# Deviation Description Corrective Action/Necessary Change Reference Laboratory Response DOW Response Laboratory Response 1 The requested method for TSS, EPA 160.2, is not currently approved by the EPA to be used for wastewater compliance. Method must be in accordance with 40 CFR 136. KY DOW has inserted SM 2540 D-1997 as the method for TSS on the laboratory’s list. Please confirm which approved method the laboratory will be using and update documents accordingly. Note: SM 2540 D-2011 (SM 22nd Ed.) is also approved as a test method for TSS. 40 CFR 136.3 WWCM1 Chapter II Section 10 Acceptable. Update TSS SOP to include year of SM committee approval for the specific version of the method in use (SM 2540 D-1997). Document will be reviewed at time of on-site audit. N/A
2 The requested method for pH, EPA 150.2, is not consistent with the method detailed in the laboratory’s SOP (PROC.052.001). EPA 150.2 is an automated procedure. EPA 150.1 is the electrode method similar to the method described in the SOP. However, EPA 150.1 is not currently approved by the EPA to be used for wastewater compliance. Method must be in accordance with 40 CFR 136. KY DOW has inserted SM 4500 H+ B-2000 as the method for TSS on the laboratory’s list. Please confirm which approved method the laboratory will be using and update documents accordingly. Note: SM 4500 H+ B-2011 (SM 22nd Ed.) is also approved as a test method for pH. 40 CFR 136.3 WWCM1 Chapter II Section 10 Acceptable. Update pH SOP to include year of SM committee approval for the specific version of the method in use (SM 4500 H+ B-2000). Document will be reviewed at time of on-site audit. N/A
3 QAP: Appendix D includes methods the lab is utilizing outside of the scope of the certification request. QAP does not include list of SOPs and the effective dates. Several documents are referenced that were not submitted to KY DOW. Table 25.1 does not include the methods which the laboratory is seeking certification for. Control charting is not described in the QAP. Revise Appendix D to specify which methods are to be used for wastewater compliance samples (for KPDES permits). Include list of relevant SOPs and the effective date of each. Submit the following to KY DOW: PROC.001.015, PROC.001.016, PROC.001.031, PROC.001.032, PROC.001.033. Update Table 25.1 to include information for TSS, oil and grease, and pH. QAP needs to describe the use of control charts (or other trend analyses of quality control results) to monitor for trends and ensure acceptance criteria are met. Controls charts are to include all of the relevant results, not just the passing results. WWCM1 Chapter II Sections 3.3, 3.4, 3.6, 3.7 KWLCP App2 Section 8 Acceptable. Revise QAP to include the updated method references (Standard Methods rather than EPA methods). Document will be reviewed at time of on-site audit. N/A
4 SOPs: Effective dates on SOPs are prior to the approval dates. TSS SOP has not been signed (approved) by the lab director (Eric Cole). pH SOP only references the instrument manual, does not include review/revision history sheet, and only 3 of 7 pages were submitted. SOPs must be approved by the appropriate personnel prior to becoming effective. Revise pH SOP accordingly (method reference, revision sheet) and resubmit in its entirety to KY DOW. WWCM1 Chapter II Section 3.3 Acceptable. N/A 5 MDLs and DOCs: The instrument ID is not recorded for DOC or MDL studies. QAP does not specify frequency of MDL study. Record instrument ID for each DOC and MDL study. QAP needs to specify that MDL study must be performed annually. 40 CFR 136, Appendix B WWCM1 Chapter III Sections 7.1.1, 7.1.4 Acceptable. N/A
6 QAP states that Advanced TENORM Services does not collect samples. pH and temperature measurements for compliance samples must be obtained within hold time (temperature immediately, pH within 15 minutes of collection). Reported results (i.e., DMR) must be from analyses performed within hold time by personnel of a lab certified to perform the analyses. 40 CFR 136.3 Table II WWCM1 Chapter II Section 10 Acceptable. N/A 7 pH SOP does not include recording of the slope or an acceptance range for the slope. Record pH meter slope monthly, after calibration. Slope shall be between 95% and 105%. WWCM1 Chapter II Section 8.1.5 Acceptable. N/A 8 pH SOP states ± 0.2 pH units as the acceptance range for calibration verification. A pH calibration check solution shall be analyzed and read within ± 0.1 S.U. of the true value. WWCM1 Chapter II Section 8.1.6 SM 4500H+ B-2000 Section 2a Acceptable. N/A
9 pH SOP does not include analysis of duplicate samples or a quarterly quality control sample (QCS). Duplicate analysis of samples shall be performed once per batch of twenty samples, at a minimum. Sample batch may extend beyond one day. Acceptance criteria for duplicates must be specified in QAP and/or SOP (± 20% RPD). A quality control sample (QCS) shall be analyzed at least quarterly. A purchased second source standard (used for 4.3.1.2) that is a primary standard meets this requirement and no additional QCS is needed. WWCM1; Chapter II Sections 4.3.1.4, 4.3.2.1; Chapter III Sections 7.0, 7.3 Acceptable. N/A
Procedure in TSS SOP does not meet requirements of SM 2540 D. Minimum residue not specified. Filter rinsed once with 10ml ultra-pure water. Filtration for 1-2 minutes post-rinse. Filter desiccation and weighing repeated, but drying not repeated. Acceptance criteria for duplicates is 20% RPD. Choose a sample volume to yield between 2.5 and 200 mg of dried residue. The filter must be washed 3 times with 10mL successive washes. After filtration of sample and washings is complete, analyst shall continue suction for 3 minutes. Analyst must repeat cycle of drying, cooling, desiccating, and weighing samples until the weight change is less than 4% of the previous weight or 0.5 mg, whichever is less. Acceptable duplicate must be within 5% of the average weight of the sample and sample duplicate. SM 2540 D-2011 Section 3c Acceptable. N/A
Laboratory’s MRL for TSS is set at 2mg/L. Laboratory’s determination of the MRL must meet method requirement to process sufficient sample volume (up to 1L) to yield a minimum residue of 2.5 mg. If the laboratory continues using a sample volume of 500 mL, the laboratory’s MRL must be raised to 5 mg/L. MRL has been listed on list by KY DOW as 5mg/L. SM 2540 D-2011; Section 3b Acceptable. N/A Oil and grease SOP does not include balance calibration verification after each analytical batch. Verify calibration of the balance (per Section 10 of the method) before and after each analytical batch. If calibration is not verified after measurement of the analytical batch, recalibrate the balance and reweigh the batch. EPA 1664 Rev. A Section 9.5 Unacceptable. Sections 9.1 and 9.2 do address verification of balance calibration but do not specify that this must be done before and after each analytical batch. Added verbage to indicate that calibration shall be perfomed on balance before and after each analytical batch.