Project Integration, Inc.

1097 Highway 101 South - Suite D16 Greer, SC 29651

864-334-5085

sales@pintegration.com

John Deere

Des Moines, Iowa

Sampling and Analysis Plan for Delisting of

F006 and F019 Sludge Filter Cake

June 2012

References: 

Sampling and Analysis Plan, Revised January 2012

Quality Assurance Project Plan, Revised June 2012
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Table of Contents

Basis for Amendment Request................................................................................................................................. ii

Introduction............................................................................................................................................................... iii

1. Background ......................................................................................................................................................1

1.1 Site Description ....................................................................................................................................1

1.2 Plant Process Operations ....................................................................................................................1

1.3 Wastewater Treatment Plant (WWTP) Operation...........................................................................3

1.3.1 Hexavalent Chrome Reduction Unit...................................................................................3

1.3.2 Wastewater Treatment and Discharge ...............................................................................4

1.3.3 Sludge Treatment ..................................................................................................................5

1.3.4 Filter Cake Storage and Disposal ........................................................................................5

2. Analytical Plan.................................................................................................................................................7

2.1 Constituents of Concern .....................................................................................................................7

2.1.1 Identification of Constituents of Potential Concern..........................................................7

2.1.2 Initial Filter Cake Sample .....................................................................................................7

2.1.3 Final List of Constituents of Concern .................................................................................8

2.1.4 Analysis of Samples ..............................................................................................................9

2.2 Identification of Analytes .................................................................................................................10

2.2.1 Demonstration Without Laboratory Analyses that Certain Constituents Are Not Present 

at Hazardous Levels............................................................................................................10

2.2.2 Appropriate Waste Analytical Methods ..........................................................................10

2.2.3 Appropriate Quality Control Protocols............................................................................10

2.3 Summary of Analytical Requirements............................................................................................11

3. Sampling Methods ........................................................................................................................................13

3.1 Waste Description..............................................................................................................................13

3.2 Sampling Strategy..............................................................................................................................13

3.3 Sampling Procedures.........................................................................................................................13

3.4 Sampling Personnel...........................................................................................................................14

4. Schedule..........................................................................................................................................................15

Tables and Figures

1.1 Raw Material List for Manufacturing (included for convenience in review)

 2. Potential Constituents of Concern by Category (included for convenience in review)
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Basis for June 2012 Revision

In 2011, John Deere began the process of delisting the F006 filter cake with the belief that there were no other 

operations at the facility specifically included under RCRA as listed hazardous waste. However, in early 

2012, it was determined that a small amount of aluminum parts had been treated for the chemical conversion 

process and that this wastewater had been a small fraction of the wastewater into the treatment facility. The 

sludge generated from treatment of this wastewater would be a listed F019 hazardous waste.

During 2011, John Deere prepared and received approval for Sampling and Analysis Plan (SAP, March 2011) 

for the delisting of the filter cake sludge. The initial sample event to confirm constituents of concern was 

completed August 2011, and after discussions with EPA, the SAP updated with selected Constituents of 

Concern and samples (Revised January 2012). The Quality Assurance Project Plan also was approved 

(March 2011) and updated (Revised January 2012).

The change with this revision is to incorporate the delisting for F019 hazardous waste into the delisting plan. 

In particular, this document has been revised to document that F019 constituents are addressed in the 

approved SAP.
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Introduction

John Deere Des Moines Works (John Deere) is a manufacturer of agriculture equipment. Plant operations 

generate wastewater which is treated onsite at the John Deere wastewater treatment plant (WWTP), a 

pretreatment facility discharging to the Ankeny Publicly Owned Treatment Works (POTW).

The John Deere WWTP treats wastewater that includes discharge from an electroplating unit. Therefore, the 

sludge and resulting filter cake from dewatering the sludge is currently defined under 40 CFR 261.31 as a 

RCRA listed hazardous waste (F006). 

John Deere also determined in early 2012 that a small amount of aluminum parts had been treated for the 

chemical conversion process and that this wastewater had been a small fraction of the wastewater into the 

treatment facility. The sludge generated from treatment of this wastewater is currently defined under 40 

CFR 261.31 as a RCRA listed hazardous waste (F019).

The filter cake generated from the John Deere WWTP has not exhibited any hazardous waste characteristic. 

Regulations at 40 CFR 260.22 allow a facility to submit information to delist a hazardous waste. Therefore, 

John Deere is planning to develop representative analytical data on the F006 filter cake to support a petition 

to delist the filter cake from a listed hazardous waste to a non-hazardous industrial solid waste. 

This Sampling and Analysis Plan (SAP) has been prepared pursuant to discussions held January 27, 2011, 

between representatives of John Deere and the United States Environmental Protection Agency (EPA) 

Region 7. This SAP has been prepared in accordance with the EPA RCRA Delisting Program Guidance 

Manual for the Petitioner dated March 23, 2000.

As outlined in 40 CFR 260.22, one requirement of a successful delisting petition is a demonstration that the 

listed waste does not contain the hazardous constituents for which it was originally listed, or other 

hazardous constituents which would cause the waste to be hazardous according to the criteria found in 40 

CFR 261.11 (a)(3). This SAP contains both the analytical and sampling plans to make this demonstration,

and includes the following information:

• Background information on the John Deere facility and plant process operations;

• Description of the waste generating and waste treatment processes;

• Identification of all constituents of concern;

• Description of the waste sampling methodology;

• Outline of all laboratory analytical methods; and,

• Quality assurance/quality control (QA/QC) procedures to be employed during the sampling and 

analysis programs.

Project Personnel 
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The designated representatives for the John Deere delisting petition project are Kenneth Herstowski, P.E. of 

EPA Region 7, and Charles Busch of John Deere.
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1. Background

1.1 Site Description

The John Deere facility is located at 825 SW Irvinedale Drive in Ankeny, Iowa. The facility covers over 451 

acres including manufacturing areas (approximately 180 acres) and testing farmland. 

The manufacturing area includes four major manufacturing buildings (Buildings 1, 2, 3, and 4) and several 

smaller supporting and/or expansion building. The site originally was a war factory (World War 2) for the 

manufacture of machine gun shells. The main buildings including the wastewater building major structures 

were acquired by John Deere and modified for agriculture equipment manufacture.

The manufacturing areas are almost completely paved, relatively flat, with surface runoff to drains and 

subsurface storm piping. General drainage is to the perimeter of the manufacturing area, with the storm 

piping discharging to a storm water pond at the southeast of the area. 

1.2 Plant Process Operations

The John Deere facility produces agricultural equipment including: cotton picking equipment; spraying 

equipment; tillage (plowing) equipment; and grain drills (seeding). There may be some seasonal variability 

for each product line but overall production is fairly even. The facility can operate up to 24 hours per day, 7 

days per week, with the exception of periodic planned shutdowns for routine maintenance.

• Steel metal parts – cutting, punching, stamping, welding; cleaning, plating, and painting; plating 

includes chrome surface hardening for cotton picking spindles (this is the electroplating operation 

causing the listed F006 filter cake); cleaning includes wash lines prior to painting and embedded 

wash stations in paint lines; these operations are the major source of wastewater

• Aluminum metal parts – ladders for tractor cabs are manufactured from aluminum to be corrosion 

resistant; these ladders are cleaned in the wash lines which included operations considered as 

chemical conversion 

o Chemical conversion coating is a metal finishing process which involves the application 

of a coating (e.g., by spray or dip tank) to a previously deposited metal or a base metal to 

increase corrosion protection and to prepare the surface for additional coatings, or the 

formulation of a special surface appearance. 

o Most conversion coating operations include chromating, phosphating, metal coloring 

and/or immersion plating.

• Plastic tanks (on-site contractor) – forming tanks; this is a minor source of wastewater
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• Assembly – touch up painting, testing; this is a small source of wastewater and a minor amount of 

storm water from outside operations

• Support for research and development 

The specific wastewater sources and approximate flows are listed in Appendix A and discussed below by 

source as identified in this format: John Deere Department (building) brief description of process

• Department 19 (Building 2) E-Coat System – this is a 5-stage wash line; wastewater is generated from 

7 wash stages embedded in the line; this line included the aluminum ladders

o Wash/rinse operations: stages 2, 4, 5

o Phosphating: stage 3

• Department 20A (Building 3) Wash Pretreatment – this is a 3 stage wash system prior to painting of 

parts

• Department 20C (Building 2) Manual Wand Wash System – this is a bay with a hand wand for 

treating oversize parts and small assemblies

• Department 39 (Building 2) Chrome Electroplating – this includes two complete multi-stage plating 

systems; spent rinse waters are directed to a separate Hexavalent Chrome Reduction Unit for the 

reduction of hexavalent chromium (the plating chemical) to trivalent chromium by chemically 

treating with sodium metabisulfite; the treated spent rinse water then is discharge to the facility 

WWTP; equipment also generates scrubber blowdown from air pollution control system with this 

blowdown also treated in the Hexavalent Chrome Reduction Unit

• Department 38 (Building 3) Heat Treatment – this includes four heat treating furnaces; cooling water 

for the furnaces is discharged to the facility WWTP

• Department 55 Garage Wash Area – this is a small cabinet for cleaning equipment such as 

agricultural units after testing

• Storm drains (several locations) – there are 3 locations where outside activities that can generate 

wastewater are drained to the facility WWTP: 

o Building 1 Puck Dock Drain – this area is approximately 40 by 40 feet paved area under a 

roof where skids of metal cutting pucks (compacted cuttings) is located; area drains to the 

WWTP to isolate minor leaks from stormwater.
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o Building 16 WWTP Collection/Equalization Tank – the tank surface area is 60 feet by 100 feet 

with direct rainfall into the open tank

o Building 16 tanker containment – this area is used to contain potential tanker unloading 

spills (oil or machine coolants) and is exposed to rain water.

Information on the chemicals used in each operation is included in Appendix A and a copy of the MSDS for 

each chemical is in Appendix B.

1.3 Wastewater Treatment Plant (WWTP) Operation

The John Deere wastewater treatment operations include the main WWTP and a separate hexavalent chrome 

reduction treatment unit at the Department 39 Chrome electroplating unit. All site industrial wastewaters, 

including the Department 39 Chrome electroplating wastewater after hexavalent chrome reduction 

processing, are collected in a central equalization tank and then treated for discharge in the main WWTP. 

The filter cake for this delisting work is from the WWTP. The individual treatment operations are described 

below.

1.3.1 Hexavalent Chrome Reduction Unit

The Hexavalent chrome treatment unit handles only spent rinse waters from the chrome plating system. The 

treatment unit is a steel tank with overall dimensions of approximately 12 ft length by 4 ft width by 4 foot 

height. The tank includes two internal baffles to form three treatment zones. 

• Zone 1 receives the spent rinse waters where they are pH adjusted. The pH probe controls the acid 

feed. Discharge from this zone is an underflow opening in the internal baffle.

• Zone 2 used to treat the hexavalent chrome in the rinse water. The chemical sodium bisulfite is 

metered into this zone based on the ORP meter value.

• Zone 3 allows additional resonance time for the reaction to complete. ORP is displayed from this 

zone as an indicator of the completeness of the chrome treatment. The treated wastewater is 

discharged to the plant industrial waste water sewer where it flows to the WWTP equalization tank.

Control monitoring of the chrome treatment unit includes the pH and ORP levels via a continuous 

transmittal to a central database display accessible by PC. Control testing includes at least one test per shift 

for presence of hexavalent chrome using the “powder pillow” technique manufactured by Hach. Chemical 

addition can be manually adjusted to maintain the ORP should the pillow tests indicate so.

The chrome electroplating concentrated baths are not discharged into this chrome treatment unit or into the 

facility WWTP. The spent bath solution is pumped to a Hazardous Waste Tank and then removed by a 

permitted contractor for proper transfer and disposal off-site.
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The two chrome electroplating lines are each in a separate containment system that are not plumbed to any 

sewer lines. Small leaks and spills are rare and can be pumped into the chrome reduction system for 

treatment prior to sending to industrial waste treatment. Any large release to the containment area would be 

contained and managed by the same process to manage concentrated chrome bath disposition.

1.3.2 Wastewater Treatment and Discharge

The wastewater treatment plant (WWTP) is located at/in Building 16. There is an in-ground concrete 

equalization tank outside the building (Tank 1). The building foundation itself is the walls of the process 

tanks inside. These foundation/tanks are concrete with the inside wall exposed inside the building’s 

basement and the outside wall in-ground outside the building. 

Water from Tank 1 is pumped into the building tanks where it flows through two flocculation/clarification 

units operated in series (Tank 2 and Tank 3) and a pH adjustment stage (Tank 4) before being discharged to 

the public sewer. Settled solids from the flocculation/clarification units are pumped to a holding tank (Tank 

5a), then to a sludge thickener (Tank 5), with the thickened sludge dewatered in a plate and frame filter 

press.

• Tank 1 Equalization/Holding: The tank is an in-ground concrete structure with dimensions of 60 feet 

by 100 feet and 14 foot side wall (capacity 630,000 gallons). Normal operating level ranges from 4 to 

10 foot depth (operating volume 180,000 to 450,000 gallons). The tank is mixed with blowers and 

diffusers along the tank bottom. Chemicals added to this tank are listed in Table 1.2 and include pH 

adjustment (normal is acid with iron; caustic if needed), flocculent (normal cationic polymer), and 

anti-foam. Capability is present to add sodium metabisulfite for hexavalent chrome reduction if 

there is any detection from the chrome treatment unit testing. With a normal/typical wastewater 

flow rate of 110,000 gpd, the equalization tank has a holding capacity of 1.5 to 3 days.

• Tank 2 Stage 1 Flocculation/clarification: The tank is a concrete cell approximately 20 ft by 20 ft by 15 

ft depth, with an operating level from 10 to 12 feet. A steel package-type circular 

flocculation/contact unit in the center of the tank is fed wastewater from the equalization Tank 1. 

Normal flow is approximately 60 to 160 gpm (based on typical 110,000 gpd flow). Chemicals added 

to the tank are listed in Table 1.2 and include pH adjustment (normal is caustic), emulsion breaker, 

ferric sulfate (to promote floc formation), and flocculent (normal cationic polymer). Flocculated 

solids are maintained as a sludge blanket in the unit with blowdown to the sludge thickener initiated 

by sludge depth (electronic eye sludge blanket detector initiated a timed pump cycle). Tank is 

configured to maintain flow through the sludge blanket for solids formation. Clarified water flows 

by gravity into a weir and then into the contact unit in the Stage 2 unit.

• Tank 3 Stage 2 Flocculation/clarification: Same configuration as Tank 2. Chemical addition includes 

only the flocculent (normal cationic polymer). Flocculated solids are less dense and a lower 
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quantity than Tank 2 with blowdown initiated by sludge depth (similar to Tank 2). Clarified water 

flows by gravity into a weir and then into Tank 4.

• Tank 4 pH Adjustment: The tank is a concrete cell approximately 20 ft by 20 ft by 15 ft depth with an 

operating level of about 12 feet. Inlet discharges by underflow into tank with overflow pipe for 

discharge to the public sewer. Tank also includes a sampling station.

• Tank 5 Sludge Thickener: The tank is a cone-bottom steel tank placed inside the concrete cell (cell is 

dry). Tank is 12 foot diameter by 15 ft height. Chemical addition includes coagulant (normal is 

cationic polymer). Overflow is directed back to Tank 1. Thickened sludge is feed to the filter press.

Wastewater treatment can operate 24-hours per day continuously. However, discharge is limited to time when the 

operator is present, normally 2 shifts per day. Discharge is regulated by the City of Ankeny’s Sewer Use Permit No. 

001.

1.3.3 Sludge Treatment

Sludge is dewatered in a Netzch plate and frame filter press, including 40 plates (nominal 50 cubic foot 

capacity) with automatic plate opener. Dewatering typically is for two cycles in an operating day with 1 to 2 

operating days required for each calendar week.

Precoat is not required. The filter cake normally is approximately 40% dry solids, reddish brown color, and 

clay-like consistency. Cake is dropped directly into a roll-off container. 

The filter cycle includes cake formation, dewatering, and extended dewatering for tramp water removal. 

The unit prevents any filtrate leakage into the roll-off container during the dewatering cycle with a water 

collection pan draining to Tank 1. The drop cycle includes removing the pan, then automatic opening of 

each frame with the sludge dropping into the container. Each sludge cake is broken into several pieces 

during the drop. 

1.3.4 Filter Cake Storage and Disposal

The roll-off container for the filter cake is lined and in the treatment building. The container will normally 

hold filter cake from 12 treatment cycles with removal and replacement of a full container each 2 to 3 weeks. 

The roll-off container is closed for transport, with appropriate manifests and labeling. Disposal has been at 

the Peoria Disposal Company’s PDC #1 landfill near Peoria, IL and recently at the EQ facility in Harvey, IL.

If this waste is successfully delisted, John Deere expects to send the filter cake to the Metro Park East Landfill 

near Mitchellville, IA. 
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Filter cake has been tested most recently in 2009 and before that in 2007. The data are included in Appendix 

C. The key results are:

• Filter cake had no TCLP organic materials (2009 test) – waste codes D012 through D043

• Filter cake had no total cyanide (2009, 2007)

• Filter cake only had TCLP detections for chromium (0.009 mg/L in 2009 and 2007) and nickel 

(3.1mg/L in 2009; 0.55 mg/L in 2007.

Note that a recent process change (February 2011) in Department 19 has resulted in a cessation of the site’s 

major zinc and nickel source chemical product at the site, and one of the sources of hexavalent chrome (i.e. 

John Deere no longer uses zinc phosphate with nickel or chrome rinse in Dept 19).
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2. Analytical Plan

2.1 Constituents of Concern

EPA regulations and guidance were used to develop a list of constituents of potential concern, which were 

then evaluated using historical data and generator knowledge of plant process operations. Many of these 

constituents could be eliminated from further consideration as constituents of concern based on analytical 

data of historical F006 sludge samples, and/or their absence from raw materials used in facility operations.

2.1.1 Identification of Constituents of Potential Concern

Identification of the constituents of potential concern for the F006 and F019 cake began with the constituents 

of concern for which the waste was originally listed: F006 , cadmium, hexavalent chromium, nickel and 

cyanide (complexed); phosphate aluminum. Additional constituents include those required by EPA in 40 

CFR 260.22 (d) and the constituents recommended in the March 1996 EPA guidance document entitled 

“Region 6 RCRA Delisting Program Guidance Manual for the Petitioner.” In addition, EPA’s Guidance 

Manual requires that the identification of additional constituents found in 40 CFR 261, Appendix VIII, as 

well as the following six constituents not found in Appendix VIII: acetone, ethylbenzene, isophorone, 4-

methyl-2-pentanone, styrene, and total xylenes.

The wastewater generated by the facility is regulated by EPA under 40 CFR 433, the Metal Finishing Point 

Source Category. This category defines a list of total toxic organic (TTO) compounds which may be present 

in metal finishing wastewaters. The TTO list includes pesticides, polychlorinated biphenyls (PCBs), and 

2,3,7,8-TCDD (dioxin), none of which are present in the facility processes.

In a further effort to identify any constituents that might be present in the F006 and F019 filter cake, the 

major chemicals used at the facility were reviewed. Table 1.1 presents a list of these chemicals used in the 

plant which could potentially appear in the F006 and F019 filter cake. Material Safety Data Sheets (MSDs) for 

these materials are provided in Appendix A.

2.1.2 Initial Filter Cake Sample

An initial sample will be collected that is representative of the filter cake material from the John Deere 

wastewater treatment process. The sampling procedure will be consistent with that described in Sections 3.2 

and 3.3. This sample will be analyzed for the chemical constituents listed in Appendix IX of 40 CFR §264 

(this is more comprehensive/inclusive than the 40 CFR 261, Appendix VIII list):
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• Total and Toxicity Characteristic Leaching Procedure (TCLP) Volatile and Semi-volatile organic 

compounds 

• Toxicity Characteristic (TC) metals plus antimony, beryllium, copper, nickel, thallium, and zinc

• Total Pesticides and herbicides

• Total PCBs

• Oil and Grease

• Total Cyanide

• Total and Reactive Sulfide

• Ignitability

• pH

A list of the Appendix IX constituents is provided in Tables 2 and 3. Table 3 also lists appropriate analytical 

methods for each category of chemical compounds.

The list of constituents of concern for subsequent filter cake samples will be expanded to include any of the 

constituents detected above the laboratory’s estimated quantitation limit (EQL) in this initial filter cake 

sample. The analyte list for subsequent filter cake characterization is described in further detail in Section 

2.1.3 of this plan. A more detailed analysis of the sampling plan and methodology is provided in Section 3.

2.1.3 Final List of Constituents of Concern

Through generator knowledge of process operations and historical analyses of the F006 filter cake, many of 

the constituents of potential concern listed in Appendix IX (40 CFR-Part 264) are not applicable to the F006 

filter cake produced by John Deere and are not expected to be detected in the initial sample results. The 

major constituent categories not expected to be found in the initial sample include volatile or semi-volatile 

organic compounds, pesticides, herbicides, and PCBs. Additionally, the John Deere electroplating operation 

is non-cyanide in nature, and the three waste categories listed in the RCRA Guidance Manual as requiring 

special analytical methodologies (i.e. petroleum industry wastes, stabilized wastes, and dioxin wastes) do 

not apply to the John Deere F006 filter cake.

Based on the John Deere knowledge of the raw materials used in the manufacturing and treatment processes, 

the review of the chemicals and MSDS information, and the historical data on the F006 filter cake, a list of 

constituents of concern has been compiled and is presented in Table 2. Analytical methods to be used are 

summarized in Table 3. This list includes all of the chemical constituents listed in Appendix IX which are 
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known to be, or which may potentially be present in the filter cake based on generator’s knowledge of the 

raw materials used. It is anticipated that after analysis of the initial filter cake sample, constituents of 

concern to remain for the subsequent filter cake samples will include:

Final Constituents of Concern for Balance of Testing

Analysis of each collected sample will include (reference: Letter, August 15, 2011, David Kirby, to 

Ken Herstowski; additional communications with Mr. Ken Herstowski, EPA Region 7,,Email 

December 22, 2011):

Filter cake will be analyzed for total and extract concentrations of the following metals: 

barium, chromium, copper, lead, mercury, nickel, zinc, and vanadium.

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

Multiple leaching: pH 2.88 (acetic acid); pH 7; pH 13 (0.1 N NaOH)

The results of the initial sampling and the basis for confirming or changing the Proposed Final Constituents 

of Concern will be presented in a brief report submitted to EPA for review and approval.

2.1.4 Analysis of Samples

Analysis of the initial sample will be for total concentration of Appendix VIII and IX constituents in addition 

to the leachable concentrations of metals as discussed below. 

Analysis for all filter cake samples will include total concentration of TC metals and leachable concentrations 

of TC metals using the TCLP in SW-846 Method 1311. If the total oil and grease content of the filter cake 

sample is one percent or more, the Extraction Procedure for Oily Wastes (OWEP), SW-846 Method 1330 will 

also be performed in addition to TCLP analyses to quantify the leachable levels of all metals of concern. 

All filter cake samples will also be analyzed to determine whether the waste exhibits ignitable, corrosive or 

reactive properties, including analyses for total constituent concentration of sulfide and reactive sulfide. 

Additionally, although the John Deere wastewater generating processes are non-cyanide based, as cyanide is 
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one of the constituents for which the John Deere waste was originally listed, the filter cake samples will be 

analyzed for total cyanide.

As indicated in Section 2.1.2 above, the list of constituents of concern for all additional filter cake samples 

(Table 2) will be expanded if any of the constituents from Appendix VIII or IX are detected above the 

laboratory’s EQL, which have not already been included.

Analysis of one filter cake sample also will include constituents of concern for leachate generated by a 

Multiple pH Test for three pH concentrations, including: pH 4.93 (representing low acidic conditions in a 

landfill); pH 7.0 (representing normal conditions in a landfill); and pH 10.01 (representing high alkaline 

conditions in a landfill). 

2.2 Identification of Analytes

All constituents listed in Table 2 are capable of being analyzed in a laboratory. These constituents and their 

appropriate SW-846 methods are listed in Table 3.

2.2.1 Demonstration Without Laboratory Analyses that Certain Constituents Are Not Present 

at Hazardous Levels

All constituents of concern are capable of being analyzed in a laboratory. Therefore, there are no

constituents for which a mass balance demonstration needs to be made.

2.2.2 Appropriate Waste Analytical Methods

The material being analyzed is a dry filter cake. The analytical methods to be used are found in “Test 

Methods for Evaluating Sold Waste, Physical/Chemical Methods (SW-846)”. Table 3 lists the specific 

methods to be used in the analysis of each constituent of concern.

2.2.3 Appropriate Quality Control Protocols

The analytical laboratory which will analyze the F006 filter cake samples is Test America Laboratories.

The laboratory will follow the appropriate Quality Control (QC) protocol described in Chapter One of SW846, as well as those outlined in each SW-846 method. This includes the use of Matrix Spike and Matrix 

Spike Duplicates (MS/MSDs), Method Blank, Surrogate Spikes, Field Blank, Equipment Rinsate, Blind 

Duplicate, and Trip Blank analyses. A brief description of the field QC samples that will be used to verify 

the quality of the sampling results is described below:

Trip Blank
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A trip blank containing analyte-free water prepared by the analytical laboratory will be transported to the 

site and returned with the filter cake samples without opening. This will serve as a check for contamination 

originating from sample transport, shipping, and from site conditions. One trip blank per day will be 

utilized when analysis for VOCs is being performed. The trip blank sample will be analyzed for VOCs only.

Field/Equipment Rinsate Blanks

A field/equipment rinsate blank will be used to determine whether the equipment used for collection and/or 

compositing the samples contain chemicals of concern that may be introduced to the sample matrix. Analyte 

free water provided form the analytical laboratory will be poured over the sampling equipment and then 

transferred to sample containers before the sampling equipment is used. One field/equipment rinsate blank 

per sampling day will be utilized.

Blind Duplicate

The analytical results between the sample/blind duplicate will be used to assess variance of the total method, 

including sampling and analysis. The blind duplicate samples will be assigned fictitious identifications; the 

correct sample identification number will be recorded by the sampler. One blind duplicate per sampling run 

will be collected (laboratory and field QA combined) through the duration of the sampling event. One extra 

sample front and rear and a matrix spike will be required.

MS/MSD Samples

MS and MSD samples will be collected and submitted to the laboratory as separate samples to provide sitespecific matrix –interference data. Upon arrival at the laboratory, the MS/MSD samples will be spiked with 

appropriate analytes and analyzed by the appropriate method. The purpose of spiking and analyzing the 

samples is to evaluate any site-specific matrix interference on the analytical results. One MS/MSD sample set 

will be collected through the duration of the sampling event.

2.3 Summary of Analytical Requirements

Following is a summary of the information presented above:

• 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).
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• All filter cake samples will be analyzed for the RCRA hazardous waste characteristics of ignitability, 

corrosivity, and reactivity, including analysis for total constituent concentrations of sulfide and 

reactive sulfide, total cyanide, chromium +6, and pH.

• All filter cake samples will be analyzed for oil and grease content. If the oil and grease content of the 

sample is one percent or greater, the Oily Waste Extraction Procedure (SW-846 Method 1330) will 

also be used in addition to TCLP analyses to quantitate the leachable levels of all metals of concern.

• In addition to the parameters listed above, the initial filter cake sample will also be analyzed for total 

and TCLP concentrations of volatile and semi-volatile organic compounds.

• Total concentrations of pesticides, herbicides, and PCBs. Any constituents detected above the EQL 

in the initial filter cake sample will be targeted for analysis in a minimum of two remaining filter 

cake samples.

• One sludge sample will be analyzed for the constituents of concern for leachate generated by a 

Multiple pH Test for three pH concentrations, including: pH 4.93; pH 7.0; and pH 10.01.

• An engineering analysis was made of the John Deere facility process operations and of all the raw 

material that could potentially be present in the F006 filter cake. Based on this analysis, there are no 

additional constituents of concern.

• Table 2 is a complete list of constituents of concern. This list may be expanded based on the results 

of the initial filter cake sample (described in Section 2.1.2).

• Table 3 present the appropriate analytical methods.

• No mass balance is necessary since all constituents of concern can be analyzed by a laboratory.
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3. Sampling Methods

3.1 Waste Description

The waste to be sampled is a dewatered sludge filter cake generated from the wastewater treatment plant 

filter press. The John Deere WWTP (a pretreatment plant discharging to the local wastewater plant) treats 

wastewater associated with an electroplating process. The resultant sludge drops from the single filter press 

into a 25 cubic yard roll-off container. The filter cake is a reddish-brown solid (approximately 40% solids) 

and has a density of approximately 80 to 85 pounds per cubic foot. The filter cake contains elevated 

concentrations of certain metals.

The WWTP treats and discharges approximately 110,000 gallons of wastewater per day. All raw wastewater 

is combined in one equalization basin with 1.5 to 3 day detention time. Typical filter press operation is two 

filter press cycles for one or two operating days each calendar week. The roll-off is typically filled in two to 

three weeks. 

3.2 Sampling Strategy

John Deere will confirm prior to the initial sample collection that operation is typical for the facility 

regarding processes, products and raw materials. Due to the uniformity of the process and the consistency 

of the wastewater discharge, temporal (time) variability of the waste filter cake is not a concern. John Deere 

will test the initial sample for all Appendix VIII and IX constituents identified and wait for results prior to 

embarking on the remainder of the testing. After the results have been obtained, John Deere will confirm the 

sampling protocol (number of additional samples and Final Constituents of Concern) for the remainder of 

the project and review the protocol with EPA to verify approval. 

The filter cake then will be characterized using 6 additional sample events each analyzed for the Final 

Constituents of Concern listing. These results will be compared to determine any data anomalies. If needed, 

the sampling program will be continued to address such anomalies.

3.3 Sampling Procedures

The initial sample event will include a large number of sample containers due to the wide range of 

constituents for analysis. This sample event will be performed by a qualified consultant team and will be 

used to train the John Deere personnel for subsequent events.

Each sample event will collect filter cake material from the roll-off container after a dewatering cycle and 

filter cake drop. The sample will be prepared by collecting at least three individual aliquots and then 

preparing a composite sample, except for the volatile constituent test which will be a discrete sample. The 

filter cake is not expected to have a substantial temporal variability because of the consistent manufacturing 
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operations, the large equalization basin, and the large sludge holding capacity of the thickener. Therefore 

the sample collection plan is to collect two samples during each week. Each sample will be from filter cake 

from one treatment cycle (i.e., each filter press cycle). The two samples for a week may be on consecutive 

days. 

All samples will be collected with a trowel, collecting sample from surface to a depth about 2 feet. The 

trowel will be wiped clean of gross solids between aliquots. The sample aliquots will be placed in a clean 

stainless steel bowl and mixed to form a composite sample, and a sample of this composite placed in a clean, 

laboratory-supplied sample jar. 

The sample for VOC analysis will be collected from approximately the center of the roll-off with a clean 

sample trowel and placed immediately into a clean, laboratory-supplied glass VOC sample jar. 

The stainless steel mixing bowl and trowel will be cleaned prior to and between each sample event using a 

solution of Aloconox detergent and distilled water, followed by a triple rinse with distilled water. To 

minimize the potential for sample contamination, clean latex sampling gloves will be worn during all sample 

handling procedures, and only clean, laboratory-supplied glass sample jars will be used for all samples. A 

sample of a blank chain-of-custody and sample label is described in the QAPP.

Composite samples will be identified by the sequential number for the sample (e.g., first composite sample 

will be numbered 1; second composite sample will be numbered 2). For field notes, individual aliquots will 

be identified by sample number and grid (e.g., 1-1 for front 1/3 sample for event 1). Relative location of the 

grids will be described in the field notes.

The individual mixed composite samples will be placed in separate, clean, laboratory-supplied glass sample 

jars, and then sealed, labeled and placed on ice in a sample cooler for shipment to the analytical laboratory 

under strict chain-of-custody procedures. The sample cooler will be shipped to the laboratory for next-day 

delivery. 

Duplicate samples will be obtained on a random basis and will be identified as “D” for quality control.

3.4 Sampling Personnel

Filter cake sampling and sample handling procedures for the first sample will be performed by personnel 

from the consulting firm MWH, 1153 Auburn Avenue, Des Moines Iowa. During the sample event, John 

Deere personnel will be trained on the sampling, record keeping and chain of custody procedures to be 

followed. After this training is complete, John Deere personnel will complete the remainder of the sampling.
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4. Schedule

John Deere expects that filter cake sampling can commence within one month after EPA approval of the 

SAP. An initial sample will be for the full constituent list with the objective of confirming those constituents 

for the balance of the sampling. Results of the initial comprehensive testing (Appendix VIII and IX analyses) 

will be reviewed to determine if the proposed Constituents of Concern remain valid for the balance of the 

testing (discussed in Section 3). The results will be submitted to EPA for review and approval of the Final 

Constituents of Concern. John Deere will discuss comments on the proposed Final Constituents of Concern 

with EPA (telephone conference or meeting). Based on resolution of any comments, the Final Constituents 

of Concern and balance of the sampling will be documented. 

The continued filter cake sampling will be completed in 30 days or less with analysis for the Final 

Constituents of Concern. Laboratory analyses normally are completed within four weeks of receipt of the 

last composite sample, so all results are expected in 60 days or less after the continued sampling begins.

All analytical data will be compiled by John Deere and reviewed to confirm the data are consistent with the 

requirements for delisting. A brief progress letter report summarizing the data will be transmitted to EPA 

within two weeks of receipt of the data. John Deere will discuss comments on the Data Summary report 

with EPA (telephone conference or meeting). Based on resolution of any comments on the data, John Deere 

will continue with development of the Delisting Petition. 

The draft Delisting Petition document will be submitted to EPA within four weeks of completing the Data 

Summary report. John Deere will discuss comments on the draft Delisting Petition with EPA (telephone 

conference or meeting). 

It is understood that the draft Proposed Delisting Notice will be prepared by EPA for review by John Deere. 

Any comments from John Deere will be furnished to EPA within 30 days of receipt of the proposed Delisting 

Notice.

It is understood that the Proposed Delisting Notice will be published in the Federal Register for 30 day 

public comment. It is understood that with no adverse comments, the Final Delisting Notice and approval is 

typically available 60 days after the end of the comment period.
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Tables
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1.1 Raw Material List for Manufacturing

SOURCE / CHEMICAL DESCRIPTION

Dept. 19 Pretreatment "Washer" Chemicals

Cor Clene 16

Potassium hydroxide; tetrapotassium 

pyrophosphate

Activator ZN

Potassium titanium fluoride; disodium 

phosphate

Surcoat 88 Iron phosphate

Accelerator 96 Sodium nitrite

Eco Seal Nonchrome final rinse (zirconium based)

Cor Add ZR Hydrofluorozirconic acid

Caustic Soda 50% Sodium hydroxide

Muriatic Acid Hydrochloric acid

Soda Ash Sodium carbonate

20A Pretreatment "Washer" Materials/Chemicals

Surcoat 88 (replace CorClene) Iron phosphate cleaner/coater

City Water (replace EcoTreatM)

Two (2) Manual "Wand" Wash Systems

Coralite 500 Glycol ether; tetrapotassium pyrophosphate

Dept. 20C Two (2) Manual "Wand" Wash Systems

Flash-Clean 1414

Potassium hydroxide; tetrapotassium 

pyrophosphate

Surcoat SW100 Phosphoric acid; nitrobenzene sulfonic acid

Dept. 38 Chrome Electroplaters:

Used EPS 4000 Electropolish Phosphoric acid; sulfuric acid

HEEF 25 R (500)* Chromium trioxide 

HEEF 25 C* Chromium trioxide 

Sodium Bisulfite Solution 40%* Sodium bisulfite

Dept. 38 Heat Treat

Alusol 39

Amine neutralized carboxlic acid; propylene 

glycol

P3 Neutracare 5175 Amine borate; surfactant

Dept. 55 Garage Wash Unit

None

Stormwater Drain Sources

None
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2. Potential Constituents of Concern by Category

Category for 

Constituents of 

Concern Reason for Inclusion

# of Samples for 

Analysis

Laboratory 

Analyses

Volatile, semi-volatile, 

pesticide and herbicides, 

and PCB compounds

Analyze first filter cake sample for 

compounds listed in 40CFR 264, 

Appendix IX, per EPA 

requirements Initial (1)*

Total and TCLP 

VOCs, SVOCs; 

Total Pesticides, 

Total Herbicides and 

Total PCBs

Cyanide

Cyanide was one of the 

compounds that the filter cake 

was originally listed

Initial plus 6

Total cyanide

Arsenic, Barium, 

Cadmium, Chromium, 

Lead, Mercury, Selenium, 

and Silver

TC metals currently listed in 40 

CFR 261.24

Initial plus 6 Total and TCLP 

metals

Nickel, Zinc

Generator knowledge and 

historical data of filter cake

Initial plus 6 Total and TCLP 

metals

Chromium +6

Generator knowledge and 

historical data of filter cake

Initial plus 6

Total metals

Chromium +6 Required by EPA 6 samples

Method 1313

Extraction at pH 2.88;

7; 13

Extract Analysis

Sulfide Required by EPA

Initial plus 6 Total and reactive 

sulfide

Oil and Grease Required by EPA

Initial plus 6

Total

D001 Required by EPA

Initial plus 6

Ignitability

D002 Required by EPA

Initial plus 6

Corrosivity (pH)

D003 Required by EPA

Initial plus 6

Reactivity

pH Required by EPA Initial plus 6 pH

Acetone, 2-butanone

Detected in Initial Sample; added

to initial SAP Plus 6 Total

Note:

* = Any constituent detected above the EQL in the initial filter cake sample will also be targeted for analysis in subsequent samples. 

Compounds that exceed the EQL will be analyzed in subsequent samples for total and TCLP.