CONFIDENTIAL

TREATMENT OF AVR FLY ASH

BY CEMENT-LOCKsM TECHNOLOGY

Prepared by: ENDESCO Services. Inc. 1700 S. Mt Prospect Road Des Plaines, Illinois 60018

Submitted to:

CONFIDENTIAL
September 2000

TREATMENT OF AVRFLY ASH BY CEMENT -LOCJ(SMTECHNOLOGY

SUMMARY
The A VR fly ash was analyzed for its major and minor oxides by XRF method. The analysis showed that the fly ash contains 42.5% Si02, 23.1 % CaO, 11.1% A1203, and 4.0% F~03' The fly ash was mixed with naturally occurring modifiers (90% fly ash + 10% modifiers wt ratio) and processed in a laboratory-scale equipment to produce Ecomelt'" utilizing the Cement-Lockf" Technology. The Ecomelt was analyzed for total metals and their leaching behavior (for eight RCRA metals + Antimony, Molybdenum, and Vanadium). All of the metals are present in the fly ash, however, none of the metals was detected in the leachate except Barium. The concentration of Barium in the leachate was 0.065 mg/1; the regulatory limit for Barium is 100. Therefore, all heavy metals are immobilized within the Ecomelt matrix in its silicate network, rendering it environmentally stable. The Ecomelt easily passes the US EPA TCLP. The Ecomelt was also examined by the Construction Technology Laboratories, Inc. (CTL; research arm of the Portland Cement Association) using microscopic and XRD techniques. The samples were examined under an optical microscope using both the plane-polarized and cross-polarized light. The amount of amorphous phase was visually estimated to be more that 98 percent. A broad hump in the XRD pattern also confirmed the amorphous (noncrystalline) nature of the Ecomelt. Based on the amorphosity of the Ecomelt, the material is suitable for producing construction-grade cement.

FLY ASH CHARACTERIZATION

The AVR fly ash received from. was analyzed by the Construction Technology Laboratories, Inc. (CTL; researc arm of the Portland Cement Association) for its major and minor oxides by the X-ray Diffraction (XRF) method. The XRF. ~ysis showed that the fly ash contains 42.5% Si02, 23.1%CaO, 11.1% A1203 and 4.0% F~03 (Table 1). As per the ASTM 618 Specification, the ash is a Class C fly ash since (Si02 + J\l203 + F~03) is between 50% and 70% by wt. The fly ash contains 3.42% carbon (average of two values, namely, 3.08% and 3.76%; lab reports are included in the Appendix).

ECOMELT PRODUCTION
Based on the fly ash characteristics, a recipe for producing Ecomelt was determined. The feed mixture for Bcomelt production consisted of90% fly ash, 9% Modifier 1 (Limestone), and 1% Modifier 2 (Alumina). The modifiers are naturally occurring mineral materials. Because the ash contained particles as large as 1 em, it was milled to pass 60 mesh (250j.1m) prior to mixing with the Modifiers.

CONFIDENTIAL

Table 1. OXIDE ANALYSIS OF AVR FLY ASH Analyte

Si02 Al203 Fe203 CaO MgO S03 Na20 K20 TiOz P205 Mn203 srO Loss on Ignition Undetermined Total

%wt.
42.51
11.10 3.96 23.12 2.49 3.60 2.27 1.31 1.81 1.31 0.09 0.07

5.17
1.18 100.00

APPARATUS
The feed mixture was fused in a bottom-loading electric furnace shown in Figure 1. The Kanthal molybdenum disilicide ceramic heating elements are capable of producing temperatures in the furnace up to 18000(; (3272F). The furnace is capable of controlledatmosphere operation. Crucibles are introduced and withdrawn through the furnace bottom, resting on a ceramic pedestal which can be rotated by hand. The air is passed through a flow meter and then to an air inlet tube using a diaphragm pump. The tube is an aluminum oxide tube, extending down from the top of the furnace to slightly below the crucible rim. Because the air tube is off the crucible axis, it is used fully lowered to stir molten material by rotating the pedestal. The cylindrical fusion crucible has a capacity of 500 ml, and is made with 99 percent aluminum oxide. The inside diameter and depth are 6.6 em and 14.6 em, respectively. Fusion crucible is placed inside a guard crucible (not shown in Figure 1) of similar material but 1.2 em larger diameter to protect equipment from any escaping molten material from the fusion crucible.

CONFIDENTIAL

T }-

Furnace temperature
controller

Air inlet tube _ Heating elements _-_ - -;-- -- _ __

--Air flow meter - _

- -Crucible

-Pedestal ~ -Insulation

- -Handle Pedestal is rotated to stir slag in crucible

Figure 1. APPARATUS FOR .. COMELT SAMPLE PREPARATION E

TEST PROCEDURE The unit can process about 425 gm of material during a test. Therefore, a series of tests were conducted to process all the fly ash material. Testing was performed with the crucible uncovered in air. The molten material was heated until no more solid matter remained in the melt, as detected by lowering the air tube to feel the crucible bottom. The final temperature ranged from 1350 to 1400C (2462 to 2552F). While at that temperature, the melt was stirred by rotating the pedestal with the air tube near the crucible bottom. The molten material was held at the above specified temperature for about 30 minutes; then the pedestal was lowered below the furnace bottom. The fusion crucible was removed from inside the guard crucible with tongs. The molten material was poured into room temperature water, where it remained brightly luminous for several seconds while under water. Some of the melt was too viscous to pour, or began to solidify in the cooling crucible, so the crucible was thrown into the water to quench the material remaining in the crucible. The quenched material is referred to as Ecomelt. The Ecomelt was separated from the quench water by decanting, and was rinsed with purified water before drying at 90C in an oven. The molten material was benign in its corrosive behavior toward refractories in the laboratory
3

CONFIDENTIAL

furnace. Dissolution of aluminum oxide crucible walls was negligible. This favorable result means the material selection will be less problematic in engineering scale up.

ECOMELT CHARACTERIZATION
The Ecomelt has

a shiny, black, glassy appearance. It is easily crushed and pulverized.

The Ecomelt was analyzed for total metals. metals leachability (US EPA TCLP). and amorphosity .

Leaching Characteristics
The Ecomelt was analyzed for total metals as well as metals leachability by Commercial Testing & Engineering Company (a testing lab), South Holland, Illinois. The fate of Antimony (Sb), Molybdenum (Mo), and Vanadium (V) is of special interest to ~ Therefore) the Ecomelt was analyzed for these metals as well as eight RCRA metals. The results are shown in Table 2; copies of the laboratory report are included in the Appendix. None of the metals was detected in the leachate except Barium. The concentration of Barium in the leachate was 0.065 mgll; the regulatory limit for Barium is 100. Therefore, all heavy metals are immobilized within the Ecomelt matrix in its silicate network by ionic replacement, rendering it environmentally stable. The Ecomelt easily passes the EPA TCLP.

Table 2. TCLP RESULTS ON ECOMELT PRODUCED FROM AVR FLY ASH

TCLp Metal Antimony Molybdenum Vanadium Arsenic Barium cadmium Chromium Lead Mercury Selinium Silver FlyAs~ .- mglkg (dry) 40 23 Ecomelt ND ND Regulatory Limit

------------------m~ ---------.----.ND ND
0.065 ND

19 9.1 730

5
100

6.9
210

ND
ND

96
ND ND

1 5 5
0.2

3.7

ND ND ND

1 5

Toxicity Characteristic Leaching Procedure.

/) L _

JI c. N D f2., c.../( S' e

Cd 11C Iv T -

L ()Lt1.

CD

rl

CONF'OENT\AL

Microscopic and X-Ray Diffraction Measurements

Both the microscopical and X-ray Diffiaction (XRD) tests were performed by CTL on the ground Ecomelt sample. The sample was examined under an optical microscope using both the plane-polarized and cross-polarized light. The amount of amorphous phase was visually estimated by CTL to be more that 98 percent (Figure 2). A broad hump in the XRD pattern also confirmed the amorphous (non-crystalline) nature of the Ecomelt (Figure 3). Based on the amorphous nature of the Ecomelt, as determined by the above tests, the material is suitable for producing construction-grade cement.

Report_A VR]JyAsh.doc

CONFlOENT\AL

Cross-polarized light image of the Ecomelt powder dispersed in propylene glycol and viewed with 530-nm accessory plate. Amorphous material is the color of the background. Crystalline material is shown as the bright yellow-red crystal. Estimated amorphous content is 98% or greater.

Figure 2. PHOTOMICROGRAPH OF ECOMELT (Work Performed by Construction Technologies Laboratories, Inc.)

!"""

'I : i ':'
" i
I

'

__

I
i

, __

29 (CuKa) Figure 3. XRD PATTERN OF ECOMELT*

A Hump in pattern confirms the Amorphous nature of Ecomelt. (Work Performed by Construction Technologies Laboratories, Inc.)

CONF\nENT\Al

COMMERCIAL
SINCE 19084J

TESTING & ENGINEERING CO.

FAX: 630-953-9306 Member of tile SGS Group (Societe Gen6rale de Surveillance) ADDRESS ALL CORRESPONDENCE TO: 16130 VAN ORUNEN RD.

GENERAL OFFICES: 1919 SOUTH HIGHLAND AVE.. SUITE 210-e. LOMBARD. ILLINOIS 60148 TEL: 630-953-9300

~ SGS

May 30, 2000

SOUTH HOlLAND, IL 60473

TEL: (708) 331-2900 FAX: (708) 333-3060

ENDESCO SERVICES, INC. 1700 S. MOunt Prospect Road Des Plaines, IL 60018 Attn: Anil Goyal, PhD, PE

Sample identification by Endesco Services, Inc.

Kind of sample reported to us Sample taken at Sample taken by Date sampled Date received

Fly

Ash

-----Endesco Services, Inc_

Sample ID:

ARV1

-----May 24, 2000

Analysis Report No.

71-122841

Page

of

Dry Basis

, Carbon !!tl!!m
Carbon: ASTM D 5373

3.76

Respectfully submitted,

e:HoI:OO~ .
~ Watermarked For Your Protection

~NGgENOl~:'J

ME M B E R

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-\

OVER 40 BRANCH LABORATORIES STRATEGICALLY LOCATED IN PRINCIPAL COAL MINING AREAS, TIDEWATER AND GREAT LAKES PORTS, AND RIVER LOADING FACtUTlES

mws AND CONDI'TlONS ON REVERSE

COMMERCIALTESTING.
SINCE

ENGINEERING CO.
ADDRESS AlL CORRESPONDENCE TO: 16130 VAN DRUNEN RD. SOUTH HOLlAND, IL 60473 TEL: (708) 3312900 FAX: (708) 333-3060

GENERAL OFFICES: 1919 SOUTH HIGHlAND AVE.. SUITE 210-8. LOMBARD. ILLINOIS 60148 TEL: 630-953-9300 FAX: 630-953-9306 19080

~ SGS

Member of the SGS Group (Socl6t6 Gt!Mrale de Surveillance)

May 30, 2000 ~ ENDESOO SBRVICES, INC. 1700 S. Mount Prospect Road Des Plaines, IL 60018 Attn: Anil Goyal, PhD, PB

Sample identification by Bndesco Services, Inc.

Kind of sample reported to us Sample taken at Sample taken by Date sampled Date received

Fly Ash

-----Endesco Services, Inc.

Sample ID:

ARV2

-----May 24, 2000

Analysis Report No.

71-122842

Page

of

Dry Basis

, Carbon
METHOD Carbon: ASTM D 5373

3.0B

r
OVER 40 BRANCH LABORATORIES smATEGICAU.~
t#nal Watennarked For Your Protection

Respectfully submitted.

MERCIAL TESTING & ENGINEERING CO. c

c.

~.

/J~'

MEMBER

South Holland Laboratory

LOCATED IN PRINCIPAL COAL MINING AREAS, TIDEWATER AND OREAT LAKES PORTS, AND RIVER LOADING FACILITIES

TERMS AND CONOIT1ONS ON REVERSE

COMMERCIAL
SINCE '908~

TESTING & ENGINEERING

Member of the SGS Group (Societe Generale de Surveillance)

CO.

GENERAL OFFICES: 1919 SOUTH HIGHLAND AVE" SUITE 210-B, LOMBARD, ILLINOIS 60148 TEL: 630-953-9300

FAX: 630-953-9306

"BGB
September 15, 2000

Committed To Excellence

ENDBSCO SBRVZCBS, INC 1700 S. Mount Prospect Road Des Plaines, IL 60018 Attn: Anil Goyal, PbD, PB

ADDRESS ALL CORRESPONDENCE TO: 16130 VAN DRUNEN RD. SOUTH HOLLAND, IL 60473 TEL: (708) 331-2900 FAX: (708) 333-3060

Sample identification by Bndesco Services, Inc.

Kind of sample reported to us Sample taken at Sample taken by Date sampled Date received

Bcomelt Sample ID: -----Bndesco Services, Inc. -----September 6, 2000 Analysis Report No. 71-131591 Page 1 of 3 Bcomelt from AVR Fly Ash

TOTAL ANALYSIS: JIB'l'ALS PARAMETER CAS NO. RESULT 9.1 730 6.9 210 96
NO

FLG RLIMIT UNITS S METHOD 0.75 0.15 0.15 0.75 0.75 0.75 0.75 0.75 0.75 0.75 1.10 lng/Kg lng/Kg mg/Kg mg/Kg mg/Kg mg/'Kg lng/Kg lng/Kg mg/Kg mg/Kg lng/Kg SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 7471

DATE/TIME/ANALYST 09/13/00 09/13/00 09/13/00 09/13/00 09/13/00 09/13/00 09/13/00 09/13/00 09/13/00 17:05 17:05 17:05 17:05 17:05 17:05 17:05 17:05 17:05 JWJ JWJ JWJ JWJ JWJ JWJ JWJ JWJ JWJ

DJ:LF 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0

Arsenic, As [7440-38-2] Barium, Ba [7440-39-3] cadmium, Cd [70640-43-9] Chromium, Cr [7440-47-3] Lead, Pb (7439-92-1] Selenium, Se [7782-49-2] Silver, Ag [7440-22-4] Antimony, Sb [7440-36-0] Molybdenum, Me [7439-98-7J Vanadium, V [744-62-2] Mercury, Hg
NO:

09/13/00 17:05 JWJ 1.0

3.7

40
23

19
NO

[7439-97-6]

09/11/00 16:03 JC2 1.0

Not detected at a concentration greater than LeO - Limit of Quantitation.

Method Reference: USBPA: Test Methods For Bvaluating Solid Waste; SW-846, 3rd Bdition; Nov 1986. TCLP Extraction Procedure and Regulatory Levels: 40CFR; Part 261.24 and Appendix II.

Respectfully submitted, COMMERCIAL TESTING

& ENGINEERING

CO,

MEMBER

r
OVER 40 BRANCH lABORATORIES

oulh Holland Laboratory

6:

~I "--N"'Ud

~
LOADING FACIUTIES

STRATEGICAlLY LOCATED IN PRINCIPAL COAL MINING AREAS, TIDEWATER AND GREAT LAKES PORTS, AND R

F465

Original watermarked For Your Protection

TEAMS AND CONDIllONS ON REVERSE

COMMERCIAL
GENERAL SINCE 19088 OFFICES; 1919 SOUTH HIGHLAND

TESTING & ENGINEERING

AVE . SUIlE 210-8. LOMBARD. ILLINOIS 60148' TEL: 630-953-9300

CO.

FAX; 630-953-9306

~5iG5i

Member of the SGS Group (Societe Gllnerale de SUrveillance)

Committed

To Excellence

ADDRESS All

CORRESPONDENCE TO:

16130 VAN DRUNEN RD.

september 15, 2000 ~ ENOESCO SBR~CBS, INC. 1700 S. MOunt Prospect Road Des Plaines, IL 60018 Attn: Anil Goyal, PhD, PE

SOUTH HOllAND. Il 60473 TEL: (708) 331-2900

FAX; (70B) 333-3060

Sample identification by Endesco Services, Inc.

Kind of sample reported to us Sample taken at Sample taken

by

Ecamelt Sample ID: -----Bndesco Services, Inc. -----September 6, 2000 Ecamel t from AVR. Fly Ash

Date sampled Date received

Analysis Report Ho.

71-131591

Page

2 of

TOXICI"rY CHARAC'1'BRISTICLEACHATE PROCBDtJRB: HB'.rALS PARAMETER CAS NO. RESULT FLG RLIMIT UNITS S METHOD 0.10 0.050 0.020 0.050
0.10

DATE/Tr.ME/ANALYST DILF 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 08:12 08:12 08:12 08:12 08:12 08:12 08:12 08:12 08:12 08:12 CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS 1.0 1.0
1.0

ArseniC, As [7440-38-2] Barium, Ba [7440-39-3] cadmium, Cd [7440-43-9] Chramium, Cr [7440-47-3] Lead, Pb [7439-92-1] Selenium, Se [7782-49-2} silver, Ag [74040-22-4] Antimony, Sb [7440-36-0] Molybdenum, Mo (7439-98-7] Vanadium, V [744-62-2] Mercury, Hg
ND:

NO u 0.065
NO

u
U

NO NO
NO

0.20

NO NO NO NO NO

u 0.20

u 0.020

u 0.10 u 0.050

mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L

SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW7470

1.0 1.0 1.0 1.0 1.0

1.0

1.0

[7439-97-6]

u 0.0020 mg/L

09/13/00 16:05 JC2 1.0

Not detected at a concentration greater than LOQ - Limit of Quantitation.

Method Reference: OSEPA: Test Methods For Evaluating Solid Waste; SW-846, 3rd Edition; Nov 1986. TCLP Extraction Procedure and Regulatory Levels: 40CFR; Part 261.24 and Appendix II.

Respectfully submitted, COMMERCIAL TESTING & ENGINEERING CO.

t;;/
OVER 40 BRANCH LABORATORIES STRATEGICALLY LOCATED F--486
IN

,/.7)'

(J ,tt>~.
t,

/? 0_

(._"~""-<

~ /
,
"t-'

~, \~ t. (,u-t.. '\ \\

~.

South Holland Laboratory

'J
LOADING FACIUTIES

PRINCIML COAL MINING AREAS, nDEWATER AND GREAT LAKES PORTS, AND

~ER

Original Watennarked

For

Your Protection

TERMS CONDITIONS ON REVERSE AND

COMMERCIAL TESTING & ENGINEERING CO.

GENERAl OFFICES: 1919 SOUTH HIGHlAND AVE., SUIT!; 210-B, LOMBARD, IWNOIS 60148. TEL: 630-953-9300 FAX:630-953-9306 SINCE 1908@

Ii'SGS

Member of the SGS Group (Societe Generale de Surveillance)

Committed

To Excellence

September 15, 2000 ~ BNDBSCO SERVICES, INC. 1700 S. MOunt Prospect Road Des Plaines, IL 60018 Attn: Anil Goyal, PhD, PH

ADDRESS ALL CORRESPONDENCE TO: 16130 VAN DRUNEN RD. SOUTH HOLlAND, IL 60473 TEL: (708) 331-2900 FAX: (708) 333-3060

Sample identification by Bndesco Services, Inc.

Kind of sample reported to us Sample taken at Sample taken by Date sampled Date received

Bcomelt Sample ID: -----Bndesco Services, Inc_ -----September 6, 2000 Analysis Report No. 71-131591 Page
3 of 3

Ecomelt from AVR Fly Ash

'l'OltICITr CBARACTBRISTIC LBACRATB PROCBDURB: METALS LEACHATB KATRU SPID PARAMETER CAS NO. RBSULT 2.0 100 9.8 98 2.0 101 2.0 102 2.0 99
2.0

FLG RLIMIT UNITS S METHOD mg/L , RBC 0.010 mg/L t RBC 0.020 mg/L t RBC 0.050 mg/L t RBC 0.10 mg/L t RBC mg/L 0.20 t RBC mg/L 0.020 , RBC 0.20 mg/L t RBC 0.10 mg/L t RBC 0.050 mg/L 0.00020 , RBC 0.0020 0.10 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW6010 SW7470 SW7470

DATE/TIME/ANALYST 09/14/00 09/14/00 09/14/00 09/14/00

09/14/00

DILF 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0
1.0

Arsenic, As Arsenic, As Barium, Ba Barium, Ba Cadmium, Cd Cadmium, Cd Chromium, Cr Chromium, Cr Lead, Pb Lead, Pb Selenium, Se Selenium, Se Silver, Ag Silver, Ag Antimony, Sb Antimony, Sb Molybdenum, Mo Molybdenum, Me Vanadium, V vanadium, V Mercury, Hg Mercury, Hg

(7440-38-2] (7440-38-21 (7440-39-3J

[7440-39-3]

08.20 08:20 08:20 08:20

08:20

(7440-43-9] [7440-43-9] (7440-47-3] [7440-47-3] (7439-92-1) [7439-92-1J [7782-49-2] [7782-49-2] [7440-22-41 [7440-22-4) [7440-36-0J [7440-36-0) [7439-98-7] (7439-98-7] (7440-62-2] (7440-62-2J (7439-97-6J [7439-97-6]

102 2.1 107 2.0 100 2.0 100 2.0 101 0.0020 98

09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00 09/14/00
09/14/00

08:20 08:20 08:20 08:20 08:20 08:20 08:20 08:20 08:20 08:20 08:20
08:20

09/14/00 08:20 09/14/00 08:20 09/14/00 08:20

CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS CBS

1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0

mg/L
, RBC

09/13/00 16.07 JC2 1.0 09/13/00 16:07 JC2 1.0

Respectfully submitted, COMMERCIAL TESTING & ENGINEERING CO.

6:
F...as
Original Watermarted For Your Protection

~<4~~.
MEMBER
LOADING FACILITIES

OVER 40 BRANCtf LABORATORIES STRATEGICALLY LOCATED IN PRINCIPAL COAL MINING AREAS, TIDEWATER AND GREAT LAKES PORTS, AND ~ER

TERMS AND CONDITIONS ON REVERSE