Lab certification Terri Zick to: Christopher Lambesis, Todd Ramaly 01/05/2009 02:30 PM

From:
To: Terri Zick <tzick@cticompanies.com >

Christopher Lambesis/R5/USEPA/US@EPA, Todd Ramaly/R5/USEPA/USOEPA

GentlemenAttached, please find the certification of lab data that we discussed during our most recent phone conference regarding Owosso Graphic Arts delisting petition. Please call with questions, otherwise I look forward to speaking with you on 1/13/08.

Teri Zick 313-300-7401

The information contained in this electronic message is privileged and/or confidential information intended only for the use of the individual or entity na detiver ve. If the reader of this message is not the intended recipient, or the employee or agent responsible to deliver it to the intended recipient, you are hereby notified that any dissemination, distribution or copying immediatety munication is neither allowed nor intended. If you have received this communication in error, please immediately notify us by return e-mail or by calling 800-CTI-TODAY and delete tRamaly/R5/USEPA/US@EPADecember 31, 2008

Mr. Christopher Lambesis US Environmental Protection. Agency Region V 77 West. Jackson Boulevard Mail Code LR-8J Chicago, IL 60604-3507

Re: Delisting Petition; Waste Water Treatment Sludge Owosso Graphic Arts, Owosso, Michigan

Dear Mr. Lambesis,

In accordance with your request on December 16, 2008, CTI and Associates has prepared the attached text summary of the Quality Assurance / Quality Control information provided to you on July 29, 2008. Please do not hesitate to contact me at any time should questions arise, or if additional information is deemed necessary during your review. We look forward to discussing the final details of the petition with you on January 13, 2009.

Sincerely, CTI & Associates, Inc.

Terr i L. Zick, CHMM Director of Compliance Services

Cc: Mr. Todd Ramaly, USEPA Ms, Kathy Wilson, Owosso Graphic Arts

Geotechnical, Environmental & Construction Materials Engineers

www.cti-assoc.comOWOSSO GRAPHIC ARTS DE-LISTING PETITION 

### Data Qualification and Certification Summary

Sample ID: 36660-1 Sample Date: 7/26104

With the following exceptions, the analytical data for the filter cake sample collected on 7/26/04 was within acceptable limits based on standard laboratory quality control:

1) The matrix spike (MS) / matrix spike duplicate (MSD) results for the following organic analytes fell below the laboratory's established control limits.

Compound MS/MSD Recovery Lower Limit Upper Limit

Bromornethane 22 76

-- .._ Chloroethane 29 96 Acrolein 7 65 — Carbon Disulfide 62 65
.... Hexachlorocyclopentadiene I4 45
.... Isobutanol 64 65

__ Iodomethane 48 65 -- 2-Acetylaminoflourene 67 70 -- Phenacetin 69 70
....
Since the result of organic sample analysis was less than the reporting limits for these compounds, CTI concurs with the laboratory assessment that no qualification of the dataBromomethane.

2) The mix spike (MS) / matrix spike duplicate (MSD) results for the following organic analytes were grater than the laboratory's established control limits.

Compound MS/MSD Recovery Lower Limit Upper Limit

1,3-Dichlorobenzene 115 114 1,2- Dichlorobenzene 121

-- 115 Vinyl Chloride 113 -- 106 Acenapthylene 121 ..... 112 Anthracene 127 .... 118 Bis (2-Chioroethyl) Ether 117 -- 116 4- Bromophenyl Phenylether 126 -- 113 Di-n-Butylphthalate 138 -- 126 Diethylphthalate 127 -- 119Dimethylphthlate 129 .... 116

Flourene

_ _ -- 112 Hexachlorobenzene 127 -- 113 Hexachlorobutadiene 124
..... 112 Isophorone 118 -- 112 Phenathrene 125

on.. 116 Phenol 121

_ .1 118 1,2,4-Trichlorobenzene 120 .... 112 2-Methylnapthalene 127 .... 122 Dibenzofuran 127 .... 114 1,2-Dibromo-3-chloropropane 207 -- 130

Since the result of organic sample analysis was less than the reporting limits for these compounds, CTI concurs with the laboratory assessment that no qualification of the data is necessary.

3) The MS/MSD recoveries for Zinc were reported as 0, however, this data is not considered to require qualification due to the fact that the unspiked sample concentration exceeded the spike concentration by more than a factor of four.

4) The Laboratory Control Sample (LCS) or Laboratory Fortified Blank (LFB) was above the laboratory generated control limits for the following compounds:

Compound LCS/LFB Recovery Lower Limit Upper Limit

Arochlor 1260 159

.. 138 2-Methylnapthalene 119 ..... 116 Acetone 143 -- , 130

These compounds were not detected in the filter cake sample. Therefore, qualification of the analytical resuls for these compounds is not required.

5) The LCS or LFB recovery was below the laboratory generated control limit for the following compounds:

Compound MS/MSD Recovery Lower Limit Upper Limit



### Acrolein 28 70 -- Carbon Disulfide 61 70 11111111121111111 Iodomethane 67 70 1111111.111111 d2-Na pihthl lamine 76 80 111111111111 Isobutanol 66 70 ----IIIIIIEIIMIII

These compounds were not detected in the filter cake sample. Therefore, CTI concurs with the laboratory conclusion hthlythe analytical results for thesSample ID: 36660-2

Sample Date: 8/16/04

Without exceptions, the analytical data for the filter cake sample collected on 8/16/04 was within acceptable limits based on standard laboratory quality control.

Sample ID: 36660-3 Sample Date: 12/15/04

With the following exceptions, the analytical data for the filter cake sample collected on 12/15/04 was within acceptable limits based on standard laboratory quality control:

1) The MS / MSD results for the following analyses fell outside of the control limits established by the laboratory.



### Compound MS/MSD Recovery Lower Limit Upper Limit

• Cyanide 17 80
.... Sulfide 0 1 -- Copper 179
...... 134 Zinc 0 39 --
Method specified measures were taken to reduce or eliminate interference in the cyanide and sulfide analyses. However, MS/MSD results sample results remained out of control limits.

One surrogate recovery was below the lower control limit in the MSD. Since the unspiked sample, MS and the RPD between the MS and MSD were in control, data qualification is not necessary.

The sample results for Copper and Zinc are not considered qualified since the unspiked sample concentration exceeded the spike concentration by greater than a factor of four.

2) The LCS or LFB recovery for Antimony was 126% which was above the laboratory generated control limit of 123% . Antimony was not detected in the filter cake sample. CTI concurs with the laboratory that qualification of the analytical results for antimony is not required.



### Sample ID: 36660-4 Sample Date: 1/17/05

With the following exceptions, the analytical data for the filter cake sample collected on 1/17/05 wa within acceptable limits based on standard laboratory quality control:Owosso Graphic Arts De-Listing Petition
1) The MS / MSD results for the following analytes fell outside of the control limits established by the laboratory.

Compound MS/MSD Recovery Lower Limit Upper Limit

Cyanide 74 80
.... Copper 364 / 305
.... 134 Zinc 0' 39 --
Method specified measures were taken to reduce or eliminate interference in the cyanide analysis. However, the MS/MSD sample results remained outside of control limits.

The sample results for Copper and Zinc are not considered qualified since the unspiked sample concentration exceeded the spike concentration by greater than a factor of four.

Sample ID: 36660-5 Sample Date: 2/7/05

With the following exceptions, the analytical data for the filter cake sample collected on 2/7/05 was within acceptable limits based on standard laboratory quality control:

1) The MS / MSD results for the following analytes fell outside of the control limits established by the laboratory.

Compound MS/MSD Recovery Lower Limit Upper Limit

C snide 193 -- 120 Copper 55 58
..... Antimony 52 / 53 70

....
Method specified measures were taken to reduce or eliminate interference in the cyanide analysis. However, the MS/MSD sample results remained outside of the control limits.

The sample result for Copper is not considered qualified since the unspiked sample concentration, exceeded the spike concentration by greater than a factor of four.

Antimony was not detected in the filter cake sample. Therefore, the analytical result for antimony is not qualified.Owosso Graphic Arts De-Listing Petition
Sample ID: 36660-6 Sample Date: 2/16/05

With the following exceptions, the analytical data for the filter cake sample collected on 2/16/05 was within acceptable limits based on standard laboratory quality control:

1) The MS / MSD results for the following analytes fell outside of the control limits established by the laboratory.

Compound MS/MSD Recovery Lower Limit Upper Limit

Cyanide 8 / 133 80 120 Antimony 69 70 --

_ Copper 0 58
.... Zinc 1 / 156 39 149

Method specified measures were taken to reduce or eliminate interference in the cyanide analysis. However, the MS/MSD sample results remained outside of the control limits. The relative percent difference (RPD) between the MS and MSD is greater than 20, therefore the results are considered to be estimated.

The sample results for Copper and Zinc are not considered qualified since the unspiked sample concentration exceeded the spike concentration by greater than a factor of four.

Antimony was not detected in the filter cake sample. Therefore, the analytical result for antimony is not qualified.

Sample ID: 36660-7 Sample Date: 3/8/05

With the following exceptions, the analytical data for the filter cake sample collected on 3/8/05 was within acceptable limits based on standard laboratory quality control:

1) The MS/MSD results for the following analytes fell below the control limits established by the laboratory.

Compound S/MSD Recovery Lower Limit Upper Limit



## Bromomethane 71 76 11111111111111 Copper 0 / 16 58

.... Antimon 50 / 60 70 -- Lead ( • ost digestion) 74 75 -- Zinc 0 39Owosso Graphic Arts De-Listing Petition
Method specified measures were taken to reduce or eliminate interference in the cyanide analysis. However, the MS/MSD sample results remained out of control.

The sample results for Copper and Zinc are not considered qualified as the unspiked sample concentrations exceed the spike concentration by greater than a factor of four for each sample respectively.

Antimony was not detected in the filter cake sample. Therefore, the analytical result for antimony is not qualified.

The post-digestion spike for the lead analysis was below the lower control limit, and CTI concurs that the result is considered to be estimated.

Sample ID: Sample Date: 11/15/07

The analytical report for the filter cake sample collected on 11/15/07 identified the following variances from standard laboratory quality control:

1) The laboratory reported no recovery for each of the spiked compounds in the LFB. However,, the MS and MSD spike recovery were within the laboratory specified limits, with the exception. of 2-Hexanone.

2) 2-Hexanone recovery was reported above the laboratory established upper control limit. The precision between the MS and MSD was <20%, the sample result for this compound is not qualified.

Sample ID: 28162-001 Sample Date: 4/1.1/08

With the following exceptions, the analytical data for the filter cake sample collected on 4/11/08 was within acceptable limits based on standard laboratory quality control:

1) The reported LCS recovery for the batch containing the sample is above the laboratory generated control' limits for the following compounds:

Compound LCS Recovery Lower Limit Upper Limit

Tetrachloroethylene 144 -- 141 Vinyl Chloride 209 -- 188

These compounds were not detected in the filter cake sample. Therefore, qualification of the analytical results for these compounds is not required.

2) The MS/MSD results for the following analytes fell outside of the control limits established by the' laboratory.Carbon Tetrachl Dibromoflouromethane 2-Hexanone 81 -- 71

3) The surrogates Dibromoflourornethane and Toluene d-8 failed low in the filter cake sample. However, the surrogates failed high in the LCS. The analytical result must be qualified as the surrogates appear out of the established control limits and must be considered estimated.

4) The trip blank and filter cake samples were run in two separate QA/QC batches. The MS/MSD recovery for Dibromochloromethane was lower than the lower control limit for the batch associated with the trip blank. No detectable VOC compounds were detected in the trip blank.

Sample ID: 28358-001 Sample Date: 4/22/08

With the following exceptions, the analytical data for the filter cake sample collected on

. 4/22/08 was within acceptable limits based on standard laboratory quality control:

1) The reported MS result for 1,1-Dichloroethene is below the laboratory established control limits. The precision between the MS and MSD is < 20%. The sample result for 1,1-Dichloroethene is not considered an estimate.

2) The reported MS/MSD results for 2-Hexanone are above the laboratory established upper control limit. 2-Hexanone was not detected in the filter cake sample, this sample result is not considered qualified.

Sample ID: 28653-001 Sample Date: 5/7/08

With the following exceptions, the analytical data for the filter cake sample collected on 5/7/08 was within acceptable limits based on standard laboratory quality control:

1) For the analytical batch containing the sample, no surrogate or spike recovery was reported from analysis of the MS. 2) The MSD surrogate recovery was greater than the laboratory established upper control limit for the three surrogate compounds. 3) Surrogate recovery was within the laboratory established limits for the filter cake sample. 4) No results were reported for the MS. The laboratory reported an instrument issue which prevented the analysis of the MS.Owosso Graphic Arts De-Listing Petition

The sample results for this filter cake sample are qualified. The quality assurance sample results for this batch are generally outside of the control limits and must be considered to be estimated.



### Conclusion

1 have reviewed the sample result and quality control information provided by Trimatrix and Fibertec using generally accepted industry criteria. Based on my review of the information provided by the laboratories, I certify that the analytical data was reported in accordance with accepted industry practices and, except for the limitations outlined above, the sample data appears to adequately represent the material sampled.

Philip Riley Terri. Zick Field Services Director of Compliance Services