section 6.2.

There must be documentation substantiating that 1he "blue" ice was frozen at the time of sampling and that the sample was chilled before packing.

The QA Unit acknowledges that all samples may not have time to equilibrate to 4 +2°C due to an insufficient time between sample collection and sample submittal to the laboratory.

The rejection of data in these situations will not be automatic. Each of these occurrences will be evaluated on an individual basis to determine if a good faith effort has been made to maintain the samples at the required temperatures.

Chemical Preservation Requirements

All pH adjustments performed by the laboratory must be recorded.

The pH of a sample must be recorded by the laboratory either upon receipt or before analysis, as appropriate to the specific method. Recording the pH of a sample may be documented on the chain of custody or some other appropriate form.

In lieu of a laboratory verifying that a sample has been preserved to the appropriate pH in the field, written documentation such as a laboratory copy of a sampler's field notes also provides adequate documentation of proper preservation.

Exhibit 5 Evaluation of Contractor Performance (Page 1 of 2)

Arizona Department of Environmental Quality

1110 W. Washington Street Phoenix, Arizona 85007

Description: Environmental Laboratory Contractor Performance Items

This Form is to be filled out on an annual basis for each Contract year.

Contract/Purchase Order #: Name of Contract/Description:

Contractor Name: Contractor Address:

Date of Evaluation: Contract Year:

Attach separate sheet for comments if necessary.

1. Re-run Request Frequency (Contract Section 16.4)

Did Contractor exceed the 2 % threshold in any of the evaluation periods in re-runs requested by sample submitters for any analyte when considered per analyte per program?

Yes NO

If “Yes”, what was the percentage of unique analytes exceeding the 2% threshold relative to the total of unique analytes requested in the evaluation periods?

If “Yes”, what was the percentage of individual sample tests per analyte beyond the threshold relative to the total of individual tests grouped by analyte requested in the evaluation periods?

If “Yes”, what was the total cost credited back to the agency for these re-runs?

Were any mutual investigative inquiries launched to determine the origin of QAQC problems causing re-run requests during the evaluation periods?

Yes NO

If “Yes”, were any laboratory corrective actions documented as a result of investigative inquiries?

Yes NA NO

If corrective actions were documented, were any additional re-run requests for the pertinent documented process/action logged in the evaluation periods?

Yes NA NO

Was the laboratory required to credit or refund the originally-invoiced cost of any test due to re-runs not meeting Agency criteria for acceptable agreement after corrective actions were documented?

Yes NA NO

Comments:

2. Timeliness of Result Reporting (Contract Sections 7.1, 12.1) Did Contractor meet all routine turn around times (TATs) in the evaluation periods? Yes NO If “NO”, what was the percentage of jobs or invoices requiring a 25% discount due to lateness?

If “NO”, what was the percentage of jobs or invoices requiring a 50% discount due to lateness?

Was the Contractor required to waive any Rush charges due to Rush TATs not being met? Yes NO

Exhibit 5 Evaluation of Contractor Performance (Page 2 of 2)

Arizona Department of Environmental Quality

1110 W. Washington Street Phoenix, Arizona 85007

Description: Environmental Laboratory Contractor Performance Items

3. Electronic Data Interchange (EDI) Capability/Compliance (Contract Section 13.5)

Did the Contractor supply electronic data in standardized formats for all jobs where requested to do so?

Yes NO NA

If “NO”, what was…