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 Sampling and Analysis Plan 

(SAP) and Quality Assurance Project Plan (QAPP) for Delisting of F006 

Sludge Filter Cake for your review and comment. The documents include the 

plan for sampling as we discussed along with information from the 

laboratory, TestAmerica. Please contact us with any questions that you any 

questions that you may have as you review the documents and we will 

quickly respond to your requests. As we discussed, we are planning to being 

sampling in mid-summer, pending your review and approval of the plans. 

Also, please let us know when you would like to conduct 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 questions 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 Integration 
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 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 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 has been 

completed and this letter forwards the laboratory results. In addition this letter summarizes key 

results and presents our recommendation for the continued 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 deviations from the sampling procedures. Work 

was completed by MWH Consulting and the samples were shipped to the Test America Chicago, 

Illinois laboratory for analysis. 

Laboratory Test Results 

Test America, in Chicago, Illinois is an Iowa certified laboratory. A complete report with Level II 

detail is included with this letter. If desired, additional detail on laboratory procedures and quality 

systems during the time of this testing is available (the report is 1000 pages, so electronic version is 

recommended, if needed). 

A detailed comparison of the planned testing and the actual is included in Table 1 attached to this 

letter. The major observations and our interpretation 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 also include two (2) new columns. The first new 

column provides a conclusion statement on each chemical and the second column identifies whether 
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 2 

the chemical is presently planned for further sampling or if it has been eliminated from continued 

sampling. 

Herbicide (Table 3.1), Pesticide (Table 3.2) and PCBs (Table 3.3) 

All results for these sets of chemicals were less than 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 discussions). 

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

cake. 

Recommendation: Herbicides, pesticides, and PCBs should not be required for subsequent 

samples. 

Total Semi-volatile (Table 3.4)

Most of the results for the total semi-volatile sampling were less than 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 discussions). 

The exceptions are listed and discussed below: 

Eight constituents were detected in the sludge total analysis with the data qualifier, “J”. A “J” 

result is less than the RL but greater than or equal to the MDL and the concentration is an 

approximation” 

Constituents with the J qualifier include: 

 Benzo(a)anthracene; Benzo(a)pyrene; Benzo(b)fluoranthene; Benzo(ghi)perylene; 

Benzo(k)fluoranthene; Chrysene; Dibenzo(a,h)anthracen; and Indeno(1,2,3-cd)pyrene. 

Conclusions: The results, both the non-detect and the “J” qualified, 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 RL. 

Conclusions: These results confirm the expected absence of these 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 should not be required for 

subsequent samples. 

Total Volatile Organic Constituents (Table 3.5) 

Most total results were less than 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 discussions). 

Exceptions to the above are listed and discussed below: 

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 detected in the sludge total analysis with the 

“J” data qualifier as discussed above: 

Conclusions: These results indicate that only Acetone and 2-Butanone were present in the 

sludge. 

Recommendation: Further testing should include the volatile organic 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 these constituents in the sludge 

cake. 

Recommendation: TCLP extract volatile organic chemicals should not be required for 

subsequent samples. 

Total Metals (Table 3.6)

Results for the total metals analysis indicate absence 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 quantifiable 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 the 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 copper and nickel at levels greater than the 

Reporting Limit. The following constituents had the J qualifier: barium, vanadium, and zinc. 

Conclusions: Each constituents absent in the sludge total analysis 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 vanadium 

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 quantifiable 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 TCLP Extract Mercury as not present. 

Conclusion: The results indicate that there was not a quantifiable amount of mercury in the 

sample. 

Recommendation: Continue testing the TCLP extract for mercury because 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 result. 

 

Conclusion: The tests for pH, sulfides, and flashpoint demonstrate the sludge does not 

exhibit the characteristic of a hazardous waste. The tests for solids, and oil and grease are 
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 5 

needed to perform the TCLP extraction. These tests will be continued for the testing 

program. 

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

The test for total cyanide indicates possible presence 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. The 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 sample using the normal TCLP procedure and 

alternative extraction fluids: 

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

Target pH 7.00 (ASTM method) – extraction fluid Deionized Water 

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

Bench sheets for the extraction are available in the Level III data report (see pages 945, 946, and 947 of 

1061 total pages). 

Results are summarized in the attached Table 4. The results indicate there is no significant difference 

for extract concentrations at the three pH levels. In particular, if the total concentration of the 

detected constituent is divided by 20 to approximate 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 solubility significantly different at the 

three pH conditions. 

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

Recommendations for Continued Sampling 

The Constituents of Concern List for Remaining Sampling 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, zinc, 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 concentration 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 immediately begin the completion of the remaining 

sampling to develop the Delisting Petition. 

Do not hesitate to call or e-mail with any questions 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: 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 Tables 

Analytical Report, Sludge Filter Cake Delisting, TestAmerica, 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 Tables 
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 8 

Attachment B 

Analytical Report, Sludge Filter Cake Delisting, TestAmerica, 8/04/2011 
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 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 7196A 
Mr. 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 thresholds 
Mr. 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 Integration 
4. 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 extraction 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 am 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 Letter
4. 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.

Thanks 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 D16, 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, please find three copies each of the revised Sampling and Analysis 

Plan (SAP) and Quality Assurance Project Plan (QAPP) for Delisting of 

F006/F019 Sludge Filter Cake for your review and comment. As you 

discussed previously with Fred Van Schepen, we are submitting 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 from 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 would 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 

further 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 D16, Greer, SC 29651 (864) 334-5085, sales@pintegration.com

Sincerely,

David L. Kirby

Project Integration, Inc.

Sr. Project Manager

cc: Robert P. Stevens, P.E., Project Integration

Fred Van Schepen, John Deere

Charles, Busch, John Deere
Waterloo 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 approved by EPA on September 28, 2012. 

The SAP included a description of the test constituents and quantitation limits for the sludge 

samples based on the EPA standard protocols. 

John Deere has concluded that the analytic work will be performed by Test America, in 

Chicago, Illinois, an Iowa certified laboratory. In working with the laboratory we have 

identified small differences between the constituent 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 constituents listed in the SAP are not reported 

by Test America. 

We believe that the constituents not reported do not have a negative effect on the results of 

this work. Therefore, we are requesting that EPA agree that the constituent list can be 

slightly modified as outlined below: 

Table 3.1 Herbicides: 

• We request that the following constituents be removed from the SAP: 

o MPCA, MCPP 

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

Test America 

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

• CONCLUSION: excluding these from the Table 3.1 Herbicide list will not reduce the 

validity of the delisting testing program 

Table 3.2 Pesticides: 

• We request that the following constituents be removed 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 protocol for the selected laboratory, 

Test America 

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

• CONCLUSION: excluding these from the Table 3.2 Pesticide list will not reduce the 

validity of the delisting testing program 
Waterloo SAP Lab Deviation Ltr 10-16-2012 d1.docxPage 2 

Table 3.4 Semi-volatile Organics 

• We request that the following constituents be removed from the SAP: 

o Methyl methacrylate; Tributylphosphate 

• REASON: these are not part of the usual Semi-volatile Organic protocol for the selected 

laboratory, Test America 

• REASON: chemicals with Semi-volatile Organic constituents 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 program 

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 constituents of concern. If there is the detection 

of constituents with properties similar to the chemicals listed above, we will evaluate the 

need for additional special testing. 

A second change is that the “LOQ PQL” limits achieved by Test America for some 

constituents will vary slightly from the levels listed in the SAP tables due to differences with 

the sample matrix and laboratory protocols. The actual levels are expected to be consistent 

with the work for the John Deere Ankeny delisting Initial 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 Constituents 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 questions 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 Integration 
1097 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 facility 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 cake Oil and Grease concentrations ranged from 

8,910 mg/kg to 21,500 mg/kg. Since this exceeds the 1% level, the Sampling and Analysis Plan 

requires testing a sample for the Mobile Metal Content, using the Extraction Procedure for Oily 

Wastes, Method 1330. Therefore, John Deere proposes 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 Iowa but we have located a laboratory in the state 

that can perform the test. Their qualification package 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 metals in the liquid (not applicable for this 

sludge - no liquid) 

• extract solid with tetrahydrofuran and test total metals in the liquid 

• extract same solid with toluene and test total metals 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 'total' metal in the original sample. This data 

has been collected from the testing already completed. 

The filter cake samples are being held by Test America 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 forward with the completion of the petition. 

 Please review and provide any comments that you may 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 Integration 
1097 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 Ankeny facility has been completed. This 

letter serves to provide an overview analysis of the 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 testing 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 and data packages, a discussion of the data 

quality reports, summary of the testing reports, and 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 independent event. 

The laboratory data packages for each event have been 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, general 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 that includes the results from the detailed 

testing along with the data qualifiers for each sample 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 data 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 filter 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 information 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 limits; FC2 and FC4 with high 

levels causing MS/MSD accuracy and precision not evaluated; FC4 with internal 

sample response out of limits; and FC5 with one internal 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 results 
1097 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 and 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 consistent 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 control 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 control limits 

(4) Oil and grease FC1 and FC6 with MS/MSD recovery outside control limits 

Conclusion: no significant Quality Control issues with General Chemistry except the 

sulfide data should be closely reviewed to see if results are of consequence 

The Data Quality information for Equipment Blanks and 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 detected but less than reporting 

limit 

(3) FC3 Equipment Blank reported Hexavalent Chromium detected 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 sampling 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 with observations noted 

below for exceptions 
1097 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, chromium, nickel, zinc) these 

are slightly higher for the sample with lower Oil and Grease 

(4) General chemistry: higher hexavalent chromium for the 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 are 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 0.062 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 results for sludge testing 

Conclusion on Data Quality 

Based on the detailed review of all data quality reports, our conclusion is that the results 

represent valid data. 

Test Reports Discussion 

A summary table was prepared to facilitate the review 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 observations: There is not a 

significant relationship with TCLP metals and the Oil and Grease for samples 

• FC1 and FC4 inverse relationship (high Oil and Grease 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 the 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 (TCLP) may be under-reporting actual 

metal mobility, for example, with oil. The test evaluates 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 Metal Concentration (MC). 

The results showed slightly elevated concentrations in THF extract for Chromium, 

Copper, Nickel, and Lead but not at low concentrations. 

Conclusion: 

(1) Metal mobility is not affected by Oil and Grease levels found in the filter cake 

samples 

Test Data Results – Hazardous Waste Characteristics

Results: 

• All test results for TCLP were lower than the Hazardous Waste Characteristic for 

the tested metals 

Conclusion: 

(1) The Hazardous Waste Characteristic is not present in 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 the FC1 to FC6 sample results 

for nickel and zinc; however, the TCLP result for FC1 was not higher with the 

elevated total metal levels 

Conclusion: 

(1) Total Constituent results do not indicate any pattern regarding the testing 

results for leachable metals 

Test Data Results – General Chemistry 
1097 Highway 101 South Suite D16, Greer, SC 29651 (864) 334-5085, sales@pintegration.com

Results: 

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

• Reactivity for Cyanide was not found with consistent results for all filter cake 

samples 

• Reactivity for Sulfide was not found with consistent 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 in 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 and 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 information 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 Petition. 

Thank you for your continued assistance with this project. 

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 
1097 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 Tables 

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

 

Attachment B 

Delisting Petition Sampling Data