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 

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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@EPA 
December 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. 

Terri 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.com 
OWOSSO 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 -- 119 
Dimethylphthlate 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 thes 
Sample 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 39 
Owosso 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