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 201 2

Quality Assurance Project Plan, Revised June 2012John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 i 

# Table of Cont ents

Basis for Amendment Request

................................ ................................ ................................ ................................ . ii

Introduction

................................ ................................ ................................ ................................ ............................... iii

1. Background

................................ ................................ ................................ ................................ ...................... 1

1.1 Site Description

................................ ................................ ................................ ................................ .... 1
1.2 Plant Proce ss 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 Was te 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)John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 ii 

# 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 hazardou s 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 201 1 , 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 incor porate 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.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 iii 

# Introductio n

John Deer e Des Moines Works (John Deere) is a manufact urer 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 t reats 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 wastewa ter 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 informat ion 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 w ith 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 constituent s 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 wa ste 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 PersonnelJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 iv The designated representatives for the John Deere delisting petition project ar e Kenneth Herstowski, P.E. of EPA Region 7, and Charles Busch of John Deere

.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 1 

# 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 incl uding 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 c ompletely 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 Proc ess 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 overa ll 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 m etal parts

– cutting, punching, stamping, welding; cleaning, plating, and pain ting; 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 operatio ns 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 Chemica l 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 wastewaterJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 2 • Assem bly

– 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 discus sed 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 l ine 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

– thi s 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 Reductio n 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 WW TP

• 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 fa cility 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

.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 3 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 mai n WWTP and a separate hexavalent chrome reduction treatment unit at the Department 3 9 Chrome electroplating unit. All site industrial wastewaters, including the Department 3 9 Chrome electroplating wastewater after hexavalent chrome reduction processing, a re 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 Hexavalen t 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 for m 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 ri nse 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 treatme nt. 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 databa se 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 t ests 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.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 4 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 t o 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) i s 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 t he 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

- fo am. 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 capacit y 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 th e 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,
fe rric 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 i nitiated 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 lowerJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 5 quantity than Tank 2 with blowdown initiated by sludge depth (similar to Tank 2). Clarified water
flow s 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 (nor mal 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 sh ifts 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. Dewater ing 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 dro pped 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

c ollection 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 Disposa l

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 cl osed 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 s end the filter cake to the Metro Park East Landfill near Mitchellville, IA

.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 6 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 (Feb ruary 2011) in Department 19 has resulted in a cessation of the site’s major zinc and nickel sourc e 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).John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 7 

# 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 th ese 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 Po tential 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); phosp hate 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, E PA’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 wastewater s. 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 A ppendix 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

an d 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):John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 8 • Total and Toxicity Characteristic Leaching Procedure (TCLP) Volatile an d 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 d etailed 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 c oncern 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 sa mple 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

spec ial 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,

t he 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 areJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 9 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 cak e 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 He rstowski; 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 vanad ium.

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 Na OH)

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 wil l 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 sulfid e and reactive sulfide. Additionally, although the John Deere wastewater generating processes are non

- cyanide based, as cyanide isJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 10 one of the constituents for which the John Deere waste was originally listed, the filter cake samples will be analyzed for t otal 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 the ir 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 Labor atories.

The laboratory will follow the appropriate Quality Control (QC) protocol described in Chapter One of SW

846, as well as those outlined in each SW

- 846 method. This includes the use of Matrix Spike and Matrix Spike Duplicates (MS/MSDs), Method Blan k, 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 BlankJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 11 A trip blank contain ing 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 eq uipment 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 metho d, 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 site

sp ecific 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 ana lyzed 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).John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 12 • All filter cake samples will be analyzed for the RCRA hazardous waste characteris tics 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, includi ng: 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 consti tuents 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.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 13 

# 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

- br ow n 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 disc harge, 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 Sampl ing 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 person nel 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 com posite 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 manufacturingJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 14 operations, the large equalization basin, and the l arge 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 samp les 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 place d 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 b lank 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, i ndividual 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, l aboratory

- 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
delive ry.

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 f irm 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.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 15John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 16 

# 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 constitue nts 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 comme nts, 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 complete d 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

req uirements 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). Base d 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 dis cuss 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 w ithin 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.John Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 17 

# TablesJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 18 

## 1.1 Raw Material List for Manufacturing

SOURCE / CHEMICAL DESCRIPTION Dept. 19 Pretreatment "Washer" Chemicals

Cor Clene 16 Potassium hydroxid e; 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
S urcoat 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 Electr oplaters: 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
NoneJohn Deere, Des Moines IA Filename: AddF019Ankeny Delist Final 7

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Project Integration, Inc. John Deere SAP Project No. 101004C1 19 

## 2. Potential Constituents of Concern by Category Category for Constituents of Concern Reason for Inclusion # of Sa mples 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; Tot al 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 To tal

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.