Mr. Herstowski

January 20, 2001 John Deere

1097 Highway 101 South, Suite D16, Greer, SC 29651 (864) 334-5085, sales@pintegration.com 

### March 21, 2011

Mr. Kenneth Herstowski Environmental Protection Agency
901 North Fifth Street Kansas City, Kansas 66101 Phone (913) 551-7631



### RE: John Deere, Des Moines IA Delisting of F006 Sludge Filter Cake

Dear Mr. Herstowski:

Enclosed, please find three copies each of the Samp ling and Analysis Plan (SAP) and Quality Assurance Project Plan (QAPP) for Delisting of F006 Sludge Filter Cake for your review and comment. Th e documents include the plan for sampling as we discussed along with inform ation from the laboratory, TestAmerica. Please contact us with an y questions that you any questions that you may have as you review the docum ents and we will quickly respond to your requests. As we discussed, we are planning to being sampling in mid-summer, pending your review and app roval of the plans. Also, please let us know when you would like to con duct a site visit to review the process as we will be happy provide you a tour.

Again, please feel free to contact us with any ques tions as we look forward to working with you to complete this project.

Sincerely,

David L. Kirby

Project Integration, Inc. Sr. Project Manager

cc: Robert P. Stevens, P.E., Project Integration1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 1 September 8, 2011



### Mr. Kenneth Herstowski Environmental Protection Agency
901 North Fifth Street Kansas City, Kansas 66101 Phone (913) 551-7631

RE: John Deere, Des Moines IA Delisting Petition

Dear Mr. Herstowski:

The John Deere Sampling and Analysis Plan was appro ved by EPA on July 7, 2011. The first effort under the Plan was the collection and testing of an initial filter cake sample. That work has been completed and this letter forwards the laboratory r esults. In addition this letter summarizes key results and presents our recommendation for the con tinued sampling and analysis events. We anticipate addressing any questions you may have on our recommendations and then continuing the testing work in accordance with your approval.

Initial Sampling Event

The sampling was completed July 20, 2011, with no d eviations from the sampling procedures. Work was completed by MWH Consulting and the samples wer e shipped to the Test America Chicago, Illinois laboratory for analysis.

Laboratory Test Results

Test America, in Chicago, Illinois is an Iowa certi fied laboratory. A complete report with Level II
detail is included with this letter. If desired, a dditional detail on laboratory procedures and quali ty systems during the time of this testing is availabl e (the report is 1000 pages, so electronic version is recommended, if needed).

A detailed comparison of the planned testing and th e actual is included in Table 1 attached to this letter. The major observations and our interpretat ion of significance are listed below by constituent
category.

Additionally, the attached tables provide the same information in a tabular format without the detailed analysis. The tables are the same tables and table numbers as were provided in the SAP to

allow for consistent review. The attached tables a lso include two (2) new columns. The first new column provides a conclusion statement on each chem ical and the second column identifies whetherMr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 2 the chemical is presently planned for further sampl ing or if it has been eliminated from continued sampling.

Herbicide (Table 3.1), Pesticide (Table 3.2) and PC Bs (Table 3.3)

All results for these sets of chemicals were less t han the reporting limit (RL) although the RL was elevated versus the Expected Quantitation Level due to the complexity of the sludge matrix (see pages 3, 4, 5 of the Data Report for additional dis cussions).

Conclusions: These results confirm the expected absence of thes e constituents in the sludge

cake.

Recommendation: Herbicides, pesticides, and PCBs should not be req uired for subsequent samples.

Total Semi-volatile (Table 3.4)

Most of the results for the total semi-volatile sam pling were less than the reporting limit (RL) although the RL was elevated versus the Expected Qu antitation Level due to the complexity of the sludge matrix (see pages 3, 4, 5 of the Data Report for additional discussions).

The exceptions are listed and discussed below:

Eight constituents were detected in the sludge tota l analysis with the data qualifier, “J”. A “J” result is less than the RL but greater than or equa l to the MDL and the concentration is an approximation”

Constituents with the J qualifier include: Benzo(a)anthracene; Benzo(a)pyrene; Benzo(b)fluora nthene; Benzo(ghi)perylene; Benzo(k)fluoranthene; Chrysene; Dibenzo(a,h)anthrac en; and Indeno(1,2,3-cd)pyrene.

Conclusions: The results, both the non-detect and the “J” quali fied, confirm the expected absence of these constituents in the sludge cake.

Recommendation : Total semi-volatile organic chemicals should not be required for subsequent samples.

TCLP Extract Semi-volatile (Table 3.4.1)

All of the TCLP extract results are less than the R L.

Conclusions: These results confirm the expected absence of thes e constituents in the sludge
cake.Mr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 3 Recommendation : TCLP extract semi-volatile organic chemicals shou ld not be required for subsequent samples.

Total Volatile Organic Constituents (Table 3.5)

Most total results were less than the reporting lim it (RL) although the RL was elevated versus the Expected Quantitation Level due to the complexity o f the sludge matrix (see pages 3, 4, 5 of the Data Report for additional discussions).

Exceptions to the above are listed and discussed be low:

There were two constituents detected: Acetone 6.67 mg/kg (RL 0.188 mg/kg) 2-Butanone (methyl ethyl ketone) 0.0588 mg/kg (RL 0 .0188 mg/kg)

There was an additional constituent Chloroform dete cted in the sludge total analysis with the “J” data qualifier as discussed above:

Conclusions : These results indicate that only Acetone and 2-Bu tanone were present in the sludge.

Recommendation: Further testing should include the volatile organ ic chemicals, Acetone
and 2-Butanone.

TCLP Extract Volatile Organic Constituents (Table 3 .5.1)

TCLP extract results all are less than the RL.

Conclusions: These results confirm the expected absence of thes e constituents in the sludge
cake.

Recommendation : TCLP extract volatile organic chemicals should no t be required for subsequent samples.

Total Metals (Table 3.6)

Results for the total metals analysis indicate abse nce of the following constituents:

Antimony, arsenic*, beryllium, cadmium*, cobalt (J qualifier), selenium*, silver*, thallium, and tin (J qualifier).

Conclusion: The metals listed above were not found in quantif iable levels and should not be included in the subsequent tests.Mr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 4 Recommendation: Because they are present in the sludge, include t he following metals for total analysis in the subsequent testing: barium*, chromium*, copper, lead*, nickel, vanadium, and zinc.

TCLP Extract Metals (Table 3.6.1)

Results for the TCLP extract metals included only c opper and nickel at levels greater than the Reporting Limit. The following constituents had th e J qualifier: barium, vanadium, and zinc.

Conclusions: Each constituents absent in the sludge total anal ysis also was absent in the
TCLP extract.

Recommendation: Continue testing the TCLP extract for the metals in the sludge as follows:

Barium, chromium, copper, lead, nickel, zinc, and v anadium

Total Mercury (Table 3.7)

Results for the total mercury sampling demonstrated mercury at levels greater than the Reporting

Limit.

Conclusion: The results indicate that there is small but quan tifiable amounts of mercury in the sample.

Recommendation: Testing should include mercury going forward.

TCLP Extract Mercury (Table 3.7.1)

Results for TCLP Extract Mercury sampling found TCL P Extract Mercury as not present.

Conclusion: The results indicate that there was not a quantif iable amount of mercury in the sample.

Recommendation: Continue testing the TCLP extract for mercury bec ause it is present in the sludge.

pH (Table 3.8), Solids (Table 3.9), Solids (Table 3 .10), Oil and Grease (Table 3.11), Hexavalent Chrome (Table 3.12), Sulfides (Table 3.13), Cyanide (Table 3.14), and Flashpoint (Table 3.15)

Results for most of these items did not demonstrate presence with the exception of hexavalent chrome. Total cyanide provided a “J” qualified res ult.

Conclusion: The tests for pH, sulfides, and flashpoint demonst rate the sludge does not
exhibit the characteristic of a hazardous waste. T he tests for solids, and oil and grease areMr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 5 needed to perform the TCLP extraction. These tests will be continued for the testing

program.

The test for hexavalent chrome indicates a low leve l in the sludge.

The test for total cyanide indicates possible prese nce in the sludge (J qualified result).

Recommendation : All of the above tests should be continued in the subsequent testing. Most are required to complete the TCLP sampling. T he hexavalent chrome was noted as present and is also a target constituent and total cyanide, although not found present at a quantifiable level is also a target constituent.

Table 4 Multiple pH Test

Testing included the extraction of the sludge sampl e using the normal TCLP procedure and

alternative extraction fluids:

Target pH 4.93 (regular TCLP test) – extraction flu id Type 1; initial pH 4.55; final pH 6.73

Target pH 7.00 (ASTM method) – extraction fluid Dei onized Water

Target pH 10.01 (ASTM method) – extraction fluid un defined; final pH 10.01

Bench sheets for the extraction are available in th e Level III data report (see pages 945, 946, and 94 7 of 1061 total pages).

Results are summarized in the attached Table 4. Th e results indicate there is no significant differen ce for extract concentrations at the three pH levels. In particular, if the total concentration of the detected constituent is divided by 20 to approximat e the expected liquid concentration at full solubility, the observed concentration indicates a very small level of solubility demonstrated for the sludge (see notes on Table 4).

Conclusion: Sludge cake does not exhibit constituent solubili ty significantly different at the three pH conditions.

Recommendation: Sludge cake disposal in the landfill should be co nsidered acceptable.

Recommendations for Continued Sampling

The Constituents of Concern List for Remaining Samp ling events are proposed to be as identified in

Section 2.3 of the SAP:

• Filter cake will be analyzed for total and extract concentrations of the following metals: barium, chromium, copper, lead, mercury, nickel, zi nc, and vanadium.Mr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 6 • Filter cake will be analyzed for Total Cyanide and Total Hexavalent chromium because of their detection in the initial sample.

• Filter cake will be analyzed for the RCRA hazardous waste characteristics of ignitability, corrosivity, and reactivity.

• Filter cake will be analyzed for oil and grease.

• Filter cake will be analyzed for the total concentr ation of the volatile organic chemicals noted in the initial sample: acetone, 2-butanone

Please confirm that the Final List of Constituents will be satisfactory for completion of this work. After your confirmation, John Deere will immediatel y begin the completion of the remaining sampling to develop the Delisting Petition.

Do not hesitate to call or e-mail with any question s or comments that you have on the sampling results or our recommendations for moving forward w ith the sampling.



### Sincerely,

David L. Kirby Project Integration, Inc.

dlk@pintegration.com ph. 864-334-5085 / cell 864-497-6802

cc: Charles R. Busch, P.E., John Deere Fred Van Schepen, John Deere Robert P. Stevens, P.E., Project Integration

Attachments: Planned Testing Table and Actual Analytic Results T ables Analytical Report, Sludge Filter Cake Delisting, Te stAmerica, 8/04/2011,Mr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 7 

## Attachment A

Planned Testing Table and Actual Analytic Results T ablesMr. Herstowski September 8, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 8 

## Attachment B

Analytical Report, Sludge Filter Cake Delisting, Te stAmerica, 8/04/20111097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 1 October 18, 2011



### Mr. Kenneth Herstowski Environmental Protection Agency
901 North Fifth Street Kansas City, Kansas 66101 Phone (913) 551-7631

RE: John Deere, Ankeny Iowa Delisting Sampling – Chrome Review

Dear Mr. Herstowski:

The John Deere Sampling and Analysis Plan was approved by EPA on July 7, 2011. The first effort under the Plan was the collection and testing of an initial filter cake sample. That work was completed and the laboratory results were submitted for review. The sample results indicated chrome and small amounts of hexavalent chrome in the sample. The levels were well below any threshold quantities. However, the indication raised some question and John Deere committed to reviewing the chrome sampling data and methodology 

### specifically to confirm that the planned testing is sufficient to fully characterize this constituent in the filter cake as needed to confirm the

waste is not hazardous . This letter provides that review and our recommendation for the remainder of the sampling effort.



### Sampling and Analysis Plan Chromium Summary

This information outlines the Chrome testing required in the Delisting Sampling and Analysis
Plan.

a. Testing (page 10):

• All filter cake samples will be analyzed for total and TCLP concentrations of the TC metals (which include arsenic, barium, cadmium, chromium, lead, mercury, selenium, silver; and site metals nickel and zinc).

• Clarification (letter on Sample one results) – testing will include Hexavalent chrome in solid sample

b. Testing (Table 2, Table 3.12): Category: Chromium +6 Reason for Inclusion: Generator knowledge and historical data of filter cake # Samples for Analysis: Initial plus 6 Laboratory Analysis: Total Metals EQL-G Cr6 SolidInstrument: VIS SPECTROMETER
Methods: SW848 7196AMr. Herstowski October 18, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 2 Matrix: Solid Hexavalent Chromium CAS 18540-29-9 EQL 1 mg/kg

c. Testing (Table 2, Table 3.6) Category: Chromium Reason for Inclusion: Generator knowledge and historical data of filter cake # Samples for Analysis: Initial plus 6 Laboratory Analysis: Total EQL-W 2005 ICP Soil Instrument: ICP Methods: SW846 3050B/6010B (Acid Digestion, ICP) Matrix: Solid Chromium CAS 7440-47-3 EQL 1 mg/kg Matrix: Liquid Chromium CAS 7440-47-3 EQL 25 ug/L

d. Testing [Sample one only] (Table 3.12) Category: Multiple pH extraction, then Chromium Reason for Inclusion: Determine impact of pH # Samples for Analysis: Initial only Laboratory Analysis: Same as Liquid Chromium as defined above



### Initial Sample Chrome Test Results

The chromium results from the initial sample for the delisting are listed below:

a. Chromium, total, solid: 9,340 mg/kg
b. Chromium, TCLP, liquid: < 25.0 ug/L

c. Chromium, hexavalent, solid: 6.88 mg/kg
d. Chromium, multiple pH extract, pH 4.93: <25.0 ug/L

e. Chromium, multiple pH extract, pH 7.00: <25.0 ug/L f. Chromium, multiple pH extract, pH 10.01: 19.1 ug/L (J Qualified)



### Sample Results Discussion

The sample results provided the following information:

a. Initial sample results show that the chromium is present as total metal in the filter cake as expected since chrome is present in the wastewater and is removed as a precipitate during treatment
b. Initial sample results show that the chrome is not present in quantifiable amounts in extract from the filter cake as expected since soluble chrome is converted to insoluble chrome during wastewater treatment in a reaction that is not reversible with only exposure to pH adjustment

c. Sample one results show that the test protocol (total chrome, TCLP extract chrome, total hexavalent chrome) is effective in characterizing chromium for the delisting

program d. All chromium and hexavalant chromium levels noted in the initial sample were well below any hazardous thresholdsMr. Herstowski October 18, 2011

Environmental Protection Agency

1097 Highway 101 South, Suite D-16, Greer, SC 29651 P.O. Box 1414 Greer, SC 29652-1414 Phone - 864.334.5085 Fax - 864.334.5143 sales@pintegration.com Page 3 

### Sampling Recommendations

John Deere completed a thorough review of the Sampling and Analysis Plan testing requirements and the results of the initial sample. John Deere feels that the data that will be obtained through the initial sample, in conjunction with the six (6) remaining samples, will provide a thorough assessment of the filter cake’s hazardous capacity.

Based on this review, John Deere proposes to move forward with the remaining six samples using the existing sampling strategy for chromium. If an issue is identified in a sample as we move forward John Deere will review the issue with the EPA and a modification to the sampling strategy will be made, if deemed necessary. Additionally, if the EPA has any specific additions that they would like to see made to the sampling strategy presently, please make John Deere aware and we will be happy to review and discuss this request.

If this letter provides the information required by EPA, John Deere requests that an approval to move forward with the remaining samples is granted. Again, if there is additional sampling that EPA would like to discuss please call or e-mail me so we can discuss and close out any open items.

We appreciate your continued efforts to assist us with this project.



### Sincerely,

David L. Kirby Project Integration, Inc.

dlk@pintegration.com ph. 864-334-5085 / cell 864-497-6802

cc: Charles R. Busch, P.E., John Deere Fred Van Schepen, John Deere Robert P. Stevens, P.E., Project Integration4. 10

- 21

- 2011 EPA Request Chrome Letter E

- mail.docx -------- Original Message

-------- Subject: FW: Chrome Review Letter
From: Busch Charles R < BuschCharlesR@JohnDeere.com > Date: Thu, November 10, 2011 12:41 pm
To: David Kirby < dlk@pintegration.com > Cc: " rstevens@pintegration.com " < rstevens@pintegration.com >

Sorry, I didn't realize they didn't send to you...

Charles R. Busch, P.E.
John Deere Des Moines Works
BuschCharlesR@JohnDeere.com ph. 515

- 289

- 3429 / cell 515

- 537

- 4745

----- Original Message

----- From: Herstowski.Ken@epamail.epa .gov [mailto: Herstowski.Ken@epamail.epa.gov ] Sent: Friday, October 21, 2011 3:03 PM To: Van Schepen Fred A; Busch Charles R Subject: Fw: Chrome Review Letter

Gentlemen

-

Based on the results provided of the initial sludge sample results, I believe it is necessary to include additional hexavalent chromium analysis in the analysis of the remaining sludge samples.

This should be comprised of parallel batch ext raction at pH 4, 7, 10 and 13 consistent with the methodology (including qa/qc procedures) in the preliminary version of Method 1313 and analysis of the extracts using Method 218.6 with a requested detection limit of 0.02 ug/l for hexavalent chromium.

I a m available for discussion next week if necessary.

Ken Herstowski EPA Region 7 AWMD/RCAP
901 N. 5th St. Kansas City, KS 66101
9135517631 9135517947(fax)

----- Forwarded by Ken Herstowski/R7/USEPA/US on 10/21/2011 02:53 PM

-----

From: "David Kirby" < dlk@pintegration.com > To: Ken Herstowski/R7/USEPA/US@EPA Cc: "'Van Schepen Fred A'" < VanSchepenFredrickA@JohnDeere.com >, "'Busch Charles R'" < BuschCharlesR@JohnDeere.com >,

< rstevens@pintegration.com > Date: 10/20/2011 10:33 AM Subject: Chrome Review Letter4. 10

- 21

- 2011 EPA Request Chrome Letter E

- mail.docx Ken,

We have reviewed the chrome testing as you requested. Please review the attached letter and provide us any comments or questions that you may have.

T hanks for all of your assistance and have a good week.

David

David L. Kirby Project Integration, Inc. 1097 Highway 101 South
Suite D16 Greer, SC 29651
P.O. Box 1414 Greer, SC 29652

- 1414
Office

- 864

- 334

- 5085
Fax

- 864

- 334

- 5143 Cell

- 864

- 497

- 6802 dlk@pintegration.com (See attached file: Ankeny Initial Sample chrome reviewltr
10

- 18

- 11.pdf)Mr. Herstowski July 17 , 2012 John Deere

1097 Highway 101 South, Suite D1 6, Greer, SC 29651 (864) 334

- 5085, sales@pintegration.com 

### July 17 , 2012

Mr. Kenneth Herstowski Environmental Protection Agency
901 North Fifth Street Kansas City, Kansas 66101 Phone (913) 551

- 7631



### RE: John Deere, Des Moines IA Delisting of F006/F019 Sludge Filter Cake

Dear Mr. Herstowski :

Enclosed, pleas e find three copies each of the revised Sampling and Analysis Plan (SAP) and Quality Assurance Project Plan (QAPP) for Delisting of
F006 /F019 Slu dge Filter Cake for your review and comment

. As you discussed previously with Fred Van Schepen, we are submitt ing the revision to the SAP and QAPP to cover the addition of F019 waste for delisting. The updated documents are complete with the exception of some appendix
material (site location maps, MSDS, etc.) that was unchanged. That material
can be referenced f rom the initial March 2011 submittal or can be provided, if requested.

There are no required changes to the sampling strategy as the F019 does not require any additional constituents of concern. Since there are no additional constituents, John Deere w ould like to move forward with the sampling with the requested changes from our initial sampling event.

Please contact us with any questions that you may have as you review the documents and we will quickly respond to your requests. If there are no
fur ther comments John Deere would like to restart the sampling as soon as you provide approval to move forward.

Again, please feel free to contact us with any questions as we look forward to working with you to complete this project

.Mr. Herstowski July 17 , 2012 John Deere

1097 Highway 101 South, Suite D1 6, Greer, SC 29651 (864) 334

- 5085, sales@pintegration.com 

### Sincerely,

D avid L. Kirby

Project Integration, Inc. Sr. Project Manager

cc : Robert P. Stevens, P.E., Project Integration Fred Van Schepen, John Deere Charles, Busch, John DeereWaterloo SAP Lab Deviation Ltr 10-16-2012 d1.docxPage 1

October 16, 2012

Mr. Ken Herstowski US EPA Region 7 11201 Renner Boulevard Lenexa, Kansas 66219

RE: John Deere/ Crown Facility, Waterloo IA Delisting Petition

Dear Mr. Herstowski:

The John Deere Sampling and Analysis Plan was appro ved by EPA on September 28, 2012. The SAP included a description of the test constitu ents and quantitation limits for the sludge samples based on the EPA standard protocols.

John Deere has concluded that the analytic work wil l be performed by Test America, in Chicago, Illinois, an Iowa certified laboratory. In working with the laboratory we have
identified small differences between the constituen t as listed in the SAP and the constituents reported for the standard testing procedures at the laboratory. In particular, two Herbicide, four pesticides, and two semi-volatile organic cons tituents listed in the SAP are not reported by Test America.

We believe that the constituents not reported do no t have a negative effect on the results of this work. Therefore, we are requesting that EPA a gree that the constituent list can be slightly modified as outlined below:

Table 3.1 Herbicides:

• We request that the following constituents be remov ed from the SAP:

o MPCA, MCPP

• REASON: these are not part of the usual Herbicide p rotocol for the selected laboratory,

Test America

• REASON: Herbicides are not a chemical used at the C rown facility

• CONCLUSION: excluding these from the Table 3.1 Herb icide list will not reduce the validity of the delisting testing program

Table 3.2 Pesticides:

• We request that the following constituents be remov ed from the SAP:

o 2,4-DDD; 2,4-DDe; Mirex; o-Chlordane; cis-Nonachlor ; Trans-Nonachlor

• REASON: these are not part of the usual Pesticide p rotocol for the selected laboratory,

Test America

• REASON: Pesticides are not a chemical used at the C rown facility

• CONCLUSION: excluding these from the Table 3.2 Pest icide list will not reduce the validity of the delisting testing programWaterloo SAP Lab Deviation Ltr 10-16-2012 d1.docxPage 2

Table 3.4 Semi-volatile Organics

• We request that the following constituents be remov ed from the SAP:

o Methyl methacrylate; Tributylphosphate

• REASON: these are not part of the usual Semi-volati le Organic protocol for the selected laboratory, Test America

• REASON: chemicals with Semi-volatile Organic consti tuents are not used at the Crown facility

• CONCLUSION: excluding these from the Table 3.4 Semi -volatile Organic list will not reduce the validity of the delisting testing progra m

The testing affected by this change is only for the initial sample event. The results from the initial event will be used to identify the final co nstituents of concern. If there is the detection of constituents with properties similar to the chem icals listed above, we will evaluate the need for additional special testing.

A second change is that the “LOQ PQL” limits achiev ed by Test America for some constituents will vary slightly from the levels lis ted in the SAP tables due to differences with the sample matrix and laboratory protocols. The ac tual levels are expected to be consistent with the work for the John Deere Ankeny delisting I nitial Sample Event.

We propose that these changes be incorporated into the SAP during the review of the Initial Sampling Event and changes to the Final Constituent s of Concern list. We believe this approach will be most efficient for all parties.

Please confirm that the removal of the constituents listed above will be acceptable to EPA. Please also confirm that modifying the LOQ PQLs in the SAP as we agree on the Final List of Constituents will be satisfactory for completion of this work. After your confirmation, John Deere will immediately begin the initiation of the Initial Sampling Event.

Do not hesitate to call or e-mail with any question s or comments that you have on the sampling results or our recommendations for moving forward with the sampling.

Sincerely,

David L. Kirby Project Integration, Inc.

dlk@pintegration.com ph. 864-334-5085 / cell 864-497-6802

cc: Michelle Hackett, John Deere Fred Van Schepen, John Deere Robert P. Stevens, P.E., Project Integration1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com

January 22, 2013

Mr. Ken Herstowski US EPA Region 7 11201 Renner Boulevard Lenexa, Kansas 66219

RE: John Deere/ Ankeny Facility, Ankeny IA Delisting Petition – Sampling

Dear Mr. Herstowski:

The sample collection for the John Deere Ankeny fac ility has been completed and we are in the process of completing the review of the Filter Cake sample data. One item has been noted that requires a decision to move forward. The filter cak e Oil and Grease concentrations ranged from 8,910 mg/kg to 21,500 mg/kg. Since this exceeds th e 1% level, the Sampling and Analysis Plan requires testing a sample for the Mobile Metal Cont ent, using the Extraction Procedure for Oily Wastes, Method 1330. Therefore, John Deere propose s to select the sample with the highest Oil and Grease of 21,500mg/kg for this test.

Method 1330 is not a test that is “certified” by Io wa but we have located a laboratory in the state that can perform the test. Their qualification pac kage is available if you wish to review it.

For information, Method 1330 is an extraction that includes:

• separate liquid from the sample and test total meta ls in the liquid (not applicable for this sludge - no liquid)

• extract solid with tetrahydrofuran and test total m etals in the liquid

• extract same solid with toluene and test total meta ls in the liquid

• extract same solid with TCLP and test total metals in the liquid

• calculate the Mobile Metal Content by mass balance

The test does not specifically require measuring 't otal' metal in the original sample. This data has been collected from the testing already complet ed.

The filter cake samples are being held by Test Amer ica for at least 90 days. Method 1330 does not specify a hold time and metals have a long hold time. However, John Deere is very interested in completing this test and moving forwa rd with the completion of the petition.

Please review and provide any comments that you ma y have. Feel free to call and discuss as
well.1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com

Sincerely,

Project Integration, Inc.

dlk@pintegration.com ph. 864-334-5085 / cell 864-497-6802

cc: Charles Busch, John Deere Fred Van Schepen, John Deere Robert P. Stevens, P.E., Project Integration1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com

April 18, 2013

Mr. Ken Herstowski US EPA Region 7 11201 Renner Boulevard Lenexa, Kansas 66219

RE: John Deere/ Ankeny Facility, Ankeny IA Delisting Petition – Filter Cake Sampling Review

Dear Mr. Herstowski:

The detailed sample collection for the John Deere A nkeny facility has been completed. This letter serves to provide an overview analysis of th e sampling data obtained from the delisting sampling effort. This includes the planned testing in the approved Sample and Analysis Plan as well as the additional oil and grease sample testin g noted in the January 22, 2013 letter. The complete laboratory data packages are provided on a CD in Attachment A for more detailed review, as needed.

This overview includes an outline of the testing an d data packages, a discussion of the data quality reports, summary of the testing reports, an d our conclusions from the testing.



## Testing and Data Packages

The detailed sampling included 6 separate sampling events spaced over 4 weeks identified as FC1 through FC6. Each sampling event was collected from filter cake representing a unique batch of treated sludge and is considered an indepe ndent event.

The laboratory data packages for each event have be en included on the CD with two levels of
information:

Level 2 Analytical

• Data quality summary:

• Case narrative addressing sample receipt,

• VOA data qualifiers, metals data qualifiers, genera l chemistry qualifiers

Level 3 Analytical Report - Adds details:

• Laboratory data quality,

• Laboratory method detection limits,

• Laboratory analytical equipment performance

Attached with this report is a Data Summary Table t hat includes the results from the detailed testing along with the data qualifiers for each sam ple event. The table includes:1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com 

### • Summary table with all sample data (but excluding d ata qualifiers, equipment blank; trip blank)

• Results for each event including information:

o data qualifiers,

o equipment blank;

o trip blank;

o duplicates

• Case Narrative table:

o Comments for each event;

o Evaluation of the significance for the comments on data validity



## Data Quality Reports Discussion

Data Quality information (discussions) for the filt er cake samples FC1 through FC6 are provided by the laboratory in the Level 2 Analytical Report as Case Narratives. Each Case Narrative includes information for the following information categories:

(a) Sample receipt conditions; (b) GC/MS VOA results; (c) Metals; and (d) General Chemistry.

Each sample event Case Narrative for each informati on category was reviewed with the following observations:

(a) Sample Receipt conditions:

(1) No issues were reported with temperature of sample as received for any event (2) No issue with hold time except for FC6 sample; due to weather, the hold time for CRr+6 was exceeded; the sample was analyzed and the exceedance is noted

Conclusion : no significant issues with Sample Receipt

(b) GC/MS VOA results:

(1) No issues noted except for acetone and butanone

Acetone: FC1 with MS/MSD recovery outside control l imits; FC2 and FC4 with high levels causing MS/MSD accuracy and precision not ev aluated; FC4 with internal sample response out of limits; and FC5 with one int ernal sample response outside acceptance levels; conclusion is these do not have serious impact on data quality

Butanone: FC1 with MS/MSD recovery outside control limits

Conclusion : no significant Quality Control issues with VOA re sults1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com



### (c) Metals results:

(1) No issues for samples FC2, FC5, and FC6 (2) Serial dilution issue with several metals for FC1 a nd FC4 outside control limits

MS/MSD recovery was outside control limits for FC1 (Ba, Ni, V, and Zn) and FC3 (Zn, Hg); concentrations for each measurement are c onsistent with other test results; conclusion is this has insignificant impact on data quality

Conclusion : no significant Quality Control issues with Metals results

(d) General Chemistry results

(1) No issues for samples FC2, FC4, and FC5 (2) Sulfide testing FC1 with MS/MSD recovery outside co ntrol limits; Eh/pH indicated oxidizing matrices but high sulfide level possibly interfering with lower level soluble spike recoveries (3) Sulfide testing FC3 with MS/MSD recovery outside co ntrol limits (4) Oil and grease FC1 and FC6 with MS/MSD recovery out side control limits

Conclusion : no significant Quality Control issues with Genera l Chemistry except the sulfide data should be closely reviewed to see if r esults are of consequence

The Data Quality information for Equipment Blanks a nd Trip Blanks was reviewed with the following observations:

(1) No issues were noted for samples FC2 and FC6 (2) FC1 Equipment Blank reported Oil and Grease detecte d but less than reporting
limit (3) FC3 Equipment Blank reported Hexavalent Chromium de tected but less than reporting limit (4) FC4 Equipment Blank reported Acetone at 13 ug/L (5) FC5 Equipment Blank reported Acetone at 16.9 ug/L

Conclusion : no significant Quality Control issues with sampli ng equipment or sample transport

The Data Quality information for duplicate samples was reviewed with the following
observations.

FC1 sample event:

(1) Good agreement with results for most constituents w ith observations noted below for exceptions1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com 

### (2) Oil and Grease: range at 50% with 19,500 mg/kg and 12,600 mg/kg results (3) TCLP metals: when detected (barium, copper, chromiu m, nickel, zinc) these are slightly higher for the sample with lower Oil a nd Grease (4) General chemistry: higher hexavalent chromium for t he sample with lower Oil
and Grease

Conclusions : (1) variability is not unusual for sludge testing (2) variability for some parameters may be consequence of the Oil and Grease variability

FC4 sample event:

(1) Good agreement for most constituents (2) Oil and Grease: range at 24% with 11,100 mg/kg and 8,910 mg/kg results (3) TCLP metals: when detected (copper, nickel) these a re slightly higher for the sample with lower Oil and Grease

Conclusion : (1) variability is not unusual for sludge testing

FC6 sample event:

(1) Good agreement for most constituents (2) Oil and Grease: no difference with 16,600 mg/kg and 17,000 mg/kg results (3) TCLP metals: significant differences for copper (0. 442 and 0.0547 mg/L), chromium (0.826 and <0.0250), nickel (0.744 and 0.0 62 mg/L), and zinc (0.400 and <0.100 mg/L) Conclusion : (1) variability with metals (e.g., FC1 and FC4 results) may not be associated with
Oil & Grease levels but indicative of normal result s for sludge testing

Conclusion on Data Quality

Based on the detailed review of all data quality re ports, our conclusion is that the results represent valid data.



## Test Reports Discussion

A summary table was prepared to facilitate the revi ew and comparison of data between sample events. Our observations are discussed by category of analysis as follows.



### Test Data Results – Oil and Grease

Results:1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com 

### • Range 8,910 to 21,500 mg/kg (Initial FC sample was 6,920 mg/kg)

• Figure 1 plots Oil & Grease and TCLP metal with obs ervations: There is not a significant relationship with TCLP metals and the O il and Grease for samples

• FC1 and FC4 inverse relationship (high Oil and Grea se with lower metals) is not evident when comparing all samples

Higher samples exceeded the 1% concentrations which initiated the requirement to test one sample for the Oily Waste test. As noted in th e January 22, 2013 letter to EPA the FC2 sample was selected as the sample to be tested because it had the highest Oil and Grease result. The Oily Waste test is required to determine if metal levels as measured by the Toxic Characteristic Leaching Procedure (TCL P) may be under-reporting actual metal mobility, for example, with oil. The test ev aluates the sample with two additional extractions: Tetrahydrofuran (THF) and Toluene (T) extractions, with metal in the three extracts added to get the potential for Mobile Meta l Concentration (MC).

The results showed slightly elevated concentrations in THF extract for Chromium, Copper, Nickel, and Lead but not at low concentrati ons.

Conclusion : (1) Metal mobility is not affected by Oil and Grease le vels found in the filter cake samples

Test Data Results – Hazardous Waste Characteristics

Results:

• All test results for TCLP were lower than the Hazar dous Waste Characteristic for the tested metals

Conclusion : (1) The Hazardous Waste Characteristic is not present i n the Filter Cake

Test Data Results – Total Constituent Analysis

• Total results for the FC1 through FC6 samples were reasonably consistent for barium, copper, lead, and vanadium

• The Initial FC sample result was much higher than t he FC1 to FC6 sample results for nickel and zinc; however, the TCLP result for F C1 was not higher with the
elevated total metal levels

Conclusion : (1) Total Constituent results do not indicate any patte rn regarding the testing
results for leachable metals

Test Data Results – General Chemistry1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com



### Results:

• Ignitability was not detected with consistent resul ts for all filter cake samples

• Reactivity for Cyanide was not found with consisten t results for all filter cake samples

• Reactivity for Sulfide was not found with consisten t results for all filter cake samples

• Corrosivity (high pH) was not found with consistent results for all filter cake samples

Conclusion : (1) The Hazardous Waste Characteristic is not present i n the Filter Cake



## Testing Conclusions

Based on the review of the data collected from the sampling and testing, the following
conclusions were noted:

(1) Data quality objectives were met with the testing a nd the results are considered valid
data (2) There was not excessive variability between filter cake samples during the testing (3) Filter cake meets the delisting petition objective of demonstrating that the filter cake
does not have Hazardous Waste characteristics (4) The objectives for the sampling program to support the delisting petition for the Ankeny waste have been met

Please review the testing data as well as the infor mation provided in this letter report and call or e-mail with any questions. After your comments have been addressed, we will continue with the preparation of the complete Delisting Peti tion.

Thank you for your continued assistance with this p roject.

Sincerely,

Project Integration, Inc.

dlk@pintegration.com ph. 864-334-5085 / cell 864-497-6802

cc: Charles Busch, John Deere Fred Van Schepen, John Deere1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com

Robert P. Stevens, P.E., Project Integration, Inc.1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com



# Attachment A

Data Summary Tables1097 Highway 101 South Suite D16, Greer, SC 29651 ( 864) 334-5085, sales@pintegration.com



# Attachment B

Delisting Petition Sampling Data