r/EPA
/109 / May 2015 / www.epa.gov/research
United States
Environmental Protection
Agency
Secondary Aluminum
Processing Waste:
Salt Cake Characterization and
Reactivity
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Office of Research and Development
National Risk Management Research Laboratory
Land Remediation and Pollution Control Division
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Notice
The U.S. Environmental Protection Agency through its Office of Research and Development partially
Funded and collaborated in the research activities described herein under Cooperative Research and
Development Agreement Number 0189-00 with the Aluminum Association and under contract numbers
EP-C-05-056 and EP-C-11-006 with Pegasus Technical Services, Inc. This report has been subject to both internal and
external Agency review and has been approved for publication as a U.S. EPA document.
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Foreword
The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting the Nation's land, air, and
water resources. Under a mandate of national environmental laws, the Agency strives to formulate and implement
actions leading to a compatible balance between human activities and the ability of natural systems to support and
nurture life. To meet this mandate, EPA's research program is providing data and technical support for solving
environmental problems today and building a science knowledge base necessary to manage our ecological resources
wisely, understand how pollutants affect our health, and prevent or reduce environmental risks in the future.
The National Risk Management Research Laboratory (NRMRL) is the Agency's center for investigation of
technological and management approaches for preventing and reducing risks from pollution that threatens human
health and the environment. The focus of the Laboratory's research program is on methods and their cost-effectiveness
for prevention and control of pollution to air, land, water, and subsurface resources; protection of water quality in
public water systems; remediation of contaminated sites, sediments and ground water; prevention and control of
indoor air pollution; and restoration of ecosystems. NRMRL collaborates with both public and private sector partners
to foster technologies that reduce the cost of compliance and to anticipate emerging problems. NRMRL's research
provides solutions to environmental problems by: developing and promoting technologies that protect and improve the
environment; advancing scientific and engineering information to support regulatory and policy decisions; and
providing the technical support and information transfer to ensure implementation of environmental regulations and
strategies at the national, state, and community levels.
This publication has been produced as part of the Laboratory's strategic long-term research plan. It is published and
made available by EPA's Office of Research and Development to assist the user community and to link researchers
with their clients.
Cynthia Sonich-Mullin, Director
National Risk Management Research Laboratory
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Executive Summary
Aluminum is a ubiquitous, highly utilized non-ferrous metal, employed in a wide range of products. Unlike other
metals, aluminum can be almost completely recycled into new products through a series of processes that re-melt
aluminum to produce aluminum ingots at secondary aluminum processing (SAP) facilities. Solid residues generated by
the aluminum melting processes are often referred to as aluminum dross, which forms on the surface of molten
aluminum through contact with oxygen during melting, holding, refining, and transfer processes. Dross obtained from
primary melting operations (also known as "white dross") consists primarily of aluminum oxide (with some oxides of
other alloying elements, such as magnesium and silicon) and may contain from 15 to 70% recoverable metallic
aluminum. Dross from secondary smelting operations (also known as "black dross") typically contains a mixture of
aluminum/alloy oxides and slag (a partially amorphous solid by-product of the smelting process) and contains
approximately 12 to 18% recoverable aluminum.
Commercial smelting of both white and black dross is often completed in a rotary salt furnace. The nonmetallic
byproduct residue that results from such furnace slag is frequently termed "salt cake", and contains only 3 to 10%
residual metallic aluminum. The formation of salt cake and the amount of salt cake formed depend on several factors
such as type and quality of input material (e.g., aluminum scraps), operating conditions, and technology applied.
Traditionally, salt cake from SAP facilities is disposed of into municipal solid waste landfills, with an annual disposal
quantity of approximately one million tons in the United States (U.S.). Worldwide, the aluminum industry produces
nearly five million tons of furnace waste (salt cake and baghouse dust) each year and this figure is tied to overall
aluminum consumption. There is a need to treat and dispose of the waste from aluminum production as well as to
reduce the generation and disposal of by-products from aluminum recycling in both the U.S. and in other countries
around the world.
Given the potential concern associated with the reactivity of salt cake in a landfill environment, the U.S. EPA initiated
a collaborative research effort with the Aluminum Association and the Environmental Research and Education
Foundation to characterize salt cake waste material and investigate its reactivity under controlled conditions. This
report presents the first systematic study on the characteristics and reactivity of salt cake derived from operating SAP
facilities in the U.S.
The specific objectives of the study were to:
• Identify and characterize the metal constituents in salt cake
• Investigate the leaching behavior of metals from salt cake following its reaction with water
• Identify the dominant crystalline mineral phases in salt cake
• Evaluate factors that impact the reactivity of salt cake
• Evaluate salt cake reactivity with water
Thirty-nine salt cake samples were collected from 10 SAP facilities across the U.S. The facilities were identified by
the Aluminum Association to cover a wide range of processes. Results suggest that while the percent metal leached
from salt cake was relatively low, the leachable metal content may still pose a contamination concern and potential
human and ecological exposure if uncontrollably released to the environment. As a result, salt cake should always be
managed at facilities that utilize synthetic liner systems with leachate collection (the salt content of the leachate will
increase the hydraulic conductivity of clay liners within a few years of installation). The mineral phase analysis
showed that various species of aluminum are present in the salt cake samples with a large degree of variability. The
relative abundance of various aluminum species was evaluated but it is noted that the method used is a semi-
quantitative method and as a result there is a limitation for the data use. The analysis only showed a few aluminum
species present in salt cake which does not exclude the presence of other crystalline species, especially in light of the
variability observed in the samples.
Results presented in this document are of particular importance when trying to understand concerns associated with
the disposal of salt cake in municipal solid waste (MSW) landfills. From the end-of-life management perspective, data
presented here suggest that salt cake should not be size reduced before disposal. Also, care should be taken not to size
reduce it after disposal by compacting it with heavy bulldozers. The MSW decomposition process is exothermic and as
a result MSW landfill temperatures are typically greater than 37°C and may reach 50°C or greater. The elevated
temperatures present in most MSW landfills can be conducive and could initiate salt cake reactions that otherwise may
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not take place. Furthermore, elevated temperatures can increase the rate of the salt cake reaction which further
propagates the salt cake reaction. Even outside of MSW landfills, once a salt cake reaction starts, it may self-propagate
and increase the rate at which the reaction occurs. While the heat generation potential per gram of salt cake sample is a
sample specific parameter, the results presented herein suggest that higher environmental temperatures tend to
intensify the salt cake reaction. This means that with increasing temperature the rate of salt cake reaction will also
increase. As stated earlier, this is of particular significance for the disposal of salt cake. Depending on their design and
capacity, MSW landfills tend to be well insulated and operate at elevated temperatures. When these conditions exist,
the reaction of salt cake with liquids tends to become more problematic since the elevated temperatures in MSW
landfills may initiate the salt cake reaction and the insulating properties of the MSW may further intensify the reaction.
Furthermore, the propagation effect that has been stated earlier can also magnify the impact of the reaction.
At elevated temperatures encountered in MSW landfills, elevated levels of hydrogen gas may be generated as a result
of salt cake reactivity and will be of concern. Hydrogen is an explosive gas and can potentially cause fires. Hydrogen
is even of greater concern if generated in MSW landfills. Apart from being a fire hazard when mixed with methane,
landfill gas collection systems are not designed to handle hydrogen since MSW landfill gas generally consists of
methane and carbon dioxide at ~ 50/50 ratio. Like hydrogen, methane is an explosive gas and care must be taken if salt
cake reacts with liquids. But unlike hydrogen, in an MSW landfill, the gas collection system is designed to handle
methane gas which is a greenhouse gas generated during the anaerobic decomposition of MSW. Since the full
combustion of methane needs more oxygen than that of hydrogen, this unstable composition of landfill gas can make
trouble for its application and management. From a human health perspective, the concentration of ammonia gas
produced from the salt cake reaction was relatively high and can potentially be of concern. However, the level of
ammonium resulting from the salt cake reaction is significantly lower compared to the levels found in landfills and as
a result, the ammonia generated from salt cake might not have a detrimental impact on the performance of MSW
landfills.
The samples of salt cake analyzed in this study represented a range of processes that produce these materials at SAP
facilities. Testing was conducted under a controlled set of laboratory conditions and represent a broad yet detailed
characterization of different salt cakes including, resultant products following reaction with water. The data generated
during this effort will help to support future, further characterization efforts which may ultimately be used to better
predict the ultimate impacts of disposing salt cake from SAP facilities in landfills. This may possibly help identify
operational techniques and procedures to minimize these impacts.
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Table of Contents
1. INTRODUCTION 1
2. METHODOLOGY 6
2.1 Sample Collection and Preparation 6
2.1.1 Field Sampling 6
2.1.2 Salt Cake Sample Processing 6
2.2 Salt Cake Characterization 7
2.2.1 Physical Properties 7
2.2.1.1 Moisture Content (MC) 7
2.2.1.2 Water Holding Capacity (WHC) 7
2.2.1.3 pH and Electrical Conductivity (EC) 7
2.2.2 Chemical Properties of Salt cake 7
2.2.2.1 Total Elemental Analysis 7
2.2.2.2 Leachate Elements Analysis 8
2.2.2.3 Toxicity Characteristic Leaching Procedure (TCLP) 8
2.2.2.4 X-ray Diffraction (XRD) Analysis 8
2.3 Reactivity of Salt cake 9
2.3.1 Apparatus for Testing Salt Cake Reactivity 9
2.3.2 Factors Impacting Salt Cake Reactivity 11
2.3.2.1 Effect of Environmental Temperature 11
2.3.2.2 Effect of Salt Cake Particle Size 11
2.3.2.3 Effect of Liquid Addition Rate 11
2.3.2.4 Effect of Liquid Chemical Composition 12
2.3.2.5 Effect of Liquid to Solid Ratio and Mass of Salt Cake 12
2.3.2.6 Effect of Aluminum Species in Salt Cake Simulators 12
2.3.3 Salt Cake Reactivity Evaluation 13
2.3.3.1 Temperature Increase 13
2.3.3.2 Heat Generation Potential 14
2.3.3.3 Gas Generation Potential 15
2.3.3.3.1 Gas Volume 16
2.3.3.3.2 Gas Composition 16
2.3.3.3.3 Gas Productivity 16
2.4 Statistical Analysis 17
2.5 Quality Metrics 18
3. PHYSICAL AND CHEMICAL PROPERTIES 21
3.1 Moisture Content 21
3.2 Water Holding Capacity 21
3.3 pH and Electrical Conductivity 22
3.4 Total Extractable Metals 24
3.4.1 Aluminum (Al) Content 24
3.4.2 Major Metals Content 24
3.4.3 Trace Metals Content 25
3.5 Leachable Elements from Salt Cake 26
3.5.1 Leachable Aluminum (Al) 27
3.5.2 Leachable Major Metals 27
3.5.3 Leachable Trace Metals 28
3.6 Results of TCLP 29
3.7 Crystalline Mineral Phases of Salt Cake 29
3.7.1 Non-Aluminum Mineral Phases 30
3.7.2 Aluminum Crystalline Phases 31
3.7.2.1 Metallic Aluminum 31
3.7.2.2 Aluminum Nitride and its Oxides 32
3.7.2.3 Aluminum Oxides 32
3.7.2.4 Elpasolite and Spinel 33
3.8 Conclusions 33
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4. SALT CAKE REACTIVITY 34
4.1 Factors Impacting Salt Cake Reactivity 34
4.1.1 Environmental Temperature 34
4.1.2 Particle Size 37
4.1.3 Liquid Addition Rate 38
4.1.4 Liquid Composition 39
4.1.5 Liquid to Solid Ratio and Mass of Salt Cake 40
4.1.6 Aluminum Speciation 43
4.2 Reactivity Indices 46
4.2.1 Maximum Temperature Change 46
4.2.2 Time to Reach the Maximum Temperature 47
4.2.3 Heat Generation Potential 48
4.2.4 Gas Generation Potential 49
4.2.4.1 Hydrogen 49
4.2.4.2 Methane 51
4.2.4.3 Ammonia 52
4.2.4.4 Nitrous Oxide 54
5. CONCLUSION 56
5.1 Salt Cake Characteristics 56
5.2 Salt Cake Reactivity 57
5.3 Implications 58
6. REFERENCES 60
7. APPENDIX
A. MDL andMRL for Metal and Gas Analysis 62
B. Physical and Chemical Properties of Salt Cake 63
C. Mineral Analysis (XRD Data) of Salt Cake 102
D. Temperature Profiles of Salt Cake 352
E. Gas Productivity of Salt Cake 380
F. QAPP F-l
VII
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List of Figures
Figure 1 -1: The formation of salt cake 2
Figure 2-1: Water holding capacity method illustration 7
Figure 2-2: Temperature increase apparatus 9
Figure 2-3: Heat measurement apparatus 10
Figure 2-4: Reactivity test apparatus for gas generation measurement 10
Figure 2-5: Sample arrangement in an insulation box for temperature change experiment 14
Figure 2-6: Example of calibration curve for heat calculation 15
Figure 2-7: Examples of mean diamonds and box plot 18
Figure 3-1: Salt cake moisture content and its distribution 21
Figure 3-2: Salt cake water holding capacity and its distribution 22
Figure 3-3: Salt cake pH and its distribution 23
Figure 3-4: Salt cake EC and its distribution 23
Figure 3 -5: Correlation of potassium by different methods 3 0
Figure 4-1: Impact of environmental temperature on maximum temperature change 34
Figure 4-2: Schematic describing self-propagation of salt cake reaction 36
Figure 4-3: Effect of particle size on salt cake reactivity 37
Figure 4-4: Temperature change as a function of (a) watering schedule and (b) salt cake mass 39
Figure 4-5: Liquid composition impact on salt cake reactivity 40
Figure 4-6: Impact of liquid to solid ratio on temperature change and time to reach maximum temperature 41
Figure 4-7: Effect of liquid to solid ratio on gas production of SC reaction 42
Figure 4-8: Effect of liquid to solid ratio on gas composition of SC reaction 42
Figure 4-9: Effect of the mass of salt cake on (a) ATmax and (b) heat generation potential 43
Figure 4-10: Temperature increase after the addition of (a) Al (b) A1N (c) Al4Cs in SC stimulators 43
Figure 4-11: The impact of the addition of A1N and Al4Cs in SC simulators on the temperature changes 44
Figure 4-12: The role of A12O3 in SC simulators on the temperature changes 45
Figure 4-13: The role of A1N in SC simulators on heat generation potential at 50 °C 46
Figure 4-14: Correlation between ATmax and heat generation 48
Figure 4-15: Correlation between gas volume generated and heat generation 49
Figure 4-16: Distribution of hydrogen concentration from gas generated by salt cake reaction 50
Figure 4-17: Relationship between (a) H2 productivity and ATmax, and (b) H2 productivity and heat generation 51
Figure 4-18: Variability of percentage of unreacted metallic aluminum in SC after gas experiments 51
Figure 4-19: Distribution of methane concentration from gas generated by salt cake reaction 52
Figure 4-20: Distribution of ammonia after salt cake reaction (a) NH3(gas), and (b) NH4+ 53
Figure 4-21: Distribution of the total ammonia productivity and unreacted A1N in SC after gas experiments 54
Figure 4-22: Relationship between the productivity of total NH3 and N2O from salt cake reaction 55
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List of Tables
Table 1-1: Approximate composition of Aluminum by-products 1
Table 2-1: SAP waste (salt cake) facility and sample identification list 6
Table 2-2: Spike recovery for metals 8
Table 2-3: Treatments for testing the effect of liquid composition on salt cake reactivity 12
Table 2-4: Treatments for testing the effect of liquid to solid ratio and mass of salt cake on the reactivity 13
Table 2-5: Composition of the SC stimulators for testing the impact aluminum species on the reactivity 14
Table 2-6: Calculations of heat generation from a fixed resistance and EAT 15
Table 2-7: Summaries of QA/QC Checks 20
Table 3-1: Salt cake moisture content 21
Table 3-2: Salt cake water holding capacity 22
Table 3-3: Salt cake pH 22
Table 3-4: Salt cake electrical conductivity 23
Table 3-5: Extractable Al content in salt cake 24
Table 3-6: Major metals content in salt cake 24
Table 3-7: Trace metal content in salt cake 25
Table 3-8: Leachable aluminum 27
Table 3-9: Major metal teachability from salt cake 27
Table 3-10: Trace metal concentration in leachate of salt cake 28
Table 3-11: Metal concentration in the TCLP solution 29
Table 3-12: Non-aluminum mineral phases in salt cake 30
Table 3-13: Aluminum crystalline phases in salt cake 31
Table 4-1: Impact of environmental temperature on heat generation potential 36
Table 4-2: Impact of environmental temperature on gas generation potential 37
Table 4-3: Effect of particle size on ATmax and tmax-T 37
Table 4-4: Effect of particle size on heat generation potential 3 8
Table 4-5: Effect of particle size on salt gas productivity 3 8
Table 4-6: Impact of liquid composition on ATmax and tmax-T 39
Table 4-7: Gas generation potential as a function of liquid composition 39
Table 4-8: Impact of liquid composition on heat generation potential 40
Table 4-9: Impact of liquid to solid ratio and leachate composition on heat generation potential 41
Table 4-10: Impact of aluminum speciation on temperature change in SC simulators 44
Table 4-11: Impact of aluminum speciation in SC simulators on the heat generation 45
Table 4-12: ATmax for salt cake reaction by facility 47
Table 4-13: tmax-T for salt cake reaction by facility 47
Table 4-14: Heat for salt cake reaction by facility at 37 °C 48
Table 4-15: Total generated gas volume from salt cake reactivity 49
Table 4-16: Hydrogen generation from salt cake reaction 50
Table 4-17: Methane generation from salt cake reaction 52
Table 4-18: Ammonia generation from salt cake reaction 53
Table 4-19: Nitrous oxide generation from salt cake reaction 54
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Acronyms and Abbreviations
AT = difference in temperature
EAT = sum of temperature change
AA = atomic absorption
AES = atomic emission spectroscopy
Al = aluminum
ANOVA = analysis of variance
ASTM =American Society for Testing and Materials
CHL = Center Hill Laboratory
DIW = deionized water
EC = electrical conductivity
BCD = electron capture detector
EPA = Environmental Protection Agency
EREF = Environmental Research and Education Foundation
GC = gas chromatograph
GFAA = graphite furnace atomic absorption
ICDD = International Centre for Diffraction Data
ICP = inductively coupled plasma
L/S = liquid to solid
MC = moisture content
MDL = method detection limit
MRL = method reporting limit
MSW = municipal solid waste
PDF = powder diffraction file
PVDF = polyvinylidene fluoride
RCRA = Resource Conservation and Recovery Act
SC = salt cake
SAP = secondary aluminum processing
TCD = thermal conductivity detector
TCLP = toxicity characteristics leaching procedure
UCL = upper confidence limit
U.S. = United States
VOA = volatile organic analyte
WHC = water holding capacity
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 1 of 478
1. INTRODUCTION
Aluminum is one of the most commonly used non-ferrous metals. Unlike other metals and recyclable commodities,
aluminum can be almost completely recycled into new aluminum products [ 1 -4]. Secondary aluminum processing
(SAP) involves the recycling and re-melting of scrap aluminum to reproduce aluminum alloys, which can produce
various types of waste, referred to as SAP wastes. The process of treating and disposing the waste from aluminum
production as well as the presence of byproducts of the aluminum recycling process is becoming not only a problem in
the U.S. [5-13], but globally [4, 14-20]. The main solid waste produced during aluminum processing in the U.S. is
referred to as salt cake (SC), and the SC from SAP is the subject of this report.
Aluminum is utilized in a large number of products, both alone or as a component of an alloy. The total amount of
aluminum production in the world was approximately 28 million tons (with over 8 million tons recycled from scrap) in
1990 and near 56 million tons (with close to 18 million tons recycled from scrap) in 2008. By 2020, aluminum metal
demand is projected to increase to around 97 million tons (including approximately 31 million tons recycled from
scrap) [4]. The total North American aluminum industry supply was 11.5 million tons in 2013, 41% of which came
from recycled aluminum [21]. The used beverage aluminum container recycling rate was 50% (52 billion cans) in
2006, and increased to 66.7% (60.2 billion cans) by 2013 [22]. Almost 90% of automotive aluminum, including
versatile aluminum alloys, is reclaimed and recycled [3]. But Americans still discarded about 2.9 million tons of
aluminum in the municipal solid waste (MSW) stream after recycling and recovery in 2012, totaling 1.4 percent of
total MSW discards [23]. Recycling scrap aluminum requires only 5% of the energy used to produce aluminum from
raw materials (i.e., ore), and avoids approximately 95% of the emissions associated with producing new aluminum
from ore [24-27]. The technologies used for SAP vary from one plant to another depending on the scrap type, oxide
content, impurities present, and other factors [3, 27, 28]. In the U.S., one popular method of producing secondary
aluminum is through the use of rotary furnaces with the addition of salt fluxes to improve recovery and reduce
oxidation of the aluminum metal [29 ]. Salt flux is a mixture of sodium chloride (NaCl) and potassium chloride (KC1)
with lower amounts of other compounds, such as calcium fluoride (CaF2) [14, 30-33]. Salt flux melts at a slightly
lower temperature than aluminum, and therefore coats the metal before it melts in the furnace and reduces aluminum
metal loss through oxidation. Additives in salt flux also penetrate and break down previously-formed aluminum oxide
layers and improve separation between aluminum metal and nonmetal material in the furnace [32-34].
Aluminum dross is a residue from aluminium melting activities. It is generated when impurities and oxidation layers
are skimmed from the top of molten metal during the melting, holding, and casting operations. The formation of dross
and the amount of dross formed depends on different factors, such as the type and quality of input material (e.g.,
aluminium scraps in secondary industry). Drosses obtained from primary melting operations (known as white drosses)
consist primarily of aluminum oxide (with some oxides of other alloying elements such as magnesium and silicon) and
may contain 15 to 70% recoverable metallic aluminum [3, 27, 29, 35, 36]. Drosses from secondary smelting operations
(black drosses) typically contain a mixture of aluminum/alloy oxides and slag, and typically contain recoverable
aluminum contents ranging from 12 to 18% [3, 27, 29, 35, 36]. Commercial smelting of both white and black dross is
often done in a rotary salt furnace. The nonmetallic byproduct residue, which results from such dross smelting
operations (SC or salt slag in Europe) contains 3 to 10% residual metallic aluminum [3, 27, 29, 35, 36] (Table 1-1).
Table 1-1: Approximate composition of Aluminum by-products [36]
Material % Metallic aluminum % Aluminum Oxide % Salt
White Dross
Black Dross
Salt Cake
15-80
7-35
3-10
20-85
30-50
20-60
0-1
30-50
20-80
The formation of SC and the amount of SC formed depends on different factors such as type and quality of input
material (e.g., aluminium scraps in secondary industry), operating conditions, type of technology, and furnace applied
[3, 27, 29, 35, 36]. It is believed that its formation involves the following steps: (a) surface oxidation, (b) crushing of
oxidic skin, (c) sinking and floating of oxide particles, (d) conglomeration of oxidic particles, (e) the filling of
interspatial areas by metallic aluminum, (f) inside oxidation of dispersed aluminium, (g) skimming of dross from melt
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 2 of 478
bath surface, and (h) metallic aluminum drip off and follow-up oxidation of solids during dross cooling, suggested by
Antrekowitsch [37] (Figure 1-1). Aluminum nitrides, carbides, and sulfides may also be present, as well as metal
oxides derived from the molten alloy [3, 27, 35, 36, 38].
n
n _ _
Figure 1-1: The formation of salt cake [37]
a) Surface oxidation
b) Crashing of oxidic skin
c) Sinking and floating of oxidic particles
d) Conglomeration of oxidic particles
e) The filling of interspatial areas by metallic aluminum
f) Inside oxidation of dispersed aluminum
g) Skimming of dross from melt bath surface
h) Metallic aluminum drip off and follow-up oxidation of solids during dross cooling.
Traditionally, SC has been disposed of in landfills. Almost one million tons of SC are placed in MSW landfills
annually in the U.S. [39]. Worldwide, the aluminum industry produces nearly five million tons of furnace waste (e.g.,
SC and baghouse dust) each year [28], and this number continues to grow with the increase in aluminum
consumption, especially from the SAP [40]. SC is recognized as a hazardous waste in European Union countries [41]
because it is considered to be "highly flammable" (Category H3-A) and an "irritant" (Category H4) [42] . When SC
comes in contact with water or damp air, highly flammable gases form. These gases can be explosive as well as act as
irritants to skin and mucous membranes. Furthermore, the SC particles have been found to be harmful if inhaled or
ingested (Category H5) [42]. SC is also in the category of substances that are capable, after disposal (landfill or other),
of potentially yielding another substance (e.g., leachate) which can possess any of the characteristics associated with
the solid SC or gaseous products (Category H13) [42]. Therefore, landfill disposal of SC can be costly and attempts in
Europe to landfill this type of waste are dwindling due to the lack of landfill space [43].
Because of aluminum's amphoteric properties (meaning it dissolves in both acid and alkaline solutions, generating
heat and gas), the disposal of large quantities of aluminum-containing SC can be problematic. The many forms of
aluminum (i.e., metallic aluminum (Al), aluminum nitride (AIM), aluminum carbide (Al4Cs), aluminium sulfide
(Al2Ss), and aluminum oxynitride (Al5OeN)) that may be contained in SC can undergo a wide range of potential
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 3 of 478
reactions after interacting with water during disposal. These reactions are listed in Equations 1-1 through 1-10:
2A1 + 2OH~ + 6H2O -> 2(A1(OH)4)~ + 3H2(g) t + heat (1-1)
Note that reaction 1-1 could only occur in alkaline solutions above a pH of 8. Metallic aluminum could also react
under acidic solutions to produce complex aluminum-containing ions and hydrogen gas in the following manner:
2A1 + 6H3O+ + 6H2O -> 2(A1(OH)6)3+ + 9H2(g) t + heat (1-2)
The presence of aluminum nitride and carbide in the SC is due to the reactions of molten aluminum with the different
gases during the melting process. These reactions include:
2A1 + N2(g) -> 2A1N (1-3)
6A1 + 3CO2(g) -> A14C3 + A12O3 (1-4)
4A1 + 3S02(g) -» A12S3 + A1203 (1-5)
The formation of aluminum nitride (A1N) in SC is a function of the melting duration, casting, and temperature. The
influence of temperature on the A1N composition in SC has been described [44]. When SC is generated at a
temperature of 700°C, the A1N content in SC is approximately 2% by weight. This concentration rises to around 18%
when formation occurs at approximately 1,000°C. Aluminum nitride and its oxide in SC have often been documented
in reviews and reports [3, 11, 16, 27, 36, 38, 45-49]. The formation of aluminum carbide is believed to occur at above
900°C [44], especially in the white dross form [36]. Aluminum carbide in SC has also been observed by some
investigators [3, 16, 49-51].
The reaction of aluminum nitride is also pH-dependent. Under alkaline conditions, the reaction products are aluminum
hydroxide and ammonium hydroxide (1-6):
A1N + 4H20 -> A1(OH)3 + NH4OH (1-6)
Under acidic conditions, below a pH of 8, the reaction proceeds to produce ammonia gas:
A1N + 3H2O -> A1(OH)3 + NH3(g) t (1-7)
Aluminum oxide nitride can also react with water to yield aluminum oxide and ammonia gas:
2A15O6N + 3H2O -> 5A12O3 + 2NH3(g) t (1-8)
Aluminum carbide can react with water to produce methane [52]:.
A14C3 + 12H20 -> 4A1(OH)3 + 3CH4(g) t (1-9)
Aluminum sulfide hydrolysis can also generate hydrogen sulfide [53]:
A12S3 + 6H20 -> 2A1(OH)3 + 3H2S(g) t (1-10)
As outlined earlier, various forms of aluminum may be present in SC waste, which can react with water to generate
flammable gases (e.g., hydrogen and methane). There is no current policy or guidance from the U.S. EPA for a
specific test to determine if SC exhibits the reactivity characteristic for the purpose of hazardous waste classification.
If there is a decision to test for reactivity, one type of testing in the U.S. that could be used as guidance for potential
testing protocol is the Department of Transportation's "Hazardous When Wet" test (CFR 173.124-Class 4) [54].
Hazardous When Wet material (Division 4.3) means a material that, when it contacts water, is liable to become
spontaneously flammable or to give off flammable or toxic gas at a rate greater than 1 L per kilogram of the material
per hour, when tested in accordance with the United Nations Manual of Tests and Criteria at an ambient temperature
(20°C) [54, 55]. Meanwhile, there is a requirement for generators to use "generator knowledge" in making the
reactivity characteristic determination. It is noted that the U.S. EPA does not classify aluminum processing waste as
ignitable, corrosive, reactive, or toxic (the four hazardous characteristic categories) at the present time. Therefore, U.S.
EPA regulations do not exclude aluminum processing waste from disposal in MSW landfills.
While, secondary aluminum processing waste may not meet the U.S. Federal definition of a hazardous waste, reactions
with leachate in MSW landfills have been documented and are of potential concern to engineered protective
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components of the landfill (e.g., bottom liners that capture leachate that percolates through the waste). In MSW
landfills, heat is generated as a result of biochemical processes and the decomposition of organic components in waste
[56]. Temperature is considered to affect waste decomposition in two ways: short-term effects on reaction rates and
long-term effects on the microbial population balance are expected [57]. In laboratory studies, optimum temperature
ranges for the growth of mesophilic and thermophilic bacteria involved in waste decomposition were identified to
range from 35 to 40°C and 50 to 60°C, respectively [58, 59]. There is no specific landfill design for the handling of SC
in the U.S.; most of the generated SC is still currently disposed of in MSW landfills (Subtitle D municipal and
industrial, non-hazardous waste), which are usually designed with liners to protect groundwater from contamination.
The liners are expected to provide this protection for the entire period of time that a landfill may contain leachable
chemicals, thus damage could result in a negative impact on the environment. The potential for groundwater
contamination by a landfill may continue to be a concern for many decades after the landfill has ceased waste disposal
operations. Current liner designs include a geomembrane and either a geosynthetic clay liner or a compacted clay liner.
As long as the geomembrane component of the composite liner retains its structural integrity, this barrier successfully
limits landfill leachate and gases from impacting groundwater and the surrounding environment. A geosynthetic clay
or compacted clay layer incorporated into a MSW landfill composite liner system may also lose this integrity when
exposed to a thermal gradient, which can induce desiccation and cracking of the clay layer. The potential for
desiccation of the clay layer results from thermal gradients, which can arise between the liner and the cooler ground
under the liner [60]. This becomes especially problematic if the geomembrane above the clay liner develops defects
such as cracks or holes as it ages because the clay liner then acts as the primary barrier to leachate. Benchtop
laboratory experiments have determined that the initial moisture content of the foundational soil below the clay liner is
a critical factor affecting the potential for clay liner desiccation, with lower initial subsoil water content resulting in
greater desiccation potential. In addition, the higher the temperature gradient a geosynthetic clay liner experiences, the
greater the potential for desiccation induced cracking. As seen with the geomembrane, a temperature of 60°C applied
to the top of a test cell will create a temperature gradient that increases the risk of desiccation [61]. There is currently
information available that suggests that engineered landfill components designed to protect the environment from
contamination by MSW landfills can develop significant problems over time due to exothermic biological activity and
exothermic reactions associated with other waste [62-64].
Some MSW landfills in the U.S. have reported operational challenges that may be attributable to reactions from SC
disposal, including:
• High subsurface temperatures
• Elevated gas flow, and hydrogen and ammonia concentration
• Nuisance odors with potential hazardous gaseous emissions
• Increased leachate volume with potential heavy metal contaminants
• Subsurface oxidation events
• Outbreaks of leachate from side slopes
• High rates of landfill settlement/subsidence
• Reduction in landfill gas collection efficiency
• Impacts to groundwater quality
As an example, aluminum processing waste disposed in an unlined landfill by the Recycled Aluminum Metals
Company (RAMCO) resulted in a host of issues. SC and a smaller amount of baghouse dust were placed in an unlined
landfill near Dallesport, WA, between 1982 and 1989. A Site Hazard Assessment conducted by the Washington State
Department of Ecology showed elevated concentrations of salt in the groundwater and borings beneath the landfill
surface showed elevated temperatures and the presence of ammonia gas. Measurements indicated that the composition
of the landfill included up to 29% aluminum, 8% sodium, 2.8% magnesium, 2.1% calcium, and 1.5% potassium, with
lesser amounts of metals such as chromium, manganese, iron, copper, nickel, and zinc present. Groundwater impacts
from nitrate, sodium, chloride, and total dissolved solids were also observed. Ultimately, the waste was removed from
the site and transported to a landfill in compliance with the liner and monitoring requirements of Resource
Conservation and Recovery Act subtitle D [6].
Another example is Brantley Landfill (Island, McLean County, Kentucky). Over a two-year period from 1978-1980, a
total of 250,306 tons of SC fines were deposited in the landfill (previously the site of a coal strip mine). Site
investigations found contamination in air, ground water, sediment, soil, and surface water that could potentially harm
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people in the area. Contaminants of concern included chromium, copper, titanium, vanadium, aluminum, magnesium,
and sodium, which react with water to form several gases, including ammonia, acetylene, methane, hydrogen,
and hydrogen sulfide. A number of options were evaluated as remedial treatments, including the removal of the waste
from the site. However, since the landfilled waste was 60 feet thick at its deepest point, this option would have
required special equipment and excavation techniques. It was determined that the waste would remain at the fenced in,
isolated location. A new landfill cap and an alkaline recharge trench were constructed, surface and groundwater were
monitored, and leachate was collected, treated and disposed off-site. The total cost of the remedial action was
projected to exceed $5,000,000, with an additional annual cost of $57,000 to $223,000 allotted for site monitoring [5].
SAP waste, placed in an MSW landfill, may result in an exothermic reaction upon contact with water, which can
initiate incomplete combustion or pyrolysis of other waste materials [11, 65, 66]. Aside from the potential impacts on
engineered systems relating to leachate collection, gas collection, and liner systems, there are potentially significant
environmental and community health impacts associated with air emissions and surface water/groundwater releases
from these reactions. For example, between 1993 and 2006, the County wide Recycling and Disposal Facility in East
Sparta, OH, accepted approximately 600,000 tons of aluminum processing waste, primarily aluminum dross and SC.
In 1998, Countywide began re-circulating leachate, and in 2001, elevated temperatures were detected in gas wells in
two cells of the landfill. Odor complaints were made by citizens in 2004, and so an odor suppression system was
installed in 2005. By the end of 2005, hundreds of odor complaints were again being filed and landfill gas wells were
showing elevated temperatures. In 2006, well temperatures were still increasing, leachate outbreaks were occurring,
accelerated settlement was observed and odor problems increased [7]. Numerous actions were taken during this period
to alleviate the problems. Leachate recirculation was halted; aluminum processing wastes were no longer accepted and
site monitoring actions were increased. Despite these and other efforts, the Ohio EPA concluded that a fire was
occurring in the landfill which involved the SAP wastes and the MSW. Although additional actions recommended or
required by the Ohio EPA and the U.S. EPA were implemented, evidence of a continuing subsurface reaction
involving the aluminum processing waste and water was observed in 2008, which may also have caused pyrolysis of
landfilled MSW. Acetylene, hydrogen, and carbon monoxide were also detected at the site along with methane.
Mixtures of these gases may cause an explosive atmosphere near the surface of the landfill [67]. In June 2009, a
remedial strategy involving the removal of the problematic areas within the landfill excavation was completed,
resulting in the extraction of approximately 400,000 cubic yards of waste. A liner was installed to cover the excavated
area to reduce contact by moisture and atmospheric oxygen [7].
In light of the issues that have been documented regarding SC disposal at unauthorized landfills and at Subtitle D
landfills, there is a need to more fully understand the conditions that lead to reaction of SC and the effect those
reactions have on landfill operation and landfill engineered components. The U.S. EPA initiated a collaborative
research effort with the Aluminum Association and the Environmental Research and Education Foundation (EREF) to
examine safe management practices for SC waste. The U.S. EPA is seeking to better understand SC waste material, its
potential risk, and strategies for safe management of municipal landfills. This research report presents a systematic
study on the characteristics of SC and evaluation of SC reactivity when exposed to liquid water. The specific study
objectives were as follows:
• Evaluate the physical and chemical properties of SC
• Evaluate the factors impacting SC reactivity
• Evaluate SC reactivity with liquids
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2. METHODOLOGY
2.1 Sample Collection and Preparation
Thirty nine SC samples were collected from 10 secondary aluminum processing facilities (designated as B, C, D, E, F,
H, J, L, M and N; Table 2-1). The facilities were identified in collaboration with the Aluminum Association and EREF
to cover a wide range of SAP processes.
Table 2-1: SAP waste (salt cake) facility and sample identification list
Sample
#
1
2
o
J
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Facility
B
B
B
B
C
C
D
D
D
D
E
E
F
F
F
F
F
H
H
H
Sample
ID
2452
2468
2478
2454
2433
2435
2532
2536
2538
2540
2437
2439
2502
2504
2506
2508
2510
2544
2555
2559
Date
Received
2/24/2010
2/24/2010
2/24/2010
3/19/2010
11/25/2009
12/28/2009
11/5/2009
1/15/2010
2/24/2010
3/19/2010
2/25/2010
2/24/2010
11/20/2009
12/28/2009
12/28/2009
2/24/2010
4/6/2010
11/13/2009
12/14/2009
1/11/2010
Sample
#
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
Facility
H
H
J
J
J
J
L
L
L
L
L
M
M
M
M
N
N
N
N
Sample
ID
2046
2568
2512
2515
2517
2519
2482
2484
2488
2486
2490
2601
2605
2609
2613
2492
2494
2496
2498
Date
Received
3/12/2010
2/12/2010
11/20/2009
12/2/2009
1/8/2010
2/5/2010
12/2/2009
12/28/2009
2/2/2010
2/2/2010
4/6/2010
2/24/2010
2/24/2010
3/8/2010
5/14/2010
12/28/2009
2/2/2010
3/8/2010
4/6/2010
2.1.1 Field Sampling
SC samples were collected by a designated third party at a storage area from each facility approximately once a month
for four months. After cooling (72 to 120 h), the stored materials were size reduced following ASTM Method C702 -
98: "Standard practice for reducing samples of aggregate to testing size" [68]. Each SC sample was collected using
pre-cleaned sampling equipment and divided into two fractions. The first fraction, approximately 1 kg sample, was
delivered to U.S. EPA's Center Hill Laboratory (CHL) Research Facility in a shipping container. The second sample
fraction (10 to 20 kg) was stored at the test site for further analysis, if needed, based on current findings.
2.1.2 Salt Cake Sample Processing
Upon receipt at CHL, samples were logged and stored in a storage unit. Within two weeks, individual samples were
processed by placing them into a stainless steel pan and crushing them to a size less than 9 mm by sieve. After
thorough mixing, approximately 500 g of the 9 mm sieved materials was further size reduced down to a size of 2 mm
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using a grinding machine. About 50 g of the 2 mm size SC sample was further reduced to a size of 0.05 mm using a
sealed stainless steel jar mill equipped with zirconia grinding beads. Any sample that was not used in the experiment
was returned to its original labeled container and placed in storage.
2.2 Salt Cake Characterization
2.2.1 Physical Properties
2.2.1.1 Moisture Content (MC)
MC of the SC samples was measured after the sample size was reduced to less than 2 mm. The samples were then
placed in an oven and moisture content was determined following ASTM Method D-2216 [69].
2.2.1.2 Water Holding Capacity (WHC)
WHC of the SC samples was measured using a modified ASTM Method F1815-06 [70]. Approximately 10 g of
sample (size < 2 mm) was placed into a cylinder (see Figure 2-1), and cold water (Temperature <12°C) was added to
saturate the sample. The saturated sample within the cylinder was placed on top of an absorbent membrane until the
excess water was drawn away by gravity. Once equilibrium was reached (usually in approximately 16 h), the WHC
was calculated based on the weight of the water held in the sample vs. the sample's dry weight. Note that the WHC
data must be used with caution because of the reactions that can occur when the SC is mixed with water.
Absorbent Membrane
Figure 2-1: Water holding capacity method illustration
2.2.1.3 pH and Electrical Conductivity (EC)
The pH and EC of the SC samples (< 2 mm) were measured after the sample reacted with deionized water (DIW) at
50°C for 5d of incubation in a closed system with a gas capture apparatus. The liquid to solid ratio was 20 to 1 (100 ml
DIW/5g). After filtering by using a 0.45-um polyvinylidene fluoride (PVDF) media, pH and EC were measured
directly using a hydrogen ion selective electrode and conductivity probe following Standard Methods for the
Examination of Water and Wastewater (Standard Method 4500-H pH Value, 2510 Conductivity) [71], respectively.
Both the pH and conductivity meters were calibrated before analysis.
2.2.2 Chemical Properties of Salt cake
2.2.2.1 Total Elemental Analysis
The SC samples (< 0.05 mm) were acid digested following EPA Method 3051A [72]. Because of the need for
aluminum quantification, a mixture of hydrochloric and nitric acid (1 part HC1 and 3 parts HNOs) was employed.
Furthermore, the microwave temperature was set at 185°C for 30 min rather than the 175°C for 10 min that is
specified in the method to increase the recovery of aluminum. The weight of the SC samples was approximately 0.1 g
instead of the 0.5 g called for by Method 3051 A. After acid digestion, major metal composition (Al, Ca, Cu, Fe, K,
Mn, Na, S, and Zn) was measured via EPA Method 60IOC using a Thermo inductively coupled plasma atomic
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emission spectroscopy (ICP-AES) [73]. Analysis of As, Cd, Cr, Pb, and Se was conducted using a Perkin-Elmer
graphite furnace atomic absorption spectrometry (GFAA) (EPA Method 7010) [74]. The method detection limits
(MDL) for metals in aqueous phase and the method reporting limit (MRL) for metals in solid phase for ICP are
presented in Appendix A (Table A-l). Standard reference material 1633b (Coal Fly Ash), blank spikes and SC samples
spikes were also digested during each batch for quality control. The average recovery of spiked Al, K, Na, and Mg in
the blank, 1633b, and SC samples (2452-B, 2433-C, 2502-F, 2046-H, 2512-J, 2490-L, and 2613-M) are presented in
Table 2-2.
Table 2-2: Spike recovery for metals
Recovery (%)
Metal R1 Reference material Salt cake samples
,^ s'swt \ s T\
(1633b) (n=7)
Al
K
Na
Mg
104
93
97
102
103
94
105
103
96±14
98±11
85±4.0
100±4.5
2.2.2.2 Leachate Elements Analysis
Leachable elements (Al, Fe, Mg, Cu, Zn, K, Na, Ca, Mn, Pb, Cr, As, Se, Cl and F), following the mixing of SC with
water during 5d-long incubation at 50°C (5 g SC to 100 ml DIW in a 500 ml bottle), were analyzed using Thermo ICP-
AES using EPA Method 60 IOC [73] for the macro metals, Perkin-Elmer graphite furnace AA for trace metals by EPA
Method 7010 [74], and 1C for anions using EPA Method 300.1 [75]. The leachate was filtered using 0.45-um PVDF
media. The MDL and MRL for the metal analysis using GFAA are presented in Appendix A (Table A-2). Due to the
high quantity and variation of sodium and aluminum in the leachate, a standard addition method for GFAA analysis
was employed for leachate As, Cr, Pb and Se [76, 77].
2.2.2.3 Toxicity Characteristic Leaching Procedure (TCLP)
The toxicity characteristics leaching procedure (TCLP) was conducted as prescribed in U.S. EPA Method 1311 [78].
Two different extraction fluids were employed based on the buffering capacity of each sample. The TCLP extracts
were digested following EPA Method 3015A after filtration and acidification (pH < 2.0) and the concentrations of
metals were analyzed using Thermo ICP-AES [73]. Of the eight Resource Conservation and Recovery Act (RCRA)
toxicity characteristic metals, mercury was not analyzed.
2.2.2.4 X-ray Diffraction (XRD) Analysis
The crystalline mineral phases of SC were investigated from 5 to 110 degrees 26 on a Philips X'Pert Pro
Diffractometer using copper Ka radiation. The SC sample was further powdered (< 0.05 mm) by a sealed stainless-
steel jar mill with zirconia grinding beads. The powder diffraction file (PDF) patterns database from the International
Centre for Diffraction Data (ICDD) was employed for the search, match, and identification steps. A subset of
reference patterns was built for all SC samples. The semi-quantitative phase analysis was performed by the X'Pert
HighScore Plus software, based on the CHUNG Normalized RIR Method [79]. The relative intensity of each phase is
given by the scale factor, which is determined by least squares fit through all matching reference pattern lines in X'Pert
HighScore. The concentration X of phase a is calculated using:
xw =
K RIR Irel
K1K«'(hkl)K
(2-1)
where RIRK is Reference Intensity Ratio, based on the relative net peak height ratio of the strongest line (Irel = 100%)
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of the phase and of the strongest line of corundum, measured with copper Ka radiation in a mixture of equal weight
percentages and I(hki)K is Intensity of reflection of hkl in phase a. hkl are the reflection indices.
The normalization used in this method assumes that the sum of all identified phases is 100%. This means that there are
no unidentified crystalline phases or amorphous phases assumed to be present in the sample. Only under these
conditions can meaningful, semi-quantitative results be obtained.
2.3 Reactivity of Salt cake
The chemical reaction of aluminum species with water typically generates heat and gas. Therefore, the reactivity of SC
as a result of SC reaction with liquid was evaluated using three indicators: 1) temperature increase as well as time to
reach the maximum temperature; 2) heat generation potential; and 3) gas generation potential. It is noted that the SC
samples in this work were from 10 different facilities, which might contribute some variability of the reactivity of SC.
However, this report will focus on the general patterns of the reactivity of SC.
2.3.1 Apparatus for Testing Salt Cake Reactivity
The apparatus presented in Figure 2-2 was utilized to evaluate the increase in temperature caused by the reaction of SC
with liquid. The target SC sample was placed in a 60 ml volatile organic analyte (VOA) vial and purged with argon for
five minutes. The vial was then sealed and connected to a 1 L Tedlar bag for pressure release. Pre-heated DIW was
then added to the sealed vial to achieve certain liquid to solid ratio. The change in temperature as a result of the SC
reaction with liquid was monitored using a thermocouple wire placed in the sample. Sand samples were utilized as
control under the same experimental condition (e.g. liquid to solid ratio). When the average temperature difference
between the sample and control reached less than 0.5°C, the experiment was stopped. The overall experimental
duration typically ranged from 72 to 120 h. It is noted that the sensitivity of the thermocouple is 0.5°C and as a result
this value was utilized to determine the end of the experiment. Furthermore, once the difference between the control
and the SC sample reached the 0.5°C, the experiment was kept for 10 h to ensure the stability of the temperature
difference at this level.
Temperature Data Logger
Thermocouple wire
1:1 Ratio of SC (10 g)
and DI water (10 ml)
1 L Tedlar bag for
pressure relief
60 ml VOA Vial
Figure 2-2: Temperature increase apparatus
The heat generation potential was evaluated using a custom-made reaction calorimeter presented in Figure 2-3. The
calorimeter is composed of double glass vessels, an inner-vessel (40 ml VOA vial) and an outer-vessel (250 ml vial
with a three-port Teflon cap). The inner-vessel is immersed in the outer-vessel containing 90 ml ethylene glycol as a
thermal buffer since it has a low specific heat capacity. The calorimeter is equipped with three thermocouple wires
immersed in the ethylene glycol solution and connected to a data logger. The inner-vessel is connected to a 1 L Tedlar
bag to relieve any pressure resulting from the reaction of SC with liquid.
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The gas generation potential of SC was evaluated under anaerobic conditions (to simulate MSW landfill environment)
using the test apparatus presented in Figure 2-4. The target SC sample was placed into a 500 ml lined media bottle
sealed with a lyophilization stopper and a cap. The media bottle was then purged with argon for 10 minutes. An
aliquot of oxygen-free, argon-purged, and pre-heated water was then added to the sample to achieve a certain liquid to
solid ratio. AIL Tedlar bag was connected to the bottle to collect the gas generated from the reaction. The media
bottles were then placed in a 50°C incubator (Fischer Scientific Isotemp Dual CCh Incubator) for 5 d, after which the
Tedlar bag was disconnected and gas quantity and composition were measured. It is noted that the sample bottles were
allowed to reach room temperature before performing the gas volume and composition measurements.
Syringe pusher
Temperature
Controlled Room
Saltcakewith
water, e.g.
5g/10mlDIW
Figure 2-3: Heat measurement apparatus
Three-port teflon cap
Tedlar bag (gas capture)
for off-line analysis
One-way gas valve
Headspace
Dl-Water
SC Sample
Figure 2-4: Reactivity test apparatus for gas generation measurement
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2.3.2 Factors Impacting Salt Cake Reactivity
Several factors may impact the SC reactivity and include environmental temperature, SC particle size, liquid addition
rate, liquid to solid ratio, chemical composition of the liquid, and chemical composition of SC. The impact of these
parameters on SC reactivity was evaluated and the results were utilized to select the experimental conditions for the
temperature increase and gas generation experiments.
2.3.2.1 Effect of Environmental Temperature
Randomly selected SC samples (2439-E, 2510-F, 2482-L, 2488-L, and 2601-M) were employed to investigate the
impact of environmental temperature (20, 37, and 50°C) on the temperature change upon exposure to water. Samples
with particle size < 2 mm (size was achieved as described in section 2.1.2) were mixed with pre-heated DIW (pH 6.2)
to achieve a liquid to solid ratio of 1 to 1 (10 ml DIW to 10 g sample) and the temperature increase was measured using
the apparatus described in section 2.3.1.
To evaluate the impact of environmental temperature (37 and 50°C) on the heat generation potential of SC, samples
(2502-F, 2046-H, 2490-L, and 2613-M) with size < 0.05 mm were utilized. A 10 ml pre-heated DIW (pH 6.2) was
added to the samples to achieve a liquid to solid ratio of 2 tol (10 ml DIW to 5 g sample). The heat generation
potential was measured using the apparatus described in section 2.3.1.
To evaluate the impact of environmental temperature (4, 20, 37, and 50°C) on the gas generation of SC, samples
(2439-E, 2046-H and 2512-J) with size < 2 mm were utilized. A 20 ml of pre-heated DIW to the target temperature
(pH 6.2) was added to the samples to achieve a liquid to solid ratio of 20 tol (20 ml DIW to 1 g sample, duplicated).
The hydrogen and methane productivity were measured after five days reaction in 60 ml vials, which were similar to
the apparatus described in section 2.3.1.
2.3.2.2 Effect of Salt Cake Particle Size
Randomly selected SC samples (2502-F, 2512-J, and 2046-H) were tested at 37°C. Three different particle sizes were
compared, < 0.05, < 2, and < 9 mm. Ten ml pre-heated DIW (37°C) with a pH 6.2 was added to 10 g SC sample to
achieve 1:1 liquid to solid ratio. The increase in temperature as a function of particle size was measured using the
apparatus described in section 2.3.1.
To evaluate the impact of particle size (< 0.05 and < 2 mm) on the heat generation potential of SC, samples (2502-F,
2512-J, 2046-H, and 2490-L) were utilized. Ten ml pre-heated DIW (pH 6.2) was added to the samples to achieve a
liquid to solid ratio of 2 to 1 (10 ml liquid to 5 g sample). The heat generation potential was measured using the
apparatus described in section 2.3.1.
To evaluate the impact of particle size (< 0.05, < 2, and < 9 mm) on the gas generation potential of SC, samples (2512-
J, 2046-H, and 2613-M) were utilized. Twenty ml pre-heated DIW (pH 6.2) was added to the samples to achieve a
liquid to solid ratio of 20 tol (20 ml liquid to 1 g sample, duplicated) at 37°C environmental temperature. The
hydrogen and methane productivity was measured after five days reaction in 60 ml vials, which were similar to the
apparatus described in section 2.3.1.
2.3.2.3 Effect of Liquid Addition Rate
Ten g of SC sample 2069M with particle size < 2 mm was exposed to two treatments to investigate the impact of
liquid addition rate on the reactivity of SC. The first treatment received 10 ml DIW at once and acted as a control. The
second treatment received 10 ml DIW intermittently over a period of 72 h. Both treatments were conducted at 3 7°C.
The increase in temperature as a function of hydration/dehydration cycle was measured using the apparatus described
in section 2.3.1.
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2.3.2.4 Effect of Liquid Chemical Composition
The effect of chemical composition of liquid on SC reactivity was evaluated by measuring the temperature increase,
heat generation and gas generation from samples exposed to liquids with different chemistry.
The apparatus described in section 2.3. 1 was utilized for conducting this test. Randomly selected SC samples (Table 2-
3) with particle size < 2 mm (for temperature increase and gas generation) and < 0.05 mm (for heat generation and gas
generation) were employed. The ratio of liquid to solid and the various liquids utilized are presented in Table 2-3. All
liquids used were pre-heated to 37 or 50°C, the temperatures at which the experiments were carried out.
2.3.2.5 Effect of Liquid to Solid Ratio and Mass of Salt Cake
Randomly selected SC samples were employed to investigate the effect of liquid to solid ratio and mass of SC on SC
reactivity. Different treatments were used where the liquid to solid ratio or the mass of SC were varied as presented in
Table 2-4. Pre-heated DIW (pH 6.2) was used as the liquid. The effect of liquid to solid ratio was evaluated at 50°C
and the effect of mass of SC was evaluated at 37°C. The reactivity of SC in each case was evaluated by measuring the
temperature increase, heat generated or gas generated for the samples using the apparatus described in section 2.3.1.
Table 2-3: Treatments for testing the effect of liquid composition on salt cake reactivity
Reactivity
Indicator
Temperature
Change
Heat Generation
Gas Generation
Liquid to Solid Ratio
1:1 (10 ml liquid to 10 gSC,
< 2 mm, 37°C)
2: 1(10 ml liquid to 5 g SC,
< 0.05 mm, 50°C)
20 : 1(20 ml liquid to 1 g SC,
< 0.05 mm, 50°C)
Solution chemical
composition
DIW
0.1MHC1
O.lMNaOH
1% salt of humic acid*
VFA**
Landfill Leachate***
DIW
0.1MHC1
O.lMNaOH
VFA
Landfill Leachate
DIW
0.1MHC1
O.lMNaOH
Landfill Leachate
1% salt of humic acid
VFA
pH
6.2
1.0
13
8.3
5.3
8.1
6.2
1.0
13
5.3
8.1
6.2
1.0
13
8.1
8.3
5.3
Sample ID
2502-F, 2555-H, 2046-H,
and 261 3 -M
2502-F, 2555-H, and
2613-M
2512-J, 2489-L, 2046-H,
2555-H, and 2613-M
*Salt of humic acid, Sigma-Aldrich (CAS # 68131-04-4).
** VFA composition: 1,795 mg L"1 acetic acid; 1,296 mg L"1 propionic acid; and 1,284 mg L"1 n-butyric acid;
***Landfill leachate: DOC: 20,000 mg L4
2.3.2.6 Effect of Aluminum Species in Salt Cake Simulators
To understand the mechanism of temperature increase in SC and the effect of SC composition on the magnitude of
temperature change, commercial chemicals NaCl, KC1, Al2Os, metallic aluminum, A1N, and Al4Cs were used in
varying mixtures to simulate the SC chemical composition. The reason for synthesizing SC for the purpose of this test
over using the actual SC samples is to enable the understanding of the role of each individual aluminum species in SC
reactivity. The particle sizes of Al2Os, AUCs, metallic aluminum, and A1N in the mixture were 0.05, 10, 20, and 44 jam
respectively. The particle sizes of added salt (NaCl and KC1) were less than 1 mm. The liquid to solid ratio was 1 to 1
(10 ml DIW to 10 g solid sample). The experiments were conducted at 37°C using the apparatus described in section
2.3.1 to measure the temperature change for each scenario. The basic mixture (Mixture I) was composed of 5% KC1,
10% NaCl, and 85% A12O3. The details of the chemical composition in these SC simulators are presented in Table 2-5
It is noted that a control sample (sand) was employed with each set of experiments.
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2.3.3 Salt Cake Reactivity Evaluation
The results of the experiments conducted in section 2.3.2 to evaluate the impact of various parameters on SC reactivity
were the basis for selecting the experimental conditions for evaluating the reactivity of all the 39 SC samples
investigated in the current study. The reactivity was measured by the temperature increase, heat generation and gas
generation after SC reaction with water.
2.3.3.1 Temperature Increase
The apparatus presented in Figure 2-2 was utilized to measure the temperature increase as a result of SC reaction with
DIW. A 10 g SC sample of < 2 mm size was placed into a 60 ml VOA vial. After purging the vial with argon for 5
min, the vial was sealed and 10 ml pre-heated DIW was then added to the vial to achieve 1:1 liquid to solid ratio. The
experiments were conducted at two different temperature conditions (37 and 50°C). The temperature conditions were
selected based on reported ideal temperatures for mesophilic (35 to 40°C) and thermophilic (50 to 60°C) bacteria that
are normally present in MSW landfills [58, 59] and temperatures consistent with reported landfill temperatures [80-
82]. The temperature conditions were achieved by placing the experimental apparatus in an incubator heated to the
desired temperature (Fischer Scientific Isotemp Dual CC>2 Incubator). Usually, six to 12 sample vials and one control
sample vial were grouped as one set arranged in an insulated box inside the incubator (Figure 2-5). Insulation
materials were used to isolate the heat transfer among the vials and to decrease the influence among the samples. The
increase in temperature as a function of time was measured as previously described in section 2.3.1.
Table 2-4: Treatments for testing the effect of liquid to solid ratio and mass of salt cake on the reactivity
Reactivity Liquid to Solid Liquid Volume Solid Mass Particle Size „ , TTV
T .•• ^ T.X- /•% / % / % Sample ID
Indicator Ratio (ml) (g) (mm) r
Temperature
Increase
Heat Generation
Gas Generation
Variable
Variable
Fixed (3: 10)
Fixed (1:2)
Fixed (1:1)
Variable
Fixed (2:1)
Variable
3
5
10
15
3
3
3
1.5
3
4.5
6
2.5
5
7.5
5
10
15
20
10
10
6
10
15
20
2.5
5
10
10
10
10
5
10
15
5
10
15
20
5
10
15
5
10
15
20
1
2
o
j
5
7.5
10
5
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
0.05
0.05
005
0.05
0.05
0.05
2
2478-B
2478-B
2478-B
260 1-M
2482-L, 2506-F, and
243 9-E
2613-M
2046-H, 2490-L and
2502-F
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243 3-C, 2512-J, and
2613-M
2.3.3.2 Heat Generation Potential
The heat generation potential was evaluated using the calorimeter described in section 2.3.1. A 5 g SC sample (size <
0.05 mm) was added to the 40 ml inner-vessel which was then capped and placed in the 250 ml outer vessel containing
90 ml pre-heated ethylene glycol. The experiments were conducted at two different temperature conditions, 37 and
50°C, which were achieved by placing the calorimeter in an incubator heated to the desired temperature (Fischer
Scientific Isotemp Dual CC>2 Incubator). Ten ml pre-heated liquid was injected to the inner-vessel using a syringe to
achieve a liquid to solid ratio of 2:1. The temperature of the ethylene glycol solution was monitored over time (one
reading every two min recorded using a data logger) until no temperature change was observed from the reaction (at
least 72 h). With each batch (4 double vessels in an insulated box) sand samples were employed as controls under the
same experimental conditions.
Table 2-5: Composition of the SC stimulators for testing the impact aluminum species on the reactivity
Experiment
I
II
III
IV
V
Composition
1
2
3
4
1
2
3
4
5
1
2
3
4
1
2
3
4
1
2
3
Al (%)
0
5
10
20
0
0
0
10
10
5
20
5
20
0
5
10
20
20
20
20
A1N (%)
0
0
0
0
2
5
10
2
10
1
1
2
2
0
0
0
0
0
5
10
AUCs (%)
0
0
0
0
0
0
0
0
0
0
0
0
0
5
5
5
5
0
0
0
Other (%)
100- Mixture I*
95- Mixture I
90- Mixture I
80- Mixture I
98- Mixture I
95- Mixture I
90- Mixture I
88- Mixture I
80- Mixture I
94- Mixture I
79- Mixture I
93 -Mixture I
78- Mixture I
95- Mixture I
90- Mixture I
85- Mixture I
75- Mixture I
54%NaCland26%KCl
50%NaCland25%KCl
47%NaCland23%KCl
*Mixture I is composed of 5% KC1, 10% NaCl, and 85% A12O3.
Figure 2-5: Sample arrangement in an insulation box for temperature change experiment
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For every recorded reading, the difference in temperature (AT) between the SC sample and control was calculated. It is
noted that each temperature reading is the average of the three thermocouple readings. The sum of temperature change
as compared to the control (EAT) was converted to heat using a calibration curve. The calibration curve was
constructed between the EAT and the heat generated by a fixed resistance (R) when applying varying electric current
(I) with time. The power (P) is calculated using the following relationship:
P = VI
Where P is the power, I is the current, and V is the voltage (V = I
related to the power and time as follows:
Q = PT
(2-1)
R). The generated heat (Q) from a resistance is
(2-2)
The calibration curve is constructed by plotting the EAT and Q. Examples of detailed calculations and calibration
curve are presented in Table 2-6 and Figure 2-6, respectively. The following relationship was obtained from the
calibration curve under laboratory setting:
Q = 0.006ZAT
(2-3)
Table 2-6: Calculations of heat generation from a fixed resistance and EAT
Resistance
(0)
45.8
Current
(mA)
135
174
191
246
348
427
174
246
Time
Energized
(min)
60
60
60
60
60
60
120
120
Power
Applied
(W)
0.83
1.4
1.7
2.8
5.6
8.3
1.4
2.8
Voltage
(V)
6.2
8.0
8.7
11
16
20
8.0
11
Energy
(kJ)
3
5
6
10
20
30
10
20
EAT
(°C per
2min)
480
800
1,100
1,700
3,100
5,000
1,700
3,000
SB
01
SC
35 -|
30 -
25 -
20 -
15 -
10 -
5 -
0
Heat = 0.006xATsl
R2 = 0.993
0 1000 2000 3000 4000 5000
Sum of Temperature change ATSU111 (C/2min)
6000
Figure 2-6: Example of calibration curve for heat calculation
2.3.3.3 Gas Generation Potential
The apparatus presented in Figure 2-4 was utilized for evaluating the gas generation potential as a result of SC reaction
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with water. A 5 g SC sample with size < 2 mm was placed into a 500 ml lined media bottle sealed with a lyophilization
stopper and cap. The media bottle was then purged with argon for 10 mins. One hundred ml of oxygen-free, argon-
purged, pre-heated (50°C) water was then added to the sample to achieve a 20:1 liquid to solid ratio. The volume and
composition of the gas generated were measured after 5d reaction as presented below.
2.3.3.3.7 Gas Volume
The gas volume was measured after 5d reaction using 60 ml gas-tight syringe. The gas volume generated was
composed of two portions, one is the gas present in the bottle's headspace and the other is the gas collected in the
Tedlar bag. Disconnected the Tedlar bag, and placed both bottle and Tedlar bag under a chemical fume hood at room
temperature (25 °C) for 4 hours. The headspace gas fraction was measured by attaching a 20 gauge needle to the
syringe and then inserting the needle through the bottle septum allowing the syringe plunger to move freely. The gas
volume fraction collected in the Tedlar bag was extracted using the syringe. The total gas volume was calculated by
the sum of the two fractions.
2.3.3.3.2 Gas Composition
Hydrogen (Hi) and Methane (CHt)
The concentrations of hydrogen (H2) and methane (CH4) gas content were determined via analysis of a 100 uL
headspace sample using an Agilent 6980 Gas Chromatograph equipped with a thermal conductivity detector
(GC/TCD). The gas components were separated by the two analytical columns (PorapakN packed column, and
Molesieve 5A packed column), controlled by an automated valve switch. A five-point calibration curve was prepared
to quantify the gas composition. The calibration range was 1 to 100% for H2 and 1.67 to 100% for CH4. The MRL was
0. 14% for H2 and 0.2% for CH4 (Appendix A, Table A-3). A standard gas mixture (15% CO2, 15% CH4, 4% H2, and
66% N2) purchased from Matheson TRI-GAS Inc. was used as a standard check before and after gas analysis.
Nitrous Oxide (NiO)
Nitrous oxide (N2O) concentration was determined via analysis of a 100 ul headspace sample using an Agilent 5975
Gas Chromatograph equipped with a split/splitless injection port operated in the split mode and Electron Capture
Detector (GC/ECD). The gas components were separated using a J&W GS-Gaspro column, 60 meters in length and
0.32 mm in diameter, then detected by a |a-ECD detector. A six-point calibration curve was prepared to quantify the
N2O composition. The retention time of N2O for the specified conditions was 4.94 minutes, and the linear
concentration ranged from 20 to 2000 parts per billion in volume (ppbv). The MRL for N2O was 20 ppbv (Appendix
A, Table A-3).
Hydrogen Sulfide
Hydrogen sulfide (H2S) gas content was measured using a Jerome meter (JEROME® 63 1-X, Arizona Instrument LLC)
according to the method presented in the instrument manual [83] . The detection range of the Jerome meter for H2S
ranges between 3 ppb to 50 ppm [83] with a large flow rate (150 ml min"1).
Ammonia (gaseous NHs) and Ammonium (aqueous NH4+)
After the SC reacts with water, the generated ammonia can be present in the gaseous form as NH3 or in aqueous form
as hydrated ions (NH4+) and dissolved gas. The equilibrium between these two forms is mainly dependent on solution
pH. To measure NH3 content in the gaseous form, a 20 ml headspace gas sample was injected into 20 ml of 0. 1 M
H2SO4 acid solution to transfer all the gaseous form of ammonia into NH4+. The concentration of NH4+ in the solution
was measured using an ammonia electrode (Standard Methods for the Examination of Water and Wastewater, 4500-
NH3 D, E) [71]. To measure the NH4+ concentration in the liquid form, approximately 2 to 5 ml of liquid in the media
bottle (Figure 2-4) was collected (without filtration) and injected using a syringe into a 50 ml volume of 0.05M H2SO4
acid solution. The concentration of NH4+ was determined as previously described [71].
2.3.3.3.3 Gas Productivity
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The H2, CH4 and N2O gas productivity (mole gas g"1 SC sample) was calculated as follows:
• Multiply the total gas volume (measured using syringe) by the gas concentration (measured using GC) to get
the volume (L) of each individual gas.
• To convert each individual gas volume to moles of gas, divide the volume by 24.45 L. One mole of an ideal
gas at STP occupies 22.4 liters but under the current experimental condition (25°C) the corrected volume for
one mole of gas is 24.45 L.
• The productivity (mole g"1) of each gas is then calculated by normalizing the moles of gas produced to the
SC sample weight used.
The NH3 gas productivity (mole gas g"1 SC sample) was calculated as follows:
• The NH3 concentration measured in the acid solution in mg L"1 (section 2.3.2.2.4) was converted to molar
concentration (M).
• The moles of NH3 (moles NH3) is calculated by multiplying the acid solution volume (20 ml) by the M
concentration of NH3.
• The total moles of NH3 in the gas was calculated by multiplying the moles NH3 by the total gas volume
generated and dividing this quantity by 20 (the volume of headspace gas sample analyzed for ammonia).
• The ammonia gas productivity (mole g"1) was calculated by normalizing the total moles of gas produced to
the SC sample weight used.
2.4 Statistical Analysis
Statistical analysis and graphical representation of the data was performed using Microsoft Excel 2007, JMP 9.0, and
SigmaPlot 11.0 [84, 85]. The statistical analysis technique was chosen based on the properties of parameters. The
mean, standard error, minimum and maximum values as well as UCL9s (95% upper confidence limit) were used to
summarize the content of elements, mineral phases, and the temperature change, as well as the gas composition and
gas production. UC L9s was used to describe the potential risk or hazards in USEPA [86]. It is noted that the UCL9s is
a probability statement: it means "I am 95% confident that the true distribution of the sampling data has a population
mean less than or equal to my calculated UCL".
a)
95%
confidence
interval
.r-axis proportional
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b)
BQK ends at
Quartile
Box. starts from /—
-istCJuartile /
[ Median ]
Figure 2-7: Examples of mean diamonds and box plot
Box plots with mean diamonds were employed to graphically depict groups of numerical data through their summaries
(minimum, lower quartile, median, mean, upper quartile, and maximum). A mean diamond illustrates a sample mean
and confidence interval. Figure 2-7 is an example of Mean Diamonds and Box plot. The top and bottom of each
diamond (Fig. 2-7a) represent the 95% confidence interval for each group. The confidence interval computation
assumes that the variances are equal across observations. Therefore, the height of the diamond is proportional to the
reciprocal of the square root of the number of observations in the group. The mean line across the middle of each
diamond represents the group mean. Overlap marks appear as lines above and below the group mean. For groups with
equal sample sizes, overlapping marks indicate that the two group means are not significantly different at the given
confidence level. Basic box plots show a simple rectangular box-plot, from the first to the third quartile, with the
median marked in the center (Fig. 2-7b).
One-way ANOVA test was employed to judge the differences of these parameters among facility, including the
interaction of the random facility and the tested conditions (e.g. environmental temperature). If there were differences,
LS Means Difference Tukey HSD were further tested the differences among factors.
Correlations between the temperature change and mineral phases, or relation between trace metal content and
aluminum content, were analyzed using the Pearson product-moment correlation and Spearman's rank correlation to
calculate the p-level. The Pearson product-moment correlation coefficient is a measure of the correlation (linear
dependence) between two variables X and Y, giving a value between +1 and -1, inclusive. Spearman's rank
correlation coefficient is a non-parametric measure of statistical dependence between two variables. It assesses how
well the relationship between two variables can be described using a monotonic function. If there are no repeated data
values, a perfect Spearman correlation of+1 or -1 occurs when each of the variables is a perfect monotone function of
the other. If p < 0.05, it was assumed that the relation was significant; and if p < 0.01, the correlation was considered
very significant. If p > 0.05, it was assumed that there was no significant correlation. The linear correlations were
used for the calibrations and relations between the properties of parameters (e.g. ATmax vs heat). The correlations of the
properties of parameters, ANOVA are also performed to test the significance of facility. The bivariate normal
confidence ellipse region were also presented (p = 0.95). The density ellipsoid is computed from the bivariate normal
distribution fit to the X and Y variables. The bivariate normal density is a function of the means and standard
deviations of the X and Y variables and the correlation between them. These ellipses are both density contours and
confidence curves. As confidence curves, they show where a given percentage of the data is expected to lie, assuming
the bivariate normal distribution. The density ellipsoid is a good graphical indicator of the correlation between two
variables. The ellipsoid collapses diagonally as the correlation between the two variables approaches either +1 or -1.
The ellipsoid is more circular (less diagonally oriented) if the two variables are less correlated.
2.5 Quality Metrics
The accuracy checks, precision, calibration of instrumentation, and the determination of detection limits are used to
ensure the quality control and the confidence level of the obtained results. Precise, documented and valid data are
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needed for the ultimate decisions to be made. To ensure the quality of the data, all instruments are regularly calibrated.
QA/QC checks were done to ensure the precision and accuracy of the data. Table 2-7 summarizes the QA/QC checks
for each monitoring parameter in this report.
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Table 2-7: Summaries of QA/QC Checks
Parameter
Moisture Content
Water holding
capacity
PH
Conductivity
Total metal
Ammonia (NH4)
Metals (leachate)
Temperature
Heat measurement
Crystallinity
(XRD)
Gas volume
Gas Composition
QC Check
Initial Calibration
Initial Calibration
Initial Calibration
Initial Calibration
Calibration
Precision
Accuracy
Initial calibration
Continuing
calibration
Precision
Blank
Accuracy
Calibration
Precision
Blank
Accuracy
Initial Calibration
Initial Calibration
Calibration
Initial Calibration
Initial Calibration
Precision
Method
1 point
calibration
1 point
calibration
3 point
calibration
1 point
calibration
5 point
calibration
Sample
duplicate
Standard check
4 point
calibration
Run mid-point
standard
Sample
duplicate
Laboratory
blank
Matrix Spike
4 point
calibration
Sample
Duplicate
Laboratory
blank
Check Standard
1 point
calibration
1 point
calibration
Reference
standard
1 point
calibration
6 point
calibration
Sample
Duplicate
Frequency
At the beginning
At the beginning
At the beginning
At the beginning
Before each run
For every 12 samples
With every run
At the beginning
Every 12 samples
Every 6 samples
Every 6 samples
Every 6 samples
Before each run
Every 12 samples
Every 12 samples
Every 12 samples
At the beginning, and
once a year
Every 6 months
Prior to sample
analysis
At the beginning
Monthly
Every 12 samples
Acceptance Criteria
Within ± 5% of the full range
of the probe
Within ± 5% of the full range
of the probe
Within ± 0.1 pH unit of the
correct value
Within ± 2% of the full range
of the probe
R2>0.99
< 25%RPD
75-125% recovery
R2> 0.995
±20% of the actual
concentration
< 20% RPD
< Reported detection limit
100 ±20% recovery
R2> 0.995
< 15% RPD for macro-
elements (Al, Fe, Ca, K, Na,
S and Mg) and < 25% for
trace metals (Ag, Ba, Cu, Mn,
Zn, Cd, As, Se, Cr and Pb).
< Reported detection limit
100 ± 15% recovery for major
metals and 100 ± 25% for
trace metals
Within ± 2% of the full range
of the probe
Within ± 15%
Within ± 5% of the full range
of the probe
R2> 0.990
< 20% RPD
Corrective Action
1 . Re-calibrate
1 . Re-calibrate
1 . Re-calibrate
1 . Re-calibrate
1 . Re-calibrate
1 . Re-run
2. Prepare new standards
2. Check calculations
1 . Re-calibrate
1 . Re-calibrate
1 . Re-calibrate
1 . Redo triplicate
2. Investigate the problem
1 . Investigate problem
2. Remove contamination
3. Check other blanks
1 . Re-run spike
2. Check calculations
3 . Re-run samples as
required
1 . Re-calibrate
1 . Re-analyze
2. Investigate the problem
1 . Investigate problem
2. Remove contamination
3 . Check other blanks
1 . Re-calibrate
2- Re-run samples as
required
1 . Use new thermocouple
(within 1 year)
1 . Re-do sample
2. Investigate the problem-
Flag data
1 . Re-calibrate
1 . Re-calibrate
1 . Re-calibrate
1 . Re-do sample
2. Investigate the problem-
Accuracy
Standard Check Twice a Week
100 ±20% recovery
Flag data
1. Re-calibrate
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3. PHYSICAL AND CHEMICAL PROPERTIES
3.1 Moisture Content (MC)
The average MC of the investigated SC was 0.8%, with a range of 0.01 to 2% as presented in Table 3-1. The
variability of MC by facility and the overall distribution are presented in Figure 3 -1. The detailed MC results for each
sample are listed in Appendix B (Table B-l). No evidence was shown that there were statistically significant
differences from the various facilities, which may be due to the limited sample sizes.
Table 3-1: Salt cake moisture content
Facility Sample
number
B 4
C
D
E
F
H
J
L
2
4
2
5
5
4
5
M 4
N 4
Mean
0.7±0.4
0.9±0.6
1±0.9
0.8±0.02
0.8±0.4
1±0.2
0.6±0.4
0.9±0.7
0.9±0.9
0.4±0.3
UCL95*
1
6
2
0.9
1
1
1
2
2
0.9
Range
0.4-1
0.5-1
0.1-2
0.7-0.8
0.04-1
0.8-1
0.3-1
0.3-2
0.01-2
0.1-0.8
All Facilities
39
0.8±0.5
0.01-2
*Upper 95% confidence level on the mean
Facility
0.5
1 1.5
Moisture Content
-0.20
-0.15
-0.101
-0.05
2.5
Figure 3-1: Salt cake moisture content and its distribution
3.2 Water Holding Capacity (WHC)
Water holding capacity (WHC) is an important physical characteristic of materials. The overall average WHC of SC
was 25%, ranged from 1.4 to 70% (Table 3-2), and followed a normal distribution (Figure 3-2). Statistically, there
were significant differences in WHC between facilities. SC samples from Facility M had the highest WHC, which was
more than 20 times the average WHC of Facility B, the facility which had the SC with the lowest WHC. The detailed
WHC results for each sample are listed in Appendix B (Table B-l).
The measured WHC values should be viewed with some caution - as described, some degree of reaction of the SC
with water may occur, which could result in a mass loss and ultimately skew the WHC measurements. Mass loss
would result in an under reported WHC value.
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I c I D I E I F I H I J I L I M I N
Facility
15 30 45 60
Water Hold Capacity
Figure 3-2: Salt cake water holding capacity and its distribution
Table 3-2: Salt cake water holding capacity (%)
Facility Sample
number
B 4
C 2
D
E
F
H
J
L
M
4
2
5
5
4
5
4
N 4
All Facilities 39
Mean
2.3±0.5
6.5±4.9
6.4±5.5
19±8
19±20
27±13
24±4.6
47±13
55±12
30±25
25±20
UCL95
3.2
50
15
92
44
43
31
63
74
70
32
Range
1.9-3.0
3.0-10
1.4-11
13-24
3.1-53
11-44
20-30
38-70
43-70
2.9-63
1.4-70
3.3 pH and Electrical Conductivity (EC)
Both the pH and EC of SC were measured after SC reacted with water for five d at 50°C in the reaction device (Figure
2-4, Section 2.3.1). The liquid to solid ratio was 20 to 1. The pH of SC was alkaline, and ranged from 9.6 to 11.3 with
an average of 10.5 (Table 3-3). Sample 2506 fromFacility F had the highest pH (11.3), whereas sample 2515 from
Facility J exhibited the lowest pH (9.6). The detailed pH results for all SC samples are listed in Appendix B (Table B-
1). No evidence was shown that there were statistically significant differences among samples, and the distribution of
pH is presented in Figure 3-3.
Table 3-3: Salt cake pH
Facility Sample
number
B 4
C
D
E
F
H
J
L
2
4
2
5
5
4
5
M 4
N 4
Mean
10.8±0.3
10.OiO.01
10.5±0.3
10.5±0.2
10.8±0.3
10.7±0.1
10.2±0.6
10.8±0.1
10.2±0.2
10.4±0.2
UCL95
11.3
10.1
11.0
11.9
11.2
10.8
11.1
10.9
10.6
10.8
Range
10.5-11.3
10-10
10.3-10.9
10.4-10.6
10.5-11.2
10.5-10.9
9.6-11.0
10.7-11.0
10.1-10.5
10.2-10.7
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Facility Sample Mean UCL9S Range
number
All Facilities 39
10.5±0.4
10.7
9.6-11.3
12
11.5 -
11 -
£ 10.5 -
10 -
9.5 -
BCDEFHJLMN
Facility
12
Figure 3-3: Salt cake pH and its distribution
The EC of salt cake was relatively high with large variation (Figure 3-4), and largely depended on the sources of
sample. The average EC of all samples was 30 mS cm"1 (Table 3-4). Sample 2605 from Facility M had the lowest
measured EC (18 mS cm"1) and Sample 2532 from Facility D had the highest measured EC (47 mS cm"1). This is
expected because of the addition of salts to the SAP process. The detailed EC results for each sample are listed in
Appendix B (Table B-l).
BCDEFHJ LMN
Facility
15 20 25 30 35 40 45 50
Figure 3-4: Salt cake EC and its distribution
Table 3-4:
Facility
B
C
D
E
F
H
Salt cake electrical conductivity (EC)
Sample
number
4
2
4
2
5
5
Mean
27±4.2
28±5.3
38±8.0
31±2.7
34±8.5
28±3.7
UCL95
33
76
51
55
46
33
(mS cm'1)
Range
23-33
25-32
28-47
29-33
26-47
24-33
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Facility
J
L
M
N
All Facilities
Sample
number
4
5
4
4
39
Mean
30±2.8
28±5.9
25±6.0
27±4.2
30±6.2
UCL95
34
35
35
33
32
Range
26-33
21-33
18-31
23-31
18-47
3.4 Total Extractable Metals
The major total extractable metal content of each SC sample investigated is listed in Appendix B (Table B-2) and the
trace metals content is presented in Appendix B (Table B-3). For the purpose of this section, the percent composition
is calculated based on wet weight of the samples.
3.4.1 Aluminum (Al) Content
The average content of total Al in the SC was approximately 14%, and ranged from 6.7 to 42% as presented in Table
3-5, which was lower than the previously reported (26 to 47%) [16, 45-47, 87]. The overall distribution of % total Al
for the SC samples is presented in Appendix B (Figure B-l). Sample 2609 from Facility M had the highest Al content
at 42%, while Sample 2492 from Facility N had the lowest at 6.7% (Table 3-5). Overall, the samples from Facility M
had a significantly higher Al content compared to the rest of the sites. Excluding the samples from Facility M, the
average total Al content in SC was around 12% lower than the range reported in the literature [16, 20, 46, 87, 88].
Table 3-5: Extractable Al content in salt cake (%)
_, .... Sample
Faciht? number
B 4
C
D
E
F
H
J
L
2
4
2
5
5
4
5
M 4
N 4
Mean
11±2.2
12±0.93
10±1.1
12±0.21
13±2.5
17±3.1
14±3.0
13±1.9
29±9.7
7.8±1.3
UCL95
14
20
12
14
16
20
19
16
44
9.9
Range
8.5-14
12-13
9.2-12
11-12
9.2-16
13-21
10-17
12-16
21-42
6.7-9.3
All Facilities
39
14±6.6
16
6.7-42
3.4.2 Major Metals Content
In addition to Al, several other metals were detected in SC samples in relatively high concentrations and were denoted
"major metals" in the current study. These metals are calcium (Ca), magnesium (Mg), iron (Fe), potassium (K), and
sodium (Na) and their concentrations are presented in Table 3-6.
Table 3-6: Major metals content in salt cake (%)
Metal
Ca
Mg
Fe
K
Na
Mean
1.0±0.53
2.0±1.2
0.58±0.43
5.8±2.4
10±2.1
Median
1.0
1.8
0.44
6.6
10
UCL95
1.2
2.4
0.72
11
11
Range
0.32-2.4
0.05-4.1
0.15-2.4
2.7-13
5.6-17
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The average calcium content in the sampled SC was approximately 1.0%, and ranged from 0.32 to 2.40% (Table 3-6).
The overall distribution of % Ca for the SC samples is presented in Appendix B (Figure B-2). Facilities D and N
exhibited low Ca content, while Facilities E and C showed higher values (Appendix B, Tables B-4). Previous research
reported Ca content in SC within a range from 0.63 to 1.23% [16, 20, 45-47, 87].
The magnesium content in SC ranged from 0.05 to 4.1%, with an average of 2.0% (Table 3-6). The overall distribution
of % Mg for the SC samples is presented in Appendix B (Figure B-3). The Mg content of samples from Facilities N
and H was significantly lower than those from most other facilities (Appendix B, Table B-5). In previously-published
research, the total Mg content in SC ranged from 0.7 to 7.6% [16, 20, 45-47, 87].
The average measured iron content in SC was 0.58% and ranged from 0.15 to 2.4% (Table 3-6). The overall
distribution of the percent Fe for the SC samples is presented in Appendix B (Figure B-4) and the Fe content from all
samples analyzed is presented in Appendix B (Table B-6). With the exception of sites J and N, the Fe content in the
SC samples had low levels of variability. In previously-published research, the total Fe content in SC ranged from 0.23
to 5.85% [16, 20,45-47, 87].
The content of potassium in the studied SC ranged from 2.7 to 12.8%, with an average of 5.8% (Table 3-6). The
overall distribution of % K for the SC samples is presented in Appendix B (Figure B-5). Approximately 10% of the SC
samples contained K at concentrations greater than 9% and samples from Facility D contained the highest K content
while samples from Facility N had the lowest K content (Appendix B, Table B-7). In previously-published research,
the total K content in SC ranged from 0.48 to 3.74% [16, 20, 45-47, 87].
The average sodium content was 10% (Table 3-6), following a normal distribution (Appendix B, Figure B-6). SC from
Facility M had significantly lower Na content than SC from any other facility (Appendix B, Table B-8). In previously-
published documents, the total Na content in the SC ranged from 0.5 to 8.5 % [16, 20, 45-47, 87].
3.4.3 Trace Metals Content
The metals found in trace concentrations in SC samples were Arsenic (As), Cadmium (Cd), Chromium (Cr), Copper
(Cu), Manganese (Mn), Lead (Pb), Selenium (Se), and Zinc (Zn). The concentrations of the trace metals detected in
SC samples are presented in Table 3-7.
Table 3-7: Trace metal content in salt cake (mg kg"1)
Metal
As
Cd
Cr
Cu
Mn
Pb
Se
Zn
Mean
14±8.8
0.33±0.3
330±190
880± 1,400
1,400±1,000
43±58
9.9±7.1
750±620
Median
11
0.25
280
380
1,200
21
8.5
550
UCL95
17
0.43
390
1,300
1,700
62
12
950
Range
2.8-41
0.02-1.1
78-840
35-6,200
130-5,300
4.6-310
1.3-30
110-2,700
Arsenic was detected in all 39 SC samples analyzed. On average, the SC samples contained 14 mg kg"1 As, with a
range of 2.8 to 41 mgkg"1, as presented in Table 3-7. Approximately 80% of the SC samples contained As at
concentrations less than 20 mg kg"1, as presented in Appendix B (Figure B-7). Samples from Facility C and Facility M
had the highest As content (22 and 30 mg kg"1, respectively), as presented in Appendix B (Table B-9). It has been
reported that As can be used as a component of Al alloys [89].
Every SC sample analyzed had cadmium content greater than the MRL. On average, the SC samples contained Cd at
0.33 mg kg"1 (Table 3-7). There was a high level of variability in the samples with the Cd concentration ranging from
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0.02 to 1.1 mg kg'1 (Appendix B, Figure B-8 and Table B-10). Approximately 80% of the SC samples contained Cd at
concentrations less than 600 ^g kg'1. It is known that Cd is used in some Al alloys [89].
Chromium was detected in all SC samples, with an average value of 330 mg kg'1 (Table 3-7). There was a measurable
level of variability in the samples, with concentrations ranging from 78 to 840 mg kg"1 (Appendix B, Figure B-9 and
Table B-l 1). Approximately 85% of the SC samples contained Cr at concentrations less than 500 mg kg"1. Cr is known
to be a constituent in some Al alloys [89].
The average copper content measured in SC was 880 mg kg"1, with a range of 35 to 6,200 mg kg"1 (Table 3-7). Twenty
percent of the SC samples contained Cu at concentrations greater than 1,000 mg kg"1 (Appendix B, Figure B-10). The
total Cu content in samples from Facility J was significantly higher than those from all other facilities (Appendix B,
Table B-12). In previously-published research, the total Cu content in SC ranged from 50 to 600 mg kg"1 [16, 20, 45-
47, 87]. Cu also can be a constituent in Al alloys [89].
Manganese was detected in all SC samples, with an average concentration of 1,400 mg kg"1 as presented in Table 3-7.
Measured concentrations ranged from 130 to 5,300 mg kg"1 (Table 3-7). Approximately 75% of the SC samples
contained Mn at concentrations less than 2,000 mg kg"1 (Appendix B, Figure B-l 1). Only the samples from Facility N
had significantly lower concentration of Mn (Appendix B, Table B-13). Previously-published research shows that the
total Mn content in the SC samples ranged from 47 to 1,400 mg kg"1 [16, 20, 45-47, 87].
Lead was detected in all SC samples analyzed. The average Pb content measured was 43 mg kg"1 and ranged from 4.6
to 310 mg kg"1 (Table 3-7). Approximately 10% of the SC samples contained Pb at concentrations greater than 100 mg
kg"1; most of these samples were from Facility J (Appendix B, Figure B-12 and Table B-14). In previously-published
research, the total Pb content in SC ranged from 190 to 1,000 mg kg"1 [16, 20, 45-47, 87]. Pb can be a constituent in Al
alloys [89].
Each SC sample had detectable levels of Se, with an average of 9.9 mg kg"1 and a range of 1.3 to 30 mg kg"1 (Table 3-
7). Around 80% of the SC samples contained Se at concentrations less than 15 mg kg"1 (Appendix B, Figure B-13).
The concentrations of Se in samples of each facility are presented in Appendix B (Table B-15). Hagelstein reported the
observation of Se content in SC from 0.18 up to 156 mg kg"1 [90]. Se can be used a constituent in Al alloys [89].
Zinc was detected in all SC samples. The average Zn content measured was 750 mg kg"1 with a range of 110 to 2,700
mg kg"1 (Table 3-7). Approximately 80% of the SC samples contained Zn at concentrations less than 1,000 mg kg"1
(Appendix B, Figure B-14). Similar to Cu and Pb, the content of Zn from Facility J was much higher than that from all
other facilities (Appendix B, Table B-16). In previously published research, the total Zn content in the SC ranged from
120 to 3,000 mg kg"1 [16, 20, 45-47, 87]. Zn can be used a constituent in Al alloys [89].
Although the trace metals content had a high degree of variability, there were correlations between some metals and
the Al content (Appendix B, Table B-17). For example, the As content showed positive correlation with the total Al
content in the SC samples analyzed. Both correlation coefficients of Pearson product moment and Spearman rank
order were statistically significant (p < 0.01). Similar observations can be made for the other positively correlated
metals (Cd, Cr, Cu, Pb, Mn, Se and Zn) as presented in Appendix B (Table B-17). This may indicate that the source of
these metals in the SC is most likely Al alloys and not as impurities with the recycling.
3.5 Leachable Elements from Salt Cake
Leachable element content was measured following the reaction of SC with water (Liquid to Solid (L/S) ratio was
20:1). After filtration through a 0.45-um PVDF filter, the anions (F, Cl", SO42") were analyzed using 1C with
appropriate dilution (no acidification) [75], and acidified samples were analyzed for Al, Ca, Cr, Cu, Fe, Mg, Mn, K,
Se, Na, andZnby ICP-AES [73] and trace metals (As, Cr, Pb, and Se) were measured by AA [74]. Because of its low
total concentration, Cd was not analyzed for. For the purpose of this section, the teachability of an element is defined
as the percentage of the total leachable content divided by the total concentration of the element in the SC.
,. , T i i .1. Leachable metal concentration „ nnn, ^ ,^
Metal Leachabihty = x 100% (3-1)
Total metal concentration
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3.5.1 Leachable Aluminum (Al)
Al was detected in all leachate samples analyzed (MRL = 0.095 mg I/1). The average concentration of leachable Al
was 41 mg I/1, and ranged from 2.2 to 150 mg I/1 as presented in Table 3-8.
Approximately 75% of the SC samples exhibited a leachable Al concentration greater than 25 mg I/1 as shown in
Appendix B (Figure B-15). The overall teachability of Al was 0.6% with approximately 80% of all SC samples
leaching less than 1% of the total Al in the sample. A significantly positive correlation between leachable Al and pH of
the SC was observed and the coefficient of Pearson product moment and Spearman rank order were 0.784 and 0.813 (p
< 0.001), respectively (Appendix B, Figure B-16).
3.5.2 Leachable Major Metals
Ca was detected in all 39 leachate samples analyzed. The average leachable Ca concentration was 65 mg I/1, and
ranged from 0.33 to 400 mg L"1 (Table 3-9). Most of the leachate samples had a Ca concentration less than 80 mg L"1
(Appendix B, Figure B-18). A high level of variability of Ca teachability in the SC was found, with a range from 0.13
to 67% (Appendix B, Table B-18).
Table 3-8: Leachable aluminum (mg L"1)
Facility
B
C
D
E
F
H
J
L
M
N
Sample ,.„
f Mean
number
4 68±57
2 14±2.5
4 24±11
2 31±14
5 66±36
5 48±9.3
4 32±45
5 42±8.3
4 23±9.3
4 29±14
UCL95
160
37
41
150
110
65
100
52
46
51
Range
25-150
13-16
13-35
22-41
27-110
38-61
2.2-99
32-52
13-31
20-49
All Facilities 39 41±30 51 2.2-150
Table 3-9: Major metal teachability from salt cake
Metal
Ca
Mg
K
Na
Concentration mg L'1
Mean
65±100
0.10±0.33
2,500±1,000
2,700±400
Range
0.33-400
0.001-2
1,100-5,600
1,700-3,500
Percent Leached (%)
Mean
11±15
0.01±0.03
87±6.5
54±7.4
Median
2.5
0.002
87
53
UCL95
16
0.02
89
56
Range
0.13-67
0-0.14
70-100
42-82
Eleven of the 39 leachate samples analyzed contained Mg at a level above the MRL. The average leachable Mg
concentration was 100 (o,g L"1, with a range between 10 and 2,000 (o,g L"1 (Table 3-9). The concentrations of Mg in the
leachate of SC from each facility are presented in Appendix B (Table B-19). Though the variability of Mg
concentration in leachate was quite high, the teachability of Mg was fairly uniform compared with the other elements -
all samples had low teachability (0 to 0.14%) (Table 3-9). Approximately 90% of the samples had teachability of less
than 0.03% (Appendix B, Figure B-19), suggesting that Mg minerals present in SC were not readily soluble in water.
Only one leachate sample from Facility N was found to leach detectable levels of Fe, at 0.28 ug L"1. Therefore, the
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teachability of Fe was very low (less than 0.04%). Detectable concentrations of K were measured in all 39 leachate
samples. The average leachable K concentration was 2,500 mg I/1, with a minimum of 1,100 mg I/1 and a maximum
of 5,600 mg L"1 (Table 3-9). The concentration of K in the leachate of SC from each facility is presented in Appendix
B (Table B-20). Unlike Mg and Al, the teachability of K from SC was relatively high (from 70 to 100%) and uniform
across all samples (Table 3-9 and Appendix B, Figure B-19).
Similar to K, detectable concentrations of Na were measured in all 39 leachate samples. The average leachable Na
concentration was 2,700 mg L"1, with a range from 1,700 to 3,500 mg L"1 (Table 3-9). The concentration of Na in the
leachate of SC from each facility is presented in Appendix B (Table B-21). The average teachability of Na in SC was
54% and ranged from 42 to 82% (Appendix B, Figure B-20).
3.5.3 Leachable Trace Metals
The average leachable As concentration was 2.0 (o,g L"1, and ranged between 1.8 and 3.6 (o,g L"1 (Table 3-10)
(concentrations < MRL = MRL or 1.8 (o,g L"1). A total of seven of the 39 leachate samples analyzed had As levels
greater than the MRL, which were from Facilities B, E, H and J (Appendix B, Table B-22). The overall teachability of
As in SC was low, 0.4%, with a range of 0.09 to 1.3% (Appendix B, Figure B-21 and Table 3-10).
Eleven of the 39 leachate samples analyzed were above the MRL for Cr. The average leachable Cr concentration was
1.5 (o,g L"1, with a range between 0.75 and 4.6 (o,g L"1 (Table 3-10). The concentration of Cr in the leachate of SC from
each facility is presented in Appendix B (Table B-23). The mean overall teachability of Cr in SC was very low, 0.01%,
with a range from 0.002 to 0.09% (Table 3-10 and Appendix B, Figure B-22).
Table 3-10: Trace metal concentration in leachate of salt cake (ug L"1)
Metal Leached Concentration (jig L'1)
As
Cr
Cu
Mn
Pb
Se
Zn
Mean
2.0±0.5
1.5±2.3
73±220
19±1.6
3.3±2.0
24±40
26±43
Median
1.8
0.75
7.1
19
2.5
10
5.2
UCL95
2.2
2.2
150
20
3.9
38
40
Range
1.8-3.6
0.75-4.6
7.1-1000
16-25
2.5-10
10-190
5.2-200
Percent Leached (%)
Mean
0.41±0.27
0.01±0.02
0.18±0.26
0.06±0.07
0.50±0.42
5.3±4.8
0.08±0.13
Median
0.4
0.01
0.07
0.03
0.4
4
0.03
UCL95
0.5
0.02
0.3
0.08
0.6
7
0.1
Range
0.09-1.3
0.002-0.09
0.01-1.2
0.01-0.32
0.02-1.6
0.8-21
0.001-0.8
Sixteen of the 39 leachate samples analyzed were above the MRL for Cu, and some detected concentrations were
elevated, up to 1,000 (o,g L"1. The average leachable Cu concentration was 73 (o,g L"1, with a range from 7.1 to 1000 (o,g
L"1 (Table 3-10). The concentration of Cu in the leachate of SC from each facility is presented in Appendix B (Table
B-24). The overall teachability of Cu in SC was 0.18%, ranging from 0.01 to 1.2% (Appendix B, Table B-24 and
Figure B-23).
Mn was detected in all 39 leachate samples analyzed (MRL = 14 (o,g L"1). The concentration of Mn in leachate fell in a
relatively narrow range, from 16 to 25 (o,g L"1 (Table 3-10). The concentration of Mn in the leachate of SC from each
facility is presented in Appendix B (Table B-25). The average teachability of Mn in SC was also relatively low
(0.06%) (Table 3-10) and 70% of the samples had a teachability of less than 0.05% (Appendix B, Figure B-25).
Seven of the 39 leachate samples analyzed were above the MRL for Pb. The average leachable Pb concentration was
3.3 M-gL"1, with a range between 2.5 and 10 |agL-1 (Table 3-10). The concentration of Pb in the leachate of SC from
each facility is presented in Appendix B (Table B-26). The overall teachability of Pb in SC was low, 0.5%, with a
range from 0.02 to 1.6% (Table 3-10). Detectable concentrations of Pb were found in samples from a relatively low
number of facilities (Appendix B, Table B-26).
Only 11 of the 39 leachate samples analyzed were above the MRL for Se, but detected concentrations were as high as
190 (o,g L"1. The average leachable Se concentration was 24 (o,g L"1 (Table 3-10). The corresponding teachability ranged
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from 0.8 to 21%, with an average of 5.3% (Table 3-10). Approximately 10% of the samples had greater than 12%
teachability (Appendix B, Figure B-26), which was high compared with the other trace metals. The concentration of
Se in leachate and its overall teachability was facility-specific. For example, no Se was detected from Facilities C, D,
E, M, and N, whereas high teachability of Se was found for Facility B (37-190 (o,g L"1) (Appendix B, Table B-27).
Eighteen of the 39 leachate samples analyzed contained Zn at a level above the MRL. The average leachable Zn
concentration was 26 (o,g L"1, with a range between 5.2 and 200 (o,g L"1 (Table 3-10). The concentration of Zn in the
leachate of SC from each facility is presented in Appendix B (Table B-28). Similar to Mn, the teachability of Zn in SC
was low (from 0 to 0.8%) (Table 3-10). Approximately 70% of the leachable Zn in the SC comprised less than 0.1% of
the total Zn mass (Appendix B, Figure B-27).
3.6 Results of TCLP
The toxicity characteristic leaching procedure (TCLP) was also carried out on the SC samples. Of the 39 samples, 14
(35%) were extracted using extraction fluid #2 (1.14% glacial CH3CH2OOH, pH 2.88) due to their high buffer
capacity, whereas the other 25 samples were leached using extraction fluid #1 (1.14% glacial CH3CH2OOH-NaOH,
pH 4.95). In addition to Al, the concentration of seven out of the eight toxicity (TC) metals were measured (As, Se,
Ag, Ba, Cr, Cd, and Pb) as presented in Table 3-11. The concentrations of all seven metals (Ag, As, Ba, Cr, Cd, Pb and
Se) were consistently below their corresponding TC limit which indicates that SC from SAP are not characteristically
hazardous waste in the U.S. Facility specific results are presented in Appendix B (Table B-28 to Table B-36).
Although DIW and TCLP extraction tests were performed at the same L/S ratio (20:1), there were no significant
correlations between the results obtained from these two methods. The differences between the results obtained by
both methods may be attributed to the differences in the extraction pH. In addition, the TCLP utilizes an organic acid
(acetic acid) that tends to chelate metals.
Table 3-11: Metal concentration in the TCLP solution (mg L"1)
Metal
Al*
Ag
As
Ba
Cd
Cr
Pb
Se
Mean
90±139
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variability of each mineral and its distribution were further summarized and organized by facility, using JMP 9.0.
3.7.1 Non-Aluminum Mineral Phases
KC1 is applied in the SAP process [3, 27, 35, 36], and was detected in all the investigated SC samples. The variability
of KC1 by facility and the overall distribution are presented in Appendix B (Figure B-28); the average KC1 abundance
by weight was 8.9% with a range from 3 to 19% as presented in Table 3-12. The abundance of KC1 in SC by facility is
presented in Appendix B (Table B-39). Peterson and Revet reported that the KC1 content in two sample drosses were
16.3% and 25.0% [91], while Schmitz reported a typical KC1 content of 18 - 20% for a salt slag recycled by special
plants in Germany [27].
Significant linear correlations were found between the total K by KC1 and K2NaAlF6, quantified from XRD vs. total K
from acid digestion (r2 = 0.80, n = 39, p < 0.01); and the K content by KC1-XRD vs. leachable K content from leaching
experiments (r2 = 0.77, n = 38, p< 0.01) (Figure 3-5). This further supports the reliability of quantitative results of
mineral phase analysis in this work.
NaCl, typically added during the SAP process [3, 27, 35, 36], was detected in all of the investigated SC samples. The
overall average abundance of NaCl by weight was 18% with a range from 11 to 30%, as presented in Table 3-12. The
abundance of NaCl in SC by facility and the overall distribution and variability of NaCl in SC are presented in
Appendix B (Table B-40 and Figure B-29). Peterson and Revet reported that the NaCl content in two investigated
sample drosses were 19.1% and 24.4% [91]. Schmitz reported that the content of NaCl was approximately 40 to 50%
for typical salt slag recycled by special plants in Germany [27].
Table 3-12: Non-aluminum mineral phases (%) in salt cake
Mineral
KC1
NaCl
CaF2
CaSCM
CaCO3
SiO2
MgO
Mean±Stdev
8.9±4.0
18±3.8
5.8±2.9
5.5±1.0
1.0±0.4
1.6±0.9
1.6±1.1
Median
9.0
18
6.0
5.0
1.0
1.0
1.0
UCL95
10
19
6.1
5.9
1.3
3.6
2
Range
3-19
11-30
ND*-12
ND-8.0
ND-2.0
ND-4.0
ND-5.0
%
detected
100
100
90
85
31
85
64
*ND: Not detected.
a)
14.00
12.00
10.00
8.00
6'°°
4.00
2.00
2.00 4.00 6.00 8.00 10.00 12.00
Total K % by XRD { KCI and K2NaAIF6 ]
by2'00
10.00 -
I
° 8.00 -
.a
S. 6.00 -
4.00 -
" 2.00 -
0.00 -
°>
4.00 6.00 8.00 10.00 12.00
K% by XRD (only KCI]
Figure 3-5: Correlation of potassium by different methods
(a) Total K [blue]; (b) Leachable K [red]
CaF2 is also traditionally used in the SAP process [3, 27, 35, 36], and was detected in approximately 90% of the
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studied SC samples. The average CaF2 abundance by weight was 5.8%, with samples ranging from undetectable to
12%, as presented in Table 3-12. The variability of CaF2 by facility and the overall distribution are presented in
Appendix B (Figure B-30). The abundance of fluorite in SC from Facilities D, E, and H were significantly higher than
that of Facilities F, M and N (Appendix B, Table B-41). These differences might be related to the technology used for
the SAP [33].
In fact, the total salt content (flux), instead of the content of NaCl or KC1, was frequently reported in the literature for
SC and was observed to have a fairly wide range, from 20 to 80% [3, 35, 36]. Based on the sum of the NaCl, KC1, and
fluorite obtained in this study, the salt content in SC from SAP was about one third of the total weight (31%), with a
range from 18 to 50% as presented in Appendix B (Table B-42). The variability of total salt by facility and the overall
distribution is presented in Appendix B (Figure B-31).
CaSCM, MgO, SiO2, and CaCOs were four minor minerals identified in SC (Table 3-12). Not all of these minerals were
detected in every SC sample and the detected percentage of these minerals in the samples was 85, 85, 64 and 31%,
respectively. The average abundance of CaSCM, MgO, SiO2, and CaCOs in SC were 5.5, 1.6, 1.6 and 1.0%,
respectively, considering only the samples where these minerals were detected. More than half of these samples had
less than 2% SiO2 (74%), MgO (65%), and CaCO3 (97%) and less than 6% CaSO4. Previous research reported a MgO
content ranging from 0 to 50% with a typical range of 5 to 10%, and an SiO2 content of 0 to 10%, with a typical range
of 1 to 2% [38].
3.7.2 Aluminum Crystalline Phases
3.7.2.1 Metallic Aluminum
Metallic aluminum (Al) is generated from SAP. All SC samples had detectable abundance of metallic aluminum with
an average of 3.2% and a range from 1 to 18% (Table 3-13). It is noted that there were significant variations between
facilities. The samples from Facility M had a much higher abundance of metallic aluminum than all of the others
(Appendix B, Table B-43). In fact, there were also significant differences within samples collected from the same
facility. The variability of metallic aluminum by facility and the overall distribution is presented in Appendix B
(Figure B-32). Approximately 60% of the samples had a range of 2 to 4% metallic aluminum, 18% of the samples had
less than 2% of metallic aluminum, whereas another 18% of the samples contained a range of 4 to 8% metallic
aluminum. Only 6% of the samples contained more than 10% metallic aluminum.
Table 3-13: Aluminum crystalline phases (%) in salt cake
Crystalline Phase
Al
Total A1N
A1N
Al2.85O3.45No.55
Al2.8lO3.56N0.44
A12.78 O3.65 No.35
Total A12O3
A1203
A1267O4
Mg A12O4
K2Na A1F6
Mean
3.2±3.3
8.0±2.0
4.8±2.1
11±2.6
7.4±2.0
5.9±1.5
42±9.7
7.7±6.0
10±2.7
8.6±3.9
3.1±1.3
Median
2.0
8.0
4.0
11
7.0
6.0
40
6.0
10
8.0
3.0
UCL95
4.2
8.6
5.4
12
8.0
6.3
45
9.4
11
9.9
3.5
Range
1.0-18
3.8-13
1.0-10
6.0-17
4.0-13
3.0-10
25-68
ND*-33
5.0-17
2.0-23
1.0-6.0
% Samples
Detected
100
100
100
100
100
100
100
97
100
100
100
*ND: Not detected.
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In previously published research, the content of metallic aluminum in the SC was from 0 up to 10% [36, 38], typically
3 to 5% in North America [38]. Peterson and Revet reported that the average metallic aluminum content was 7.8% wet
weight for four SC (salty dross) samples [91]. However, crystalline metallic aluminum content has been reported to be
relatively low (1.2 to 2.8% using XRD) [45, 46, 92] in samples collected from other countries, e.g. Australia, Brazil,
and Russia. There were no correlations between the salt content and metallic aluminum in SC samples (Appendix B,
Figure B-33). It is known that both salt content and the ratio of metallic aluminum and salt content play a significant
role in the recovery of metallic aluminum in SAP [33, 93].
3.7.2.2 Aluminum Nitride and its Oxides
A1N and its oxides are one type of newly formed minerals resulting from SAP processing, and it also can originate
from the SAP source. Oxidation of A1N occurs under 650 to 1,400°C conditions [94, 95], and the presence of three
different aluminum oxide nitrides was confirmed in the investigated SC samples. Negative correlations between A1N
and its oxides were observed. The Pearson product moment correlation coefficient between A1N, and A12 ssOs 4sN0 55,
A12.siOs.seNo.44, and A12 vsOs esNo 35 was -0.42, -0.44, and -0.44 (p < 0.01), respectively. The corresponding Spearman
rank order correlation coefficients were -0.45 (p < 0.01), -0.36, and -0.35 (p < 0.05), respectively.
The average abundance of A1N was 4.8%, with a range from 1 to 10% (Table 3-13). The average abundances of
Al2.8sO3.45No.55, A12 8iOs seNo 44, and A12 vsOs esNo 35 were 11, 7.4, and 5.9% (Table 3-13), which were equivalent to 1.8,
1.0, and 0.6% of A1N, respectively. The average percentages of A1N, A12 gsOs 4sN0 55, AlisiOs.seNo^, and
AliTsOs.esNo.ss in total A1N were 58, 22, 12, and 8%, respectively. The A1N oxide (A12 gsOs 4sN0 55, A12 giOs seNo 44, and
AlijsOs.esNo.ss) content in SC by facility and their overall distributions are presented in Appendix B (Tables B-44 to B-
47 and Figure B-34). The total A1N abundance in SC by facility and the overall distribution are presented in Appendix
B (Table B-48 and Figure B-35). The total A1N abundance in SC was 8.0% with a range of 3.8 to 13% (Table 3-13).
Facility H has the highest abundance of total A1N (8.8 to 13%), while Facilities D and M had the lowest abundances
(3.5 to 8.4%). In previously-published documents, the A1N content in SC also had high variability, from 0 to 30%, and
a typical range of 15 to 30 % [38]. Kashcheev et al. reported an A1N content of 2.11% based on six samples from
Russia using XRD technology [92]; Yoshimura et al. reported an A1N content by semi-quantitative XRD as high as
28% [45], and Bruckard and Woodcock reported that A1N content of SC ranged from 1.26 to 4.8%, based on nitrogen
content [46].
The relations between A1N and the salt content in SC are complex (Appendix B, Figure B-36). It appears that KC1 and
fluorite had negative effects on the formation of A1N oxides. The Pearson product moment correlation coefficients of
KC1 to Ali8sO3.45No.s5, A12 8iO3 56N044, A12.78O3.esNo.35 and total A1N were - 0.38, -0.40, -0.36, and -0.37 (p < 0.05),
respectively. The corresponding Spearman rank order correlation coefficients were -0.38, -0.41, -0.38 and -0.35 (p <
0.05), respectively. The Pearson product moment correlation coefficients between CaF2 to A12 gsOs 4sN0 55,
AlisiOs.seNo^, and Al^sOs.esNo.ss were -0.42, -0.42, and -0.39 (p < 0.01), respectively; while the corresponding
Spearman rank order correlation coefficients were -0.41, -0.37, and -0.33 (p < 0.05), respectively.
3.7.2.3 Aluminum Oxides
Aluminum oxides are another main type of Al minerals found in SC. It was confirmed that at least Al2Os and A12 6?O4
were present in most SC samples. The other aluminum oxides included three forms of A1N oxides. Usually, one or
more aluminum oxides were detected in the same SC sample. The average alumina (Al2Os), A12 67O4, and total Al2Os
abundances in SC samples were 7.5%, 10%, and 42%, respectively (Table 3-13). The corresponding variability of
aluminum and total aluminum oxide by facility and within the overall distribution is presented in Appendix B (Figures
B-37 to B-39 and Tables B-49 to B-51).
Significant variations in quantities of aluminum oxides in SC were found, not only among different facilities, but also
among samples within the same facility. For example, alumina content in samples from Facility N was significantly
higher than that of the other facilities, whereas samples from Facility D and Facility M contained significantly lower
quantities of alumina than that of any other facilities. Previously published research also shows a wide range of
aluminum oxide in SC (20 to 60%) [27, 29, 38, 91]. Peterson and Revet also reported that the average aluminum oxide
content was 46.10% in four SC (salty dross) samples by weight [91]. Kashcheev et al. reported that the content of
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aluminum oxide in SC was 44% based on six samples from Russia, analyzed using XRD [92].
As expected, negative correlations between the aluminum oxides and metallic aluminum were found. The Pearson
product moment and Spearman rank order correlation coefficients between Al and total aluminum oxides were -0.46
(p < 0.05) and -0.37 (p < 0.05), respectively. Meanwhile, negative correlations between the salt content and the
aluminum oxides in SC samples were observed (Appendix B, Figures B-40 to B-42). For example, the Pearson
product moment and Spearman rank order correlation coefficients between KC1 and alumina were -0.37 and -0.39 (p <
0.05), respectively. The Pearson product moment and Spearman rank order correlation coefficients of CaF2 and total
aluminum oxides were -0.60 and 0.57 (p < 0.01), respectively. However, no correlations were found between NaCl
and any aluminum oxides. It should be mentioned that there was a positive correlation between KC1 and CaF2 in SC
samples.
3.7.2.4 Elpasolite and Spinel
Both elpasolite (K2NaAlF6) and spinel (MgAhO/i) are byproducts of secondary Al processes, and their presence in Al
dross is widely reported in the literature [16, 96, 97]. The average elpasolite abundance in this study was 3.1% with a
range from 1 to 6% and the average spinel abundance was 8.6% with a range from 2 to 23%, as presented in Table 3-
13. The abundance of K2NaAlF6 and MgAl2O4 by facility and the overall distribution are presented in Appendix B
(Tables B-52 and B-53 and Figures B-43 and B-44).
Significant positive correlations between the metallic aluminum and elpasolite were found in the SC samples
(Appendix B, Figure B-45). The Pearson product moment and Spearman rank order correlation coefficients were 0.85
and 0.74 (p < 0.01), respectively. Spinel was also found to be positively correlated with elpasolite. The corresponding
Pearson product moment and Spearman rank order correlation coefficients were 0.54 and 0.61 (p < 0.01), respectively.
However, no significant correlation was found between spinel and metallic aluminum. This may be attributed to the
presence of aluminum oxides.
3.8 Conclusions
A total of 39 SC samples were evaluated for MC, WHC, pH, EC, total metals, leachable metals, and crystalline phases.
Overall, SC samples were highly alkaline with a large degree of inter- and intra- sample variability which could be
attributed to variability of the Al feed stock, conditions at the processing facilities, sample processing and analysis.
There was a positive correlation between most of the trace metals concentrations and the Al content of the samples
which may be attributed to the presence of some of these metals in various Al alloys. Overall, SC samples contained
elevated total metal content but none of the SC samples exceeded the toxicity limit for seven of the eight RCRA
metals (Hg was not analyzed). While the percent metal leached was relatively low, the leachable metal content may
still pose a contamination concern and potential human and ecological exposure if uncontrollably released to the
environment. As a result, SC should always be managed at facilities that utilize synthetic liner systems with leachate
collection (the salt content of the leachate will increase the hydraulic conductivity of clay liners within a few years of
installation). The mineral phase analysis showed that various species of Al are present in the SC samples with a large
degree of variability. The relative abundance of various aluminum species was evaluated but it is noted that the
method used is a semi-quantitative method and as a result there is a limitation for the data use. The analysis only
showed a few aluminum species present in SC which does not exclude the presence of other crystalline species,
especially in light of the variability observed in the samples.
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4. SALT CAKE REACTIVITY
Three key indices were employed to evaluate the impact of reacting SC with water, particularly with regards to the
temperature profile of the reaction (the maximum temperature change, ATmax (°C) and the time to reach the highest
post-reaction temperature, tmax (h)), the heat generation, and the volume of gas generation. SC reactivity may be
impacted by various factors including but not limited to: 1) environmental temperature, 2) particle size, 3) liquid
introduction rate, 4) liquid composition, 5) L/S ratio, and 6) Al speciation in the SC sample. This chapter outlines the
impact of these factors on SC reactivity and presents the three key indices for reactivity measured for the 39 SC
samples.
4.1 Factors Impacting Salt Cake Reactivity
4.1.1 Environmental Temperature
Aluminum based reactions are often influenced by environmental temperatures. Research suggests that metallic
aluminum reaction with water requires activation [98], whereas aluminum carbide or A1N can react with water and
water vapor at room temperatures [53, 99, 100]. Temperature increase as a result of DIW addition to SC samples was
examined as a function of time under 20, 37, and 50°C environmental temperatures. As presented in Figure 4-1 (a), for
sample 2488-L, the temperature increase was minimal when DIW was added at room temperature indicating low
reactivity of the SC sample. However, when the environmental temperature was raised to 37 and 50°C, a significant
temperature increase was observed (ATmax ~ 30°C and 40°C, respectively) indicating higher degree of sample
reactivity. SC sample 2510-F exhibited different temperature profiles as demonstrated in Figure 4-1 (b). This sample
demonstrated reactivity at room temperature which resulted in an increase in the intensity of the reaction which
resulted in a higher ATmax and shorter tmax-T.
The differences between the behaviors of the SC samples in response to a change in environmental temperature could
be attributed to variation in the speciation of Al present in the SC samples. While the XRD analysis did not detect
aluminum carbide in the SC samples above its detection limit, methane presence in the gas generated from the reaction
of these samples (as will be presented later) with DIW suggests the presence of some aluminum carbide in sample
2510-M which could react with DIW at room temperature. The increase in temperature provided by the aluminum
carbide reaction may then initiate the reaction of other aluminum species present in the sample.
2488-L-SC@20C
2488-L-SC@37C
2488-L-SC @50C
Time ( hr)
Time (hr)
Figure 4-1: Impact of environmental temperature on maximum temperature change
While environmental temperature impacts the rate of reaction for SC, it has minimal impact on the heat generation
potential (kJ g"1). As presented in Table 4-1, the difference in the heat generation potential at two environmental
temperatures (37 and 50°C) was not significant. It is noted that there is some variability between heat generation at the
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two temperatures, but that could be the result of heterogeneity of the samples as well as the experimental set up and
detection.
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Table 4-1: Impact of environmental temperature on heat generation potential
Sample ID -
2502-F
2046-H
2490-L
2613-M
Heat
37°C
1.4 ±0.2
1.1±0.2
0.81±0.1
3.8±0.3
(kJg-1)
50°C
1.6±0.3
1.2±0.1
l.OiO.l
4.5±0.6
*L/S = 2:1, DIW, 5 g SC, < 0.05 mm, 5 days
Results presented here are of particular importance when trying to understand concerns associated with the disposal of
SC in MSW landfills. While the heat generation potential of a given SC sample is not impacted by environmental
temperatures, the rate at which the reaction occurs increases with increasing temperatures. MSW decomposition
process is exothermic and as a result MSW landfill temperatures are typically greater than 37°C and may reach 50°C
or greater [56, 58, 59]. The elevated temperatures present in most MSW landfills can be conducive and could initiate
SC reactions that otherwise may not take place. Furthermore, elevated temperatures can increase the rate of the SC
reaction which further propagate the reaction as described in Figure 4-2. Even outside of MSW landfills, once SC
reaction starts, it may self-propagate and increase the rate at which the reaction occurs.
Environmental System
Environmental System
,''"+Heat from Reaction'****.
/ \ /' + Heat fi^n Reaction -^
{ \ Salt Cake + Liquid |——^___Exothermic Reaction / \
U / ' '
"••^ + Boundary Heat + +
Increase in Temperature
Environmental System
x** + Heat from Reaction """"^
Salt cake + Liquid
** •* „ ___+ Boundary Heq£ - "
Exothermic Reaction Propagates N
x"'+ Heat from Reaction ***-^
S n ^.
Salt Cake + Liquid I !
T 1 I
! Salt Cake + Liquid f« "i leactionPropaeatesN U „'
\ I TT 1 I *-^ +Boundary Heat,*'
'
Environmental System
Figure 4-2: Schematic describing self-propagation of salt cake reaction
The impact of environmental temperature on gas generation potential was also evaluated. The productivity of H2 and
CH4 gases as a function of environmental temperature for randomly selected SC samples is presented in Table 4-2. It
is noted that other gases evolve from SC reaction with DIW, but H2 and CH4 are the major ones to be presented in
section 4.2.4. The results indicate that, in general, H2 productivity increased with the increase in environmental
temperature until 37°C after which no significant impacts were observed. On the other hand, CH4 productivity was
minimally impacted by changes in environmental temperatures. The H2 productivity was significantly higher than that
of CH4. This may be attributed to the limited amount of aluminum carbide in SC as compared to the relatively large
amount of metallic aluminum. Thus, at the elevated temperatures encountered in MSW landfills, elevated levels of H2
gas may be generated as a result of SC reactivity and will be of concern. It is noted that even at 4°C environmental
temperature, there was gas productivity from SC despite the minimal increase in ATmax. This shows that salt can still
react, but the reaction rate is so slow that the increase in temperature may not be observed.
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4.1.2 Particle Size
Particle size of the SC samples may also influence the reactivity of the sample and the temperature change observed.
As presented in section 2.3.2.2, the impact of SC particle size on reactivity was evaluated for three sizes. Results
presented in Figure 4-3 demonstrated that, in general, the ATmax (°C) increases with a decreasing particle size.
Furthermore, the time needed to achieve maximum temperature (tmax-i) decreases with decreasing particle size because
of a greater particle reaction surface area (i.e., specific surface area). However, the degree of this effect was sample-
specific as presented in Table 4-3. For example, the reaction of SC sample 2512-J resulted in a ATmax increase from
9.2°C for the < 2 mm size to 96°C for the fine particle size (< 0.05 mm) as compared to a ATmax increase from 51°C
for the < 2 mm size to 67°C for the < 0.05 mm for sample 2502-F.
Table 4-2: Impact of environmental temperature on gas generation potential
Sample IE
2512-J
2046-H
243 9-E
4°C
6.8±0.
0.1±0.
24±1.
Hi productivity (ml g"1)
.1
.0
1
20°C
12±0.9
8.0±0.3
30±0.7
37°C
23 ±6.6
13 ±2.5
34±1.7
50°C
18±0.5
11±0.9
32±1.3
1
0.
2
4°C
.8±0.1
5±0.08
.6±0.1
CH4 productivity (ml g"1)
2.
2
o
J
20°C
3±0.01
.5±0.1
.5±0.2
37°C
3.2±0.6
5.2±1.7
3.9±0.1
50°C
2.3±0.02
4.3±0.02
4.2±0.4
*L/S = 20:1, DIW, < 2 mm, 5 days.
98 -F
9mm, 2502-F-SC
2 mm, 2502-F-SC
0.05mm, 2502-F-SC
9mm, 2512-J-SC
2 mm, 2512-J-SC
0.05 mm, 2512-J-SC
Figure 4-3: Effect of particle size on salt cake reactivity
Table 4-3: Effect of particle size on ATmax and tmax T
Reactivity
Indices
es
H U
< 0
Sample ID
2502-F
2512-J
2046-H
Particle size (mm)
9
19
4.1
12
2
51
9.2
24
0.05
67
96
56
^ e
2502-F
2.3
1.1
0.67
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2512-J 1.6 0.81 0.23
2046-H 2.2 1.3 1.6
*17S = 1:1, DIW, 10 g SC, 37 °C, < 2 mm, 5 days.
The decrease in particle size also had an impact on the heat generation and gas generation potentials as presented in
Table 4-4 and Table 4-5, respectively. While it is difficult to quantify the sample heterogeneity and its impact on heat
and gas generation, there is a clear trend across the samples that SC with smaller particle size generate more heat and
more H2 gas (impact on CH4 generation was minimal as presented in section 4.1.1). Larger particles have smaller
surface area to volume ratio as compared to smaller particles and thus, higher SC reactivity is expected with the
decrease of particle size. From an end-of-life management perspective, data presented here suggest that SC should not
be size reduced before disposal. Also, care should be taken not to size reduce it after disposal by compacting it with
heavy bulldozers.
Table 4-4: Effect of particle size on heat generation potential (kJ g'1)
Particle size (mm)
aampie iii
2502-F
2512-J
2046-H
2490-L
9
NA*
NA
NA
NA
2
1.1
0.31
0.67
0.64
0.05
1.4
1.5
1.1
0.82
* I7S = 2:1, 10 ml DIW, 5 g SC, 5 days; NA: Not analyzed due to the instrumentation
constraints. The utilized calorimeter does not allow for the 9 mm size.
Table 4-5: Effect of particle size on salt gas productivity (ml g"1)
Sample ID*
2046-H
2512-J
2613-M
9 mm
7.7±3.2
13±8.2
49±10
H2
2 mm
13 ±2.5
23 ±6.6
58 ±9.1
0.05 mm
20 ±1.7
42 ±24
62 ±16
9 mm
6.8±2.0
1.5±1.3
4.2±3.2
CH4
2 mm
5.2±1.7
3.2±0.6
1.8±0.5
0.05 mm
5.2±2.8
1.4±0.5
1.0±0.8
* L/S = 20:1, DIW, 37°C, 5 days
4.1.3 Liquid Addition Rate
In the environment it is likely that liquids would contact SC in an intermittent fashion. To that end, a SC sample
(2069-M) received two treatments. The first treatment received 10 ml DIW at once and acted as a control (referred to
as 10G-10ML). The second treatment received DIW intermittently over a period of 72 hours and is referred to as 10G-
4-3-3ML. The temperature profiles for both treatments (Figure 4-4a) show that within the first hour, the temperature
increased by 55°C for both treatments. While the intermittent addition of DIW to the second treatment caused an
increase in temperature, that increase in AT was minor compared to the initial AT increase. It must be noted that while
the final liquid to solid ratio for both treatments was the same, the initial ratio was different. The initial liquid to solid
ratio of the control treatment was 1:1 while for the intermittent sample it was 1:2.5. Thus, while the temperature
increase in both treatments was similar, the heat generated by the control sample (within the first few hours) was
higher since the sample contained more liquid.
In a follow up experiment, the final liquid to solid ratio of the reaction was fixed; however, the initial one varied with
varying mass of SC (Figure 4-4b). In this case the initial temperature change varied as a function of the mass of SC
added. This is most likely the result of increasing mass of potentially reactive aluminum species in the reaction vessel.
Again, the largest temperature increase always occurred after the initial liquid addition; the temperature spike due to
the secondary watering was relatively minor. Nonetheless, the results of these experiments suggest that while the
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largest change in reaction temperature occurs after the first liquid addition, unless enough liquids are added to a SC
sample to fully react it, that SC would continue to react every time a new source of liquids becomes available. Since
the impact of liquid addition rate was minimal on the temperature generation, no further evaluation of this factor was
carried out on heat generation or gas generation potential.
Time (h)
b)
4G-4 ML
7G-4 ML+3 ML
10G-4ML+3ML+3L
15G-6ML+4.5ML+4.5ML
40G-10ML+10ML+10ML+10 ML
80 100 120 140 16C
Time (h)
Figure 4-4: Temperature change as a function of (a) watering schedule and (b) salt cake mass
4.1.4 Liquid Composition
The chemical composition of the liquid that starts the SC reaction may also have an impact on the observed
temperature profile. To that end, various solutions were added to the same sample of SC and temperature was
measured as a function of time as presented in Table 4-6. It is apparent that the reaction solution had an impact on the
magnitude of the reaction. The maximum temperature increase and the faster reactions occurred when SC was reacted
with alkaline solutions (0.1M NaOH) or DIW (Table 4-6). On the other hand, reactions of SC with landfill leachate or
acidic solutions showed relatively lower temperature increase and slower reactions. For example, a high pH fluid (i.e.,
0.1M NaOH) resulted in a ATmax of 54°C for sample 2613-M, whereas landfill leachate appeared to diminish the
chemical reaction rate and significantly reduce the ATmax (13°C) as presented in Figure 4-5. Similar to the impacts on
temperature change and reaction intensity, the gas productivity of SC was significantly impacted by the liquid
composition (Table 4-7) with highest H2 gas productivity obtained in the cases of alkaline solutions (0.1 M NaOH) and
DIW.
Table 4-6: Impact of liquid composition on ATmax and tmax T
Liquid
0.1MHC1
O.lMNaOH
DIW
Landfill leachate
VFA mixture
Humic acid salt
2502-F
32
56
50
12
5
3
ATmax (°C)
2555-H
14
20
19
9
9
7
2613-M
28
54
43
13
34
15
2502-F
2
0.9
1.1
3.4
7.2
12
tmax-T (h)
2555-H
3.6
2.3
2.7
3.7
4.1
4.5
2613-M
1.5
0.63
0.97
2.2
1.2
1.9
*17S = 1:1, 10 ml DIW, lOg SC, < 2 mm, 37°C, 5 days
Table 4-7: Gas generation potential (ml g'1) as a function of liquid composition
Liquid
0.1MHC1
O.lMNaOH
2512-J
16
50
H2
2046-H
17
19
2613-M
79
180
2512-J
1.7
1.6
CH4
2046-H
3.5
2.9
2613-M
0.8
2.6
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DIW
Landfill leachate
VFA mixture
Humic acids salt
39
17
38
38
20
0.5
18
12
72
55
53
59
1.3
2.0
1.3
1.7
3.2
1.2
3.5
3.5
1.8
0.8
0.8
0.9
*17S = 20:1, < 0.05 mm, 50°C, 5 days
Table 4-8: Impact of liquid composition on heat generation potential
Heat (kJ g-1)
Liquid
2502-F
*L/S =2:1, 5 g SC, <0.05 mm, 50°C, 5 days
2555-H
2613-M
0.1MHC1
O.lMNaOH
DIW
Landfill leachate
VFA mixture
1.2
1.4
1.6
1.7
1.2
1.2
1.6
0.95
0.87
1.1
2.8
3.8
5
5
4.5
2613-M-SC
{WC, 1:1)
0.1 MHjPO,
landfill leachate
DIW
0.1MHCI
O.lMNaOH
20
40
time(h)
Figure 4-5: Liquid composition impact on salt cake reactivity
While the liquids used in this evaluation had varying initial pH values, the final pH for all samples was relatively
similar at around 10. Thus, it is unclear to what degree the initial solution pH impacted the temperature increase and
the gas productivity. However, the temperature change and gas productivity may be more impacted by the sample
composition rather than by the type of liquids added. Furthermore, these results indicate that reactions of SC with
landfill leachate would be much more complex than that in the DIW system. Unlike temperature change and gas
productivity, the heat generation potential was minimally impacted by changes is solution chemistry as presented in
Table 4-8.
4.1.5 Liquid to Solid Ratio and Mass of Salt Cake
To evaluate the impact of L/S ratio on the reactivity of SC, various amounts of liquids were added to a SC sample and
reacted as presented in section 2.3.2.5. The ATmaxand tmax-T were measured as a result of varying liquid to solid ratio
as presented in Figure 4-6. The decrease observed in the ATmax accompanied with an increase in the tmax-T indicates a
reduction in the intensity of the reaction. This further implies that at some point the addition of more liquids to the SC
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sample would "cool off the reaction. The relatively small decrease in temperature as the L/S ratio doubled from 0.5
to 1 (as compared to 1:1.5) may indicate that the SC sample did not have enough liquid to completely react at the
lower ratios. The drastic decrease in the ATmax between the liquid to solid ratio of 1 and 1.5 indicates the "cooling
effects" of water on the SC reaction. Assuming a complete reaction, the heat generation potential of a sample should
not be impacted by changes to the liquid to solid ratio. Experimental data support such an observation. The heat
generation potential for a SC sample at 5:1 L/S ratio (5.2 kJ g"1) was similar to that at 10:1 ratio (5.0 kJ g"1). Similar
results were observed with different liquid compositions as presented in Table 4-9.
30 -
28 -
26 -
24 -
u 22 -
1 20 -
< IS-
IS -
14 -
12 -
10 --
•• 1.2
• 1.1
• 1.0
• 0.9
• 0.8
• 0.7
• 0.6
• 0.5
:- 0.4
0.5 1
Liquid to Solid Ratio
1.5
Figure 4-6: Impact of liquid to solid ratio on temperature change and time to reach maximum temperature
Varying L/S ratio may also impact gas generation from SC reaction since gases can dissolve in the liquid phase as
observed by others [11, 29, 46, 67, 101]. Similar to the temperature profile study, the gas production testing results
indicated variability between samples in terms of gas production and gas composition as presented in Figure 4-7 and
4-8, respectively. Liquid to solid ratio impact is mainly driven by the availability of enough liquids to completely react
with the SC sample. For example, at an L/S ratio of 5:1, samples 2512-J and 2433-C received enough liquid to
completely react and as a result the gas volume or composition did not vary when L/S ratio increased to 20:1.
However, for sample 2613 -M, the volume of gas continued to increase with increasing L/S ratio. In this case, the
volume of liquid added was not large enough to completely react with the SC sample. In general, there were no
observed impacts of L/S ratio on the relative abundance of the gas generated by SC samples as presented in Figure 4-8.
The mass of SC is another factor that may impact SC reactivity. At a fixed environmental temperature (50°C) and L/S
ratio (1:1), ATmax of SC samples 2439-E and 2482-L increased with the increase in SC mass as presented in Figure 4-
9a. Furthermore, ATmax was a function of SC mass at lower environmental temperature (37°C) or different L/S ratio
(1:0.3 and 1:0.5). On the other hand, heat generation potential, expectedly, was minimally impacted by increasing the
mass of SC (Figure 4-9b). These results indicate that heat is a better index for evaluating SC reactivity as compared to
using temperature change despite the relative simplicity of measuring the latter index. Therefore, the temperature
profile in this study, including the two indexes, ATmax and tmaXT, are related to the experimental conditions or
"operational definition." The results of the ATmaxor tmaXT only can be comparable under the fixed laboratory
conditions, and there are no physical meanings of the absolute values of these indexes if the conditions are unknown. It
is not expected that these values or changes in the current laboratory setting are presented in a full-scale landfill after
disposal of SC. However, heat is a relatively stable index to describe the reactions of SC in a landfill environment with
the relatively complicated procedures in the laboratory.
Table 4-9: Impact of liquid to solid ratio and leachate composition on heat generation potential
Heat (kJ g-1)
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Liquid
10:1(10 ml/lg) 5:1(10 ml/2g)
O.lNaOH
DIW
Landfill leachate
Volatile fatty acid mixture
3.7
5
4.5
5
4.2
5.2
5.3
5.6
*2613-M, <0.05 mm, @ 50°C.
5 10 15
Ratio of Liquid to Solids
20
Figure 4-7: Effect of liquid to solid ratio on gas production of SC reaction
a)
7 •
6 •
5 •
4 •
3 •
2 '
1 •
0
5 10 15
Ratio of Liquid to Solids
10 15
Ratio of Liquid to Solids
Figure 4-8: Effect of liquid to solid ratio on gas composition of SC reaction
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a)
Solid to
Liquid Ratio
70
60
O 50
CO 40
< 30
20
10
0
10 15
Mass of Salt Cake (g)
20
b)
2.00 i
1.60 •
1.20 •
2
- 0.80
0.40 •
0.00
Mass of Salt Cake (g)
(Liquid to solid ratio 2:1, 0.05 mm paraticle size, 37°C, DIW)
Figure 4-9: Effect of the mass of salt cake on (a) ATmax and (b) heat generation potential
4.1.6 Aluminum Speciation
Since various aluminum species tend to react with liquids at different rates, the relative abundance of various species
in SC would impact the temperature generation profile and the reaction intensity. As shown in Table 4-10, the
addition of metallic aluminum powder to the theoretical SC mix (mixture I as identified in section 2.3.2.6) had
minimal impact on ATmax and tmax-i. It is noted that some increase in temperature was observed as a result of the
addition of metallic aluminum as presented in Figure 4-10a. For example, the temperature of the sample containing
20% metallic aluminum took almost 28 h to return back to background which suggests a low intensity reaction.
However, it overall appears that the addition of metallic aluminum powder to the mix has minimal impact on its
reactivity with water. Similarly, a temperature increase was observed with the addition of A1N to the theoretical SC
and directly correlated with the A1N content (Figure 4-10b). Al4Cs also reacted with water (in the SC mix) to increase
the reaction temperature by approximately 11°C (Figure 4-10c).
The data presented above demonstrates that at concentrations many times higher than those observed in actual SC
samples, the individual aluminum species are unable to produce elevated temperatures to explain some of the field
data observed at SC disposal sites. Assuming that aluminum species present in the SC are the only species that would
react with liquids to generate heat, it is more likely that a mixture of the various species of Al would generate high
enough temperatures to explain the field observations. In another words, the reaction temperatures achieved
independently by each aluminum species are not additive which further suggests a synergetic effect between aluminum
species. For example, higher temperatures due to synergetic effects would be expected by the reactivity of a SC
simulator containing 10% metallic aluminum and 10% A1N (ATmax= 59°C) or 20% metallic aluminum and 5% Al4Cs
(ATmax= 32°C) than by merely adding ATmax for each one of those species (3 + 19 = 22°C, or 3 + 11= 14°C, based on
the data presented in Table 4-10).
(c)
Figure 4-10: Temperature increase after the addition of (a) Al (b) A1N (c) AUCs in SC stimulators
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Table 4-10: Impact of aluminum speciation on temperature change in SC simulators
Aluminum Al A1N AUCs Mix ATmax tmax-T
speciation (%) (%) (%) (%) (°C) (hrs)
Al
A1N
A14C3
A1/A1N
A1/A14C3
5
10
20
0
0
0
0
5
5
10
10
20
20
5
10
20
0
0
0
2
5
10
0
1
2
2
10
1
2
0
0
0
0
0
0
0
0
0
5
0
0
0
0
0
0
5
5
5
95
90
80
98
95
90
95
94
93
88
80
79
78
90
85
75
2.9
3.0
2.9
3.9
6.3
19
12
13
15
33
59
30
49
14
19
32
0.13
0.13
0.17
0.03
3.9
3.1
2.6
5.2
5.1
2.6
2.5
3.2
1.8
2.5
2.8
2.5
Upon the addition of A1N and metallic aluminum to the mixture I SC simulators, the reaction temperature significantly
increased above that observed for similar individual concentrations of A1N and Al (Table 4-10). For example, the
ATmax measured for a SC simulator containing 10% metallic aluminum and 2% A1N was four times more than that
generated by each individual species (Table 4-10). The temperature difference might be attributed to the interaction of
a)5
AIN Effect
-1%AIN 5%AI, 94% Mix I
•1%AIN, 20%AI, 79% Mix I
2%AIN, 5% Al, 93% Mix I
•2%AIN,20%AI, 78% Mix I
Time( h)
bf
AI4C3 Effect
5%AL4C3, 5%AI, 90% Mix I
5%AL4C3,10% Al, 85% Mix
5%AL4C3, 20% Al, 75% Mix
Figure 4-11: The impact of the addition of A1N and AUCs in SC simulators on the temperature changes
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Al,0, Effect
20%AI, 27% KCI and 54% Nad
5% AIM, 10% Al, 28% KCI and 57% NaCI
5%AIN, 20% Al, 25% KCI and 50% NaCI
10%AIN, 10% Al, 27% KCI and 54% NaCI
10%AIN, 20% Al, 23% KCI and 57% NaCI
Tlme( h)
Figure 4-12: The role of AhOs in SC simulators on the temperature changes
Table 4-11: Impact of aluminum speciation in SC simulators on the heat generation
... ., ..-. ., „ Total Heat
Aluminum Al A1N AUCs ,, ^
„ • _ j. • _ / \ / \ / \ V •*" /
spetiaiioii
Al
A1N
A14C3
A1/A1N
A1/A14C3
\Z)
1
0
0
0
0
0
0.5
0.5
1.0
1.0
2.0
2.0
0.5
1.0
\Z)
0
0.5
1
2
3
0
0.2
0.5
0.2
0.5
0.2
0.5
0
0
\Z)
0
0
0
0
0
1.0
0
0
0
0
0
0
0.2
0.2
37°C
ND
2.5
5.5
12
17
9.0
8.1
11
16
18
28
32
ND
ND
50°C
ND
2.5
3.2
9.4
17
15.6
11
14
20
24
37
39
9.8
20
*ND: not detected
A1N with metallic aluminum. Furthermore, as presented in Figure 4-11, the addition of various species also tends to
increase the rate of the reaction by reducing the time it takes to achieve the maximum temperature. A similar
synergetic effect on the reaction of aluminum with water was also observed in the presence of aluminum carbide
(Figure 4-11).
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40
30 --
§ 20 :-
a
10 --
50°C
ie:
• 0.2 gAIN, r2 = 0.99
• 0.5 gAIN, r2 = 0.99
• LOgAlN, r2 = 0.99
4-
0.5 1 1.5
Amount of Metallic Al ( g)
Figure 4-13: The role of A1N in SC simulators on heat generation potential at 50 °C
The synergetic effects of Al species in SC samples are rather complicated. For example, the exclusion of AhOs from
the mixture containing 10% A1N and 20% metallic Al resulted in an increase in tmax-T by ~ 12 h as presented in Figure
4-12. It is noted that A12O3 is a relatively non-reactive Al species. Similar to temperature change, Al species had
significant impacts on the heat generation potential from SC. The data presented in Table 4-11 indicate that mixture of
A1/A1N or Al/ALtCs generated significantly higher heat as compared to that of individual Al species which is indicative
of "synergetic effects" as previously concluded with the temperature increase data. Additionally, at the same A1N
content, the heat generation potential increased with the increase in Al content following a linear relationship (Figure
4-13). When the A1N content was increased from 0.2 to 1.0 g, similar relationship was observed with minimal impact
on the value of heat generated (Figure 4-13). In other words, at the same Al content, the difference in heat generation
potential was minimal when the A1N varied between 0.2 and 1.0 g (Table 4-11). This indicates that the presence of
A1N in SC is necessary for the reaction to generate measurable heat; however, the magnitude of heat generation is not
linearly correlated to the amount of A1N.
4.2 Reactivity Indices
4.2.1 Maximum Temperature Change (ATmax)
SC samples were reacted as outlined in section 2.3.3 and the reaction temperature was monitored for 72 h. A
temperature increase above background was observed in all 39 SC samples analyzed (at 37 and 50°C environmental
temperature conditions). On average, ATmax at 37°C and 50°C were 22 and 29°C, and ranged from 3.4 to 64 and 4.4 to
56°C, respectively, as presented in Table 4-12. The details of the temperature profile investigation results are provided
in Appendix D.
Based on the ANOVA test with the facility and environmental temperature, the ATmax at the 50°C is significantly
higher than that at 37°C (p < 0.01). This supports the earlier conclusion that environmental temperatures can impact
the reaction rate of SC samples. For instance, at an environmental temperature of 37°C, approximately 80% of the
samples exhibited a ATmax < 25°C; while at an environmental temperature of 50°C, approximately 50% of the samples
exhibited a ATmax < 25°C. These results suggest that environmental temperature has significant implications for the
disposal of SC in MSW landfills. Depending on their design and capacity, MSW landfills tend to be well insulated
and operate at elevated temperatures (compared to ambient conditions) and as a result, the reaction of SC with liquids
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tends to become more problematic. The elevated temperatures combined with the leachate in MSW landfills may
initiate the SC reaction with liquids and the insulating properties of the MSW can further intensify the reaction.
Table 4-12: ATmax (°C) for salt cake reaction by facility
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Sample
number
4
2
4
2
5
5
4
5
4
4
39
Mean
11+2.7
6.7+4.7
12+1.7
16+0.1
50+6.4
18+3.8
8.0+1.1
29+11
44+18
8.3+2.7
22+17
37°C
UCL95
16
49
15
17
57
23
9.7
43
72
13
28
Range
8.5-15
3.4-10
10-14
16-16
39-56
14-24
6.6-9.2
15-44
20-64
6.7-12
3.4-64
Mean
18+6.9
5.7+1.8
18+1.5
23+0.4
48+2.7
40+9.0
15+5.8
37+9.8
42+15
14+5.1
29+16
50°C
UCL9s
29
22
21
27
52
51
24
49
66
22
34
Range
13-28
4.4-6.9
17-20
23-23
45-52
34-56
9.4-23
28-51
22-56
7.0-18
4.4-56
4.2.2 Time to Reach the Maximum Temperature (tmax-x)
While evaluation of ATmax can provide information with regards to the reactivity of the SC samples, the time it takes a
sample to reach the maximum temperature (tmax-i) can provide some insight into the intensity of the reaction. To that
end, tmax-i for SC samples was evaluated at the two environmental temperatures examined. The average tmax-T was
observed to be 1.6 and 0.9 h, with a range of 0.5 to 4.1 and 0.3 to 2.1 h, at 37°C and 50°C, respectively, as presented in
Table 4-13.
Table 4-13: tmax T (h) for salt cake reaction by facility
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Sample
number
4
2
4
2
5
5
4
5
4
4
39
Mean
2.2+0.46
2.5+2.3
1.4+0.42
1.1+0.14
0.94+0.21
2.4+0.49
1.2+0.25
1.5+0.43
1.1+0.49
2.3+0.79
1.6+0.79
37 °C
UCL95
2.9
23
2.1
2.4
1.2
3.0
1.6
2.0
1.8
3.5
1.9
Range
1.5-2.6
0.9-4.1
0.8-1.7
1-1.2
0.7-1.2
1.7-2.9
0.9-1.5
1-1.9
0.5-1.7
1.3-2.9
0.5-4.1
Mean
1.0+0.29
2.1+0.07
0.52+0.17
0.80+0.14
0.48+0.08
1.0+0.16
0.85+0.21
0.68+0.18
0.50+0.28
1.30+0.50
0.85+0.44
50 °C
UCL95
1.5
2.7
0.79
2.1
0.58
1.2
1.2
0.90
0.95
2.1
0.99
Range
0.7-1.3
2-2.1
0.3-0.7
0.7-0.9
0.4-0.6
0.8-1.2
0.6-1.1
0.4-0.9
0.3-0.9
0.7-1.9
0.3-2.1
As expected, the time to reach the highest temperature at the 50°C environmental condition was significantly less than
that at the 37°C (p < 0.01, ANOVA test). There was also an inverse correlation between the ATmax and t-maXT. The
Pearson product moment and Spearman rank order correlation coefficients at 37°C were -0.552 and -0.483 (p < 0.01),
respectively. The corresponding coefficients at 50°C were -0.576 and -0.586 (p < 0.01), respectively. While the heat
generation potential per gram of SC sample is a sample specific parameter, the results here suggests that higher
environmental temperatures tend to intensify the SC reaction. This means that with increasing temperature the rate of
SC reaction will also increase. As stated earlier, this is of particular significance for the disposal of SC. Depending on
their design and capacity, MSW landfills tend to be well insulated and operate at elevated temperatures. When these
conditions exist, the reaction of SC with liquids tends to become more problematic since the elevated temperatures in
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MSW landfills may initiate the SC reaction and the insulating properties of the MSW may further intensify the
reaction. Furthermore, the self-propagation effect that was stated earlier can also magnify the impact of the reaction.
4.2.3 Heat Generation Potential
The heat generation potential of SC was evaluated as described in section 2.3.3.2. Based on the results of factors
impacting SC reactivity, heat generation was completed only at 37°C environmental temperature. Earlier results
(section 4.1.1) demonstrated that heat generation potential, in general, is minimally impacted by environmental
temperature. Results are outlined in Table 4-14 and the heat ranged from 0.2-3.6 kJ g"1 with an average of 1.0 kJ g"1.
Samples from Facilities B and N had the lowest heat generation potential while sample from Facility M had the
highest. Heat generation showed a correlation with metallic aluminum abundance of the samples but since the XRD
data are semi-quantitative in nature, an accurate relationship between Al content and the heat generation of SC cannot
be drawn. Given the wide range of variables that impact SC reactivity, it may be very simplistic to conclude that heat
generation and reactivity are correlated to a single parameter. Furthermore, there was a positive correlation of all
samples between the ATmax and heat as presented in Figure 4-14 (r2= 0.62, p< 0.01, andp = 0.95 bivariate normal
ellipse is the green region in the plot), though the responses were different among facilities (p < 0.01, ANOVA test).
Table 4-14: Heat (kJ g *) for salt cake reaction by facility at 37 °C
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Sample
number
4
2
4
2
5
5
4
5
4
4
39
Mean
0.43±0.20
0.65±0.11
0.52±0.21
1.0±0.27
1.3±0.42
1.0±0.20
0.93±0.50
0.82±0.19
2.8±1.1
0.43±0.27
1.0±0.77
UCL95
0.76
1.7
0.86
3.4
1.9
1.3
1.7
1.1
4.5
0.85
1.3
Range
0.20-0.70
0.57-0.73
0.4-0.84
0.81-1.2
1.0-2.1
0.74-1.2
0.41-1.5
0.64-1.2
1.3-3.6
0.28-0.83
0.20-3.6
20 40
AT.max(°C)
Figure 4-14: Correlation between ATmax and heat generation
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4.2.4 Gas Generation Potential
The volume of gas generated as a result of SC contact with DIW at 50°C environmental temperature with a L/S ratio
of 20:1 during 5 d reaction was measured for all SC samples collected. As presented in Table 4-15, the net gas volume
generated ranged from 1.5 to 210 mlg"1 of SC with an average of 35 mlg"1 (35 m3ton"1). Sample 2609 from Facility M
generated the largest volume of gas (210 mlg"1 of SC) while Sample 2536 from Facility D generated the lowest (1.5
ml g"1). Half of the samples evaluated generated less than 22 ml g"1 of SC. The detailed gas volumes generated from
SC reaction with DIW by facility and the gas composition are presented in Appendix E (Table E-l). It is noted that
while this test was carried out over a period of 5 d, most likely the gas generation occurred over a much shorter period,
perhaps within 24 h. As expected, there was a positive correlation between the gas volume generated and the heat
generation potential (Figure 4-15, r2= 0.597,/? <0.01). The ANOVA for Regression tests further demonstrated that the
facility is not related to the correlation directly (p = 0.34).
Table 4-15: Total generated gas volume (ml g"1) from salt cake reactivity
Sample
number
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N 1
All Facilities
4
2
4
2
5
5
4
5
4
4
39
17±9.9
28±4.0
18±11
36±11
48±12
15±5.1
26±7.1
20±16
130±75
18±3.9
35±40
33
64
35
130
62
22
37
39
250
24
48
7.5-30
25-31
1.5-25
28-43
31-60
9.1-22
19-35
1.5-40
47-210
12-221
1.5-210
0 30 60 90 120 150 180 210
Generated gas volume
Figure 4-15: Correlation between gas volume generated and heat generation
To determine the composition of the generated gas, H2, CH4, Ammonia, N2O and H2S concentration were measured.
However, H2S concentration was non-measurable because the adopted technique needed relatively large gas volumes
that were not generated by the SC reaction.
4.2.4.1 Hydrogen (H2)
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Hydrogen was the dominant gas generated (median 84% as presented in Figure 4-16) by the interaction of SC with
water and was detected in all but one sample. As presented in Table 4-16, the overall concentration of H2 in the
collected gas samples ranged from below the MRL (< 0.14%) to 95%, with an average of 79%. It should be noted that
the percentages presented here are based on the evolved gas generated from the reaction of the SC samples. The
average productivity of H2 from SC was 1.2 mmol g"1, or 27 m3 tonne"1 (Table 4-16). Most SC samples had a
productivity of less than 2 mmol g"1 or 50 m3 tonne"1, but some samples released a considerable amount of H2 (e.g.,
one tonne sample of 2609-M could produce as high as 180 m3 H2) in the current laboratory setting. Based on the
samples evaluated, a conservative estimate of the mean (UCL9s on the mean) for the productivity of H2 from SC is
approximately 39m3 tonne"1 of SC.
1 :
0 20 4
|
0 6
' J5:
0 SO 10
-0.50
-0.40
-0.30 =
JD
O
-0.20°"
-0.10
a
Hydrogen concentration(%)
Figure 4-16: Distribution of hydrogen concentration from gas generated by salt cake reaction
Table 4-16: Hydrogen generation from salt cake reaction
Facility
B
C
D
E
F
H
J
L
M
- 1
All Facilities
Sample
number
4
2
4
2
5
5
4
5
4
4
39
Productivity
(mmol g"1)
Mean
0.51±0.33
0.96±0.16
0.56±0.38
1.2±0.39
1.7±0.39
0.50±0.13
0.90±0.30
0.60±0.49
5.0±3.1
0.60±0.12
1.2±1.6
UCL95
1.0
2.4
1.2
4.8
2.1
0.63
1.4
1.2
9.8
0.78
1.8
Concentration
(%)
Mean
70±7
85±10
59±40
85±15
86±3
76±5
85±5
70±15
95±3
84±4
79±16
UCL95
72
85
72
85
87
78
87
75
96
85
84
A positive correlation was observed between the ATmax and the H2 productivity (Figure 4-17a) as well as heat and the
H2 productivity (Figure 4-17b, r2= 0.720, p< 0.01). The ANOVA for Regression tests indicated that the contribution
of facility is not significant (p = 0.26). For example, the Pearson Product Moment and Spearman Rank Order
correlation coefficients for ATmax and productivity of H2 were 0.544 (p < 0.01) and 0.445 (p < 0.01) at 37°C and the
corresponding coefficients were 0.438 (p < 0.01) and 0.430 (p < 0.01) at 50°C. The presence of H2 gas at such high
levels poses a particular concern for the end-of-life management of SC. H2 is explosive in a range (in air) of 4 to 79%,
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and as a result, can potentially cause fires. H2 is of even greater concern for the landfill gas export if generated in
MSW landfills. Apart from being a fire hazard when mixed with CH4, landfill gas collection, transportation and
treatment systems are not designed to handle H2 since MSW landfill gas generally consists of CH4 and CO2 at ~ 50/50
ratio, since the full combustion requirement of oxygen for CH4 and mixed gas are different from that of H2 [102]. This
combination can make more trouble for the landfill gas transport and other gas applications [103].
According to the stoichiometry of Al reactions with water, one mole metallic aluminum generates 1.5 mole H2or 36.7
L H2 at room temperature. Compared to the results of H2 productivity in the current laboratory setting, it was found
that not all metallic aluminum in SC was reacted; on average, about one of third of metallic aluminum in SC remains
unreacted based on the semi-quantitative measurement of metallic aluminum by XRD (Figure 4-18).
a)
o
•
.• *
H2 productivity (mmol g"
b)
3 -
1 -
ITu-
246
Productivity ofH2
Figure 4-17: Relationship between (a) Hi productivity and ATmax, and (b) Hi productivity and heat generation
20 40 60 80
Pracentage of Unreacted Metallic Al
Figure 4-18: Variability of percentage of unreacted metallic aluminum in SC after gas experiments
4.2.4.2 Methane (CH4)
Methane was the second most abundant gas detected from SC reaction. CH4 was measured in 99% of the samples
evaluated (Table 4-17), but typically at concentrations less than those measured for H2. Approximately half of the
samples generated CH4 gas at less than 16% by volume (Figure 4-19). The average productivity of CH4 was ~ 0.2
mmol g"1 (4.5 m3 tonne"1 SC) as presented in Table 4-17.
Assuming that the CH4 generation resulted from the reaction of aluminum carbide with liquids, the average aluminum
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carbide content of SC would be 0.6% with a 0.8% UCL9s on the mean. These concentrations are well below the
XRD's detection limit supporting the crystalline phase analysis presented earlier. Compared to H2, the average
productivity of CH4 was about 83% lower. Only two samples of all 39 studied SC samples had a higher productivity
of CH4 than H2. Like H2, CH4 is an explosive gas and care must be taken if SC reacted with liquids. But unlike H2, in
an MS W landfill, the gas collection system is designed to handle CH4 which is a greenhouse gas generated during the
anaerobic decomposition of MSW.
44:-
; = : J5i
0!i OS OS | |
-0.40
-0.30^
!B
CD
JD
-0.20^
-0.10
0 20 40 60 80 100
Methane Concentration(%)
Figure 4-19: Distribution of methane concentration from gas generated by salt cake reaction
Table 4-17: Methane generation from salt cake reaction
„ .... Sample
Facility £
number
B 4
C
D
E
F
H
J
L
M
2
4
2
5
5
4
5
4
N 4
All Facilities 39
Productivity
(mmol g"1)
Mean
0.19±0.07
o.mo.oi
o.mo.i
0.22±0.05
0.27±0.1
0.15±0.08
0.15±0.03
0.20±0.15
0.25±0.08
0.12±0.05
0.19±0.09
UCL95
0.31
0.3
0.34
0.66
0.41
0.25
0.2
0.39
0.38
0.19
0.22
Concentration
(%)
Mean
30±7
15±1
41±40
15±2
14±3
24±5
15±5
30±16
5±4
16±4
21±17
UCL9s
37
16
80
17
17
29
19
44
8
19
26
4.2.4.3 Ammonia
Ammonia, both gaseous and aqueous, is also a byproduct of SC reaction with liquids. As presented in Table 4-18, the
average concentration of NH3 (gas) was 1.1% and ranged from 0.001 to 10% (Figure 4-20). The average productivity of
gaseous NH3 was 6.4 |amol g"1. NH3 gas has a distinctive odor and humans are able to detect it down to a level as low
as 5 parts per million (ppmv). From a human health perspective, the concentration of gaseous NH3 resulting from the
SC reaction was relatively high and can potentially be of concern.
The concentration of aqueous ammonia (NH4+) ranged from 30 to 1,480 mg L"1 with an average of 570 mg L"1 (Table
4-18). As presented in Figure (4-20) ~ 70% of the SC samples generated < 1% ammonia gas (Figure 4-20a) while ~ 20
% of the aqueous concentrations were > 1,000 mg L"1 (Figure 4-20b). The productivity in the gaseous NH3 was
significantly lower than NH4+ in the liquid despite the alkaline pH of the liquid phase. On average, the productivity of
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gaseous NH3 was only about 2% of the total ammonia productivity. This may be attributed to the fact that the
experiment was conducted in a closed system where the relatively low Henry's constant for ammonia gas (0.75atm,
[104]) resulted in the majority of the ammonia gas fraction being in the liquid phase. To put this in context, H2 and
CH4 gases have Henry's constants of 68,300 atm and 37,600 atm, respectively [104].
The total ammonia productivity ranged from 0.32 to 1.2 mmol g"1, with an average of 0.68 mmol g"1 (Table 4-18).
Around 75% of the samples had a total ammonia productivity less than 1.0 mmol g"1 (Figure 4-2 la). It is noted that
MSW landfills are open systems and thus, gaseous NH3 may be significantly higher than the levels detected in this
experiment and thus odor problems in landfills as a result of SC reactivity can still be of concern. On the other hand,
the level of NH4+ resulting from the SC reaction is significantly lower compared to the levels found in landfills.
Therefore, the ammonia generated from SC might not have a detrimental impact on the performance of MSW landfills.
Table 4-18: Ammonia generation from salt cake reaction
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Sample
number
4
2
4
2
5
5
4
5
4
4
39
NH3 (gas)
Mean
1.2+0.68
0.93+0.89
3.2+4.6
0.55+0.18
0.27+0.24
2.0+0.44
0.41+0.16
1.3+1.5
0.13+0.11
0.65+0.79
1.1+1.7
(%) NH4+ (mg L"1) Total ammonia ( mmol g"1)
UCL95
0.21
1.22
0.37
1.21
0.17
0.28
0.11
0.19
0.15
0.23
0.15
Mean
1,000+200
490+350
420+380
550+470
650+440
680+450
270+210
720+700
480+150
290+160
570+420
UCL95
1360
3610
1020
4750
1200
1240
607
1580
870
537
710
Mean
1.2+0.2
0.59+0.4
0.50+0.4
0.65+0.5
0.78+0.5
0.81+0.5
0.32+0.2
0.85+0.8
0.57+0.2
0.34+0.2
0.68+0.5
UCL95
1.6
4.2
1.2
5.6
1.4
1.5
0.72
1.9
1.0
0.63
0.84
4 6
NH3 (gas) concentration
10
b)
24%
11%
8%
1
-0.25
-0.20
-0.10
-0.05
0 300 600 900 1200 1500
NH3 (liquid) Concentration
Figure 4-20: Distribution of ammonia after salt cake reaction (a)
s), and (b) NH4+
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•0.25
-0.20
-0.15I1
-0.10°
-0.05
0.5 1 1.5
Productivity of Total Ammonia
20 40 60 80
Perecentage of Unreacted Total AIM
Figure 4-21: Distribution of the total ammonia productivity and unreacted A1N in SC after gas experiments
Based on the stoichiometry of A1N, one mole A1N or A1N oxide with water will generate one mole total NH3
Compared to the total productivity of NH3 of SC in the current laboratory setting, it was found that only about 35% of
the A1N in SC had reacted with water (Figure 4-2 Ib). XRD further confirmed that metallic aluminum and A1N can be
detected in the residue of SC, even after five month long reactions (37°C/50°C, data not shown).
4.2.4.4 Nitrous Oxide
Salt cake reaction with liquids can also generate nitrous oxide (N2O) gas which is a greenhouse gas that contributes
approximately 6% to the total radiative forcing of the earth's atmosphere. N2O gas was detected with an average
concentration of 1,200 ppbv from an extremely large range of 20 to 18,000 ppbv (Table 4-19). The productivity of
N2O ranged from 0.08 to 2.0 nmol g"1 with an average of 0.57 nmol g"1 (Table 4-19), and about half of the studied SC
samples were lower than 0.25 nmol g"1 (Figure 4-22). Research suggests that N2O gas can be generated from NH3 gas
directly [105, 106]. No correlation between N2O and the NH3 gas was observed, but a significant correlation between
the productivity of N2O and the total NH3 was confirmed (Figure 4-21). The value of productivity of N2O in this study
was only 0.01% of the productivity of NH3 gas. The correlation coefficients of Pearson Product Moment and Spearman
Rank Order were 0.522 (p < 0.001) and 0.604 (p < 0.001), respectively.
Table 4-19: Nitrous oxide generation from salt cake reaction
Facility SamPle
number
B 4
C
D
E
F
H
J
L
M
2
4
2
5
5
4
5
4
N 4
All Facilities 39
Productivity
Mean
1.2±0.6
0.21±0.1
0.82±0.7
0.09±0.02
0.38±0.5
0.37±0.4
0.59±0.9
0.62±0.7
0.81±0.7
0.28±0.2
0.57±0.59
(nmol g"1)
UCL95
2.1
1.1
1.9
0.09
1.0
0.87
2.1
1.4
1.9
0.61
0.76
Concentration
(ppmv)
Mean
2.5+2.1
0.18+0.06
5.2+8.8
0.06+0.02
0.18+0.2
0.7+1.2
0.75+1.3
0.96+0.79
0.2+0.23
0.24+0.12
1.2+3.0
UCL95
5.9
0.72
1.9
0.24
0.42
2.2
2.8
1.9
0.57
0.43
2.1
Range
0.4-4.9
0.14-0.23
0.88-18
0.05-0.08
0.05-0.52
0.15-2.8
0.07-2.7
0.08-1.8
0.02-0.51
0.16-0.42
0.02-18
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2-
'
i 1.5-
o -a
1 1
CL c 1
o —
0.5-
-
• * *
•
•
; • •. •
.'•«»W.
0 0.5
t
i
•
. ,
Total ammon
•
1
1
\s
i
5
!
]
— I
-1 '
J
1
J
J — 1
1
2
productivity (mmol/g)
Figure 4-22: Relationship between the productivity of total NHs and NiO from salt cake reaction
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5. CONCLUSION
The findings presented in this report provide valuable information that may be used by managers of SAP facilities and
solid waste disposal facilities and regulators to determine the best management practices for SC (a major type of SAP
waste). A total of 39 SC samples collected from 10 SAP facilities across the U.S. were characterized and tested for
reactivity with water under controlled laboratory conditions. The major findings of this research are highlighted as
follows:
5.1 Salt Cake Characteristics
The 39 SC samples were evaluated for moisture content, water holding capacity, pH, electric conductivity, total
metals, leachable metals, and crystalline phases. Overall, SC samples had a large degree of inter- and intra-sample
variability which could be attributed to variability of the Al feed stock, conditions at the processing facilities, and
sample processing and analysis.
The moisture content of the SC samples investigated had an average value of 0.80% and ranged from 0.01 to 2.0%
(w/w). The average water holding capacity of SC was 25% and ranged from 1.4 to 70%. SC samples were highly
alkaline. When reacted with DIW, pH 6.2, S/L ratio of 1:20, 50°C, 5d test, the pH of SC ranged from 9.6 to 11 with an
average of 10.5. The electrical conductivity (EC) of SC was high and exhibited high variability among samples. The
average EC was 30 mS cm"1 and ranged from 18 to 47 mS cm"1.
The average total Al content in the SC samples was 14%, and ranged from 6.7 to 42%. Approximately 70% of the SC
samples contained total Al at concentrations between 8 and 16%, and only 6% of the SC samples contained Al at
concentrations greater than 24%. Other metals were also detected in SC samples and the general order of the elemental
content was: Al > Na > K > Mg > Ca > Fe > Mn > Cu > Zn > S > Cr » Pb > As > Se » Cd. There was a direct
correlation between most of the trace metals concentrations and the Al content of the samples which may be attributed
to the presence of some of these metals in various Al alloys.
Al was detected in the leachate from all SC samples. The average concentration of Al was 41 mg L"1 with a range of
2.2 to!50 mgL"1. The concentrations of all heavy metals in the leachate were relatively low, at the M-gL"1 level,
quantified in the following order: Cu > Zn > Se ~ Mn » Pb, As, and Cr » Cd. The teachability of an element was
defined as the percentage of the mass leached divided by the mass determined using total metal analysis. The average
teachability Al from SC was 0.6%. Approximately 80% of the SC samples leached less than 1% of the total Al content
and the rest of the samples leached up to 2% of total Al content. The other metals in SC can be divided into three
groups based on their teachability:
• Group I which leached 60 to 100% of the corresponding metal content in SC. This group contained
potassium, sodium, and sulfur and leached in the order: K > S > Na.
• Group II (up to 20%) contained selenium, arsenic, copper, lead and zinc.
• Group III (< 1%) contained manganese, magnesium, iron and chromium.
• The teachability of calcium was highly dependent on the source of SC samples.
None of the SC samples were observed to be a characteristic hazardous waste based on TCLP. While, the SC samples
contained elevated total metal content, none of the SC samples had TCLP concentrations exceeding the toxicity limit
for seven of the eight RCRA metals (Hg was not analyzed).
The dominant crystalline Al minerals in the SC samples were metallic aluminum, aluminum nitride (A1N) and its
oxides, spinel (magnesium aluminum oxide, Al2MgO/i), elpasolite (K2NaAlF6) and different forms of aluminum oxide
(e.g., A12O3, A12.67O4). Sylvite (KC1), halite (NaCl), and fluorite (CaF2) were also identified by XRD analysis. Metallic
aluminum abundance in SC was found to have a high variability, from 1 to 18%, with an average of 3.2% of the mass;
whereas the total A1N abundance ranged from 3.8 to 13% with an average of 8%. Both aluminum carbide (Al4Cs) and
aluminum sulfide (Al2Ss) were not detected by XRD analysis.
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5.2 Salt Cake Reactivity
The temperature profile of the SC reaction with water (the maximum temperature change, ATmax (°C), the time to
reach the highest post-reaction temperature, tmax (h)), the heat generation potential, and the gas generation potential
were the key indices employed to evaluate the SC reactivity with water. The impact of various factors on SC reactivity
was also investigated. The findings of these evaluations are highlighted below:
The environmental temperature, particle size, liquid composition, L/S ratio, and Al speciation in SC were found to
significantly influence SC reactivity.
The increase in environmental temperature resulted in increasing ATmax, decreasing the tmax (h) and increasing H2
productivity. The differences between the behaviors of the SC samples in response to a change in environmental
temperature could be attributed to variation in the speciation of Al present in the SC samples. Environmental
temperature, on the other hand, had minimal impact on the heat generation potential.
The decrease in particle size resulted in an increase in ATmax and a decrease in the time needed to achieve maximum
temperature (tmax-i) because the surface area to volume ratio increases as the particle size is reduced. While it was
difficult to quantify the sample heterogeneity and its impact on heat and gas generation, there was a clear trend across
the samples that SC with smaller particle size generated more heat and more H2 gas.
The chemical composition of the liquid reacting with SC impacted the temperature change and gas generation
potential. The maximum temperature increase, faster reactions, and the higher gas productivity occurred when SC was
reacted with alkaline solution (0.1M NaOH) or DIW. Unlike temperature change and gas productivity, the heat
generation potential was minimally impacted by changes in composition of liquid.
Various aluminum species tend to react with liquids at different rates. The data presented in this report demonstrated
that the individual aluminum species are unable to produce elevated temperatures at concentrations many times higher
than those observed in actual SC samples. Thus, the results are unable to explain some of the field data observed at
SC disposal sites. The reaction temperatures achieved independently by each aluminum species are not additive which
further suggests a synergetic effect between aluminum species. Similar to temperature change, aluminum species had
significant impacts on the heat generation potential from SC. The results also showed that the presence of A1N in SC is
necessary for the reaction to generate measurable heat; however, the magnitude of heat generation is not linearly
correlated to the concentration of A1N.
The metallic aluminum in SC is the key component responsible for SC reactivity. There is a trigger effect of A1N and
Al4Cs involved in the reaction of Al with water. The trigger effect of A1N on the reaction of metallic aluminum with
DIW was demonstrated.
Based on the 39 SC samples investigated, on average, the ATmax for reaction temperatures of 37°C and 50°C was 22
and 29°C, and ranged from 3.4 to 64 and 4.4 to 56°C, respectively. The average time to reach the peak temperature
(tmaxi) for reaction temperatures of 37°C and 50°C was 1.6 and 0.9 h, and ranged from 0.5 to 4.1 and 0.3 to 2.1 h,
respectively.
The heat generation potential of the 39 SC samples ranged from 0.2 to 3.6 kJ g"1 with an average of 1.0 kJ g"1.
Heat generation showed a correlation with elemental Al content of the samples, but since the XRD data are semi-
quantitative in nature, an accurate relationship between Al content and the heat generation of SC cannot be drawn.
Given the wide range of variables that impact SC reactivity, it may be very simplistic to conclude that heat generation
and reactivity are correlated to a single parameter. Furthermore, there was a positive correlation between the ATmax and
heat.
The generated gas volume of the 39 SC samples ranged from 1.5 to 210 ml g"1 of SC with an average of 35 ml g"1 (35
m3 tonne"1) with half of the samples generating < 22 ml g"1 of SC.
Hydrogen (H2) was the dominant gas generated from SC. The overall concentration of H2 in the collected gas samples
ranged from below the MRL (< 0.14%) to 95%, with an average of 79%. The average productivity of H2 from SC was
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1.2 mmol g"1, or 27 m3 tonne"1. A positive correlation was observed between the ATmax and the H2 productivity as well
as heat.
Methane (CH4) was the second most abundant gas detected from the SC reaction. CH4 was measured in all samples
evaluated, but typically at concentrations less than those measured for H2. Approximately half of the samples
generated CH4 gas at less than 16% by volume. The average productivity of CH4 was ~ 0.2 mmol g"1 (4.5 m3 tonne"1
SC).
The average concentration of ammonia in gas was 1.1% and ranged from 0.001 to 10%. The average productivity of
gaseous NH3 was 6.4 |amol g"1. The concentration of aqueous ammonia (NH4+) ranged from 30 to 1,480 mg I/1 with an
average of 570 mg I/1. Approximately, 70% of the SC samples generated < 1% ammonia gas while ~ 20% of the
aqueous ammonia concentrations were > 1,000 mg I/1. The total ammonia productivity ranged from 0.32 to 1.2 mmol
g"1, with an average of 0.68 mmol g"1. Approximately 75% of the samples had a total ammonia productivity less than
1.0 mmolg"1.
Based on the gas analysis results and the stoichiometry of aluminum reactions, not all aluminum species in the SC
reacted with water under the investigated conditions. On average, only 65% of the metallic aluminum and 35% of the
A1N reacted with water to generate H2 or total ammonia.
5.3 Implications
While the percent metal leached from SC was relatively low, the leachable metal content may still pose a
contamination concern and potential human and ecological exposure if uncontrollably released to the environment. As
a result, SC should always be managed at facilities that utilize synthetic liner systems with leachate collection (the salt
content of the leachate will increase the hydraulic conductivity of clay liners within a few years of installation). The
mineral phase analysis showed that various species of aluminum are present in the SC samples with a large degree of
variability. The relative abundance of various aluminum species was evaluated but it is noted that the method used is a
semi-quantitative method and as a result, there is a limitation for the data use. The analysis only showed a few
aluminum species present in SC which does not exclude the presence of other crystalline species especially in light of
the variability observed in the samples.
Results presented here are of particular importance when trying to understand concerns associated with the disposal of
SC in MSW landfills. From an end-of-life management perspective, data presented here suggest that SC should not be
size reduced before disposal. Also, care should be taken not to size reduce it after disposal by compacting it with
heavy bulldozers. The MSW decomposition process is an exothermic, and as a result MSW landfill temperatures are
typically greater than 37°C and may reach 50°C or greater. The elevated temperatures present in most MSW landfills
can be conducive and could initiate SC reactions that otherwise may not take place. Furthermore, elevated
temperatures can increase the rate of the SC reaction which further propagates the SC reaction. Even outside of MSW
landfills, once a SC reaction begins, it may self-propagate and increase the rate at which the reaction occurs. While the
heat generation potential per gram of SC sample is a sample specific parameter, the results presented herein suggest
that higher environmental temperatures tend to intensify the SC reaction. This means that with increasing temperature,
the rate of SC reaction will also increase. As stated earlier, this is of particular significance for the disposal of SC.
Depending on their design and capacity, MSW landfills tend to be well insulated and operate at elevated temperatures.
When these conditions exist, the reaction of SC with liquids tends to become more problematic since the elevated
temperatures in MSW landfills may initiate the SC reaction, and the insulating properties of the MSW may further
intensify the reaction. Furthermore, the propagation effect that has been stated earlier can also magnify the impact of
the reaction.
At elevated temperatures encountered in MSW landfills, elevated levels of H2 gas may be generated as a result of SC
reactivity and will be of concern. H2 is an explosive gas, can potentially cause fires and H2 is of even greater concern if
generated in MSW landfills. Apart from being a fire hazard when mixed with CH4, landfill gas collection systems are
not designed to handle H2 since MSW landfill gas generally consists of CH4 and CO2 at ~ 50/50 ratio. Like H2, CH4 is
an explosive gas and care must be taken if SC reacts with liquids. But unlike H2, in an MSW landfill, the gas
collection system is designed to handle CH4 gas which is a greenhouse gas generated during the anaerobic
decomposition of MSW. Since the full combustion of CH4 requires more oxygen than that of H2, an unstable
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composition of landfill gas can cause trouble for its management and applications. From a human health perspective,
the concentration of ammonia gas resulting from the SC reaction was relatively high and can potentially be of concern.
Due to the fact of the level of NH4+ resulted from the SC reaction is significantly lower compared to the levels found
in MS W landfills, the ammonia generated from SC might not have a detrimental impact on the performance of
landfills.
It is important to note that all of the data presented in this report were generated under controlled conditions in a
laboratory setting with some degree of uncertainties as a result of the analytical techniques and the experimental setup
and thus, this should be taken into consideration if this data are to be used for design or modeling purposes. Also,
additional work is necessary to provide a full understanding of the mechanisms of SC reactivity when exposed to
liquids. Many questions concerning the management of SC disposal are still unanswered and more research is
necessary for determining best management practices for SC disposal.
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Secondary Aluminum Processing Waste: Salt Cake Characterization and Reactivity
7. APPENDIX A: MDL and MRL for Metal and Gas Analysis
Table A-l: Method detection limit and method reporting limit for metal analysis using ICP
Element
Al
Ca
Cu
Fe
K
Mg
Mn
Na
S
Zn
MDL
33
86
2.0
35
284
3.0
5.0
457
109
2.3
MRL -leachate
95
257
7
105
850
10
14
1400
330
5.2
MRL-solid
47
129
3.5
53
426
4.9
7.2
686
163
3.5
Table A-2; Method detection limit and method reporting limit for metal analysis using GFAA
GFAA* Standard Addition Method"
Element MDL MRL-solid MDL
(jig L"1) (mg kg -1) (jig L]
MRL-leachate
As
Cd
Cr
Pb
Se
0.67
0.21
0.97
4.4
2.2
1.0
0.3
1.5
6.6
3.3
0.5
NA
0.23
0.75
0.6
1.8
NA
0.75
2.5
10
*GFAA: Graphite furnace AA, utilized for measuring trace metals;
** Standard Addition Methods: utilized for analyzing the leachable trace metals; NA: Not analyzed
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Table A-3: Method reporting limit for gas analysis using GC
Gas MRL
H2 0.14%
CH4 0.2%
N2O 20 ppbv
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Secondary Aluminum Processing Waste: Salt Cake Characterization and Reactivity
8. APPENDIX B: Physical and Chemical Properties of Salt Cake
List of Tables
Table B-l: Physical properties of salt cake 71
Table B-2: Major elemental composition of salt cake 72
Table B-3: Trace metal content of salt cake 74
Table B-4: Total calcium content in salt cake by facility 75
Table B-5: Total magnesium content in salt cake by facility 76
Table B-6: Total iron content in salt cake by facility 77
Table B-7: Total potassium content in salt cake by facility 78
Table B-8: Total sodium content in salt cake by facility 78
Table B-9: Total arsenic content in salt cake by facility 79
Table B-10: Total cadmium content in salt cake by facility 80
Table B-l 1: Total chromium content in salt cake by facility 80
Table B-12: Total copper content in salt cake by facility 81
Table B-13: Total manganese content in salt cake by facility 82
Table B-14: Total lead content in salt cake by facility 83
Table B-15: Total selenium content in salt cake by facility 83
Table B-16: Total zinc content in salt cake by facility 84
Table B-17: Correlation coefficients between metals in salt cakes 85
Table B-l8: Leachable Ca in salt cake by facility 86
Table B-l9: Leachable Mg in salt cake by facility 86
Table B -20: Leachable K in salt cake by facility 87
Table B-21: Leachable Na in salt cake by facility 88
Table B-22: Leachable arsenic in salt cake by facility 89
Table B-23: Leachable Cr in salt cake by facility 89
Table B-24: Leachable Cu in salt cake by facility 90
Table B-25: Leachable Mn in salt cake by facility 91
Table B-26: Leachable Pb in salt cake by facility 91
Table B-27: Leachable Se in salt cake by facility 92
Table B-28: Leachable Zinc in salt cake by facility 93
Table B-29: TCLP results for Al by facility 94
Table B-30: TCLP results for Ag by facility 95
Table B-31: TCLP results for As by facility 95
Table B-32: TCLP results for Ba by facility 95
Table B-33: TCLP results for Cd by facility 95
Table B-34: TCLP results for Cr by facility 96
Table B-35: TCLP results for Pb by facility 96
Table B-36: TCLP results for Se by facility 96
Table B-37: Aluminum mineral phase in salt cake 97
Table B-38: Non-Aluminum mineral phase in salt cake 99
Table B -3 9: KC1 abundance of salt cake by facility 100
Table B -40: NaCl abundance of salt cake by facility 100
Table B-41: Fluorite abundance of salt cake by facility 101
Table B-42: Total salt content of salt cake by facility 102
Table B-43: Metallic Al abundance of salt cake by facility 102
Table B-44: Mineral A1N abundance of salt cake by facility 103
Table B-45: A12 ssOs 4sN0 55 abundance of salt cake by facility 104
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Table B-46: A12 vsOs esNo 35 abundance of salt cake by facility 104
Table B-47: A12 8iOs seNo 44 abundance of salt cake by facility 104
Table B-48: Total A1N abundance of salt cake by facility 105
Table B-49: Alumina abundance of salt cake by facility 106
Table B-49: Alumina abundance of salt cake by facility 107
Table B-50: A12.eevCM abundance of salt cake by facility 107
Table B-51: Total abundance of Aluminum oxides in salt cake by facility 108
Table B-52: Elpasolite abundance of salt cake by facility 110
Table B-53: Spinel abundance of salt cake by facility 111
List of Figures
Figure B-l: Total Al distribution in salt cake samples 75
Figure B-2: Total Ca distribution in salt cake samples 75
Figure B-3: Total Mg content distribution in salt cake samples 76
Figure B-4: Total Fe distribution in salt cake samples 77
Figure B-5: Total Kcontent overall distribution 77
Figure B-6: Total Na distribution in salt cake samples 78
Figure B-7: Total As distribution in salt cake samples 79
Figure B-8: Total Cd distribution in salt cake samples 80
Figure B-9: Total Cr distribution in salt cake samples 80
Figure B-10: Total Cu distribution in salt cake samples 81
Figure B-l 1: Total Mn distribution in salt cake samples 82
Figure B-12: Total Pb distribution in salt cake samples 82
Figure B-13: Total Se content distribution in salt cake samples 83
Figure B-14: Total Zncontent distribution in salt cake samples 84
Figure B-15: Distribution of teachability of aluminum in salt cake samples 84
Figure B-16: Correlation between leachable Al and pH in leachate of salt cake 86
Figure B-17: Distribution of teachability of Ca in salt cake samples 86
Figure B -18: Distribution of teachability of Mg in salt cake samples 87
Figure B-19: Distribution of teachability of K in salt cake samples 88
Figure B-20: Distribution of teachability of Na in salt cake samples 88
Figure B-21: Distribution of teachability of As in salt cake samples 89
Figure B-22: Distribution of teachability of Cr in salt cake samples 90
Figure B-23: Distribution of teachability of Cu in salt cake samples 91
Figure B-24: Distribution of teachability of Mn in salt cake samples 91
Figure B-25: Distribution of teachability of Pb in salt cake samples 92
Figure B-26: Distribution of teachability of Se in salt cake samples 93
Figure B-27: Distribution of teachability of Zn in salt cake samples 93
Figure B-28: Distribution of the KC1 abundance in salt cake samples 100
Figure B-29: Distribution of the NaCl abundance in salt cake samples 101
Figure B-30: Distribution of the fluorite abundance in salt cake samples 101
Figure B-31: Distribution of the total salt flux in salt cake samples 102
Figure B-32: Distribution of the metallic aluminum in salt cake samples 103
Figure B-33: Relations between the abundance of metallic Al and salt in salt cake 103
Figure B-34: Overall distribution of the three aluminum nitride oxides in salt cake 105
Figure B-35: Distribution of the aluminum nitride in salt cake samples 105
Figure B-36: Relations between the abundance of A1N and salt in salt cake 106
Figure B-37: Distribution of the alumina in salt cake samples 106
Figure B-38: Distribution of A12.evCM in salt cake samples 108
Figure B-39: Distribution of total aluminum oxides in salt cake samples 109
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Date: June 6 2013
Revision No.: 1
Page 71 of 478
Figure B-40: Relations between alumina oxides and metallic Al in salt cake
Figure B-41: Relations between salt and alumina in salt cake
Figure B-42: Relations between salt and total aluminum oxides in salt cake
Figure B-43: Distribution of the elpasolite abundance in salt cake samples
Figure B-44: Distribution of the spinel abundance in salt cake samples
Figure B-45: Relations between metallic Al, elpasolite and spinel in salt cake
109
109
110
110
111
111
Table B-l: Physical properties of salt cake
Sample ID
2452-B-SC
2454-B-SC
2468-B-SC
2478-B-SC
2433-C-SC
2435-C-SC
2532-D-SC
2536-D-SC
2538-D-SC
2540-D-SC
2437-E-SC
2439-E-SC
2502-F-SC
2504-F-SC
2506-F-SC
2508-F-SC
2510-F-SC
2046-H-SC
2544-H-SC
2555-H-SC
WHC %
2.43
2.23
2.96
1.69
9.93
3.02
10.96
11.36
1.97
1.38
24.38
12.78
3.07
14.86
4.95
17.8
52.86
10.97
33.87
29.43
MC%
0.51
1.26
0.43
0.66
0.52
1.31
2.22
1.3
0.15
0.51
0.74
0.77
1.02
1.08
0.99
0.67
0.04
1.15
1.51
1.12
pH
10.72
10.72
11.27
10.49
10.00
10.01
10.74
10.85
10.31
10.27
10.41
10.63
10.53
10.85
11.15
10.59
11.07
10.91
10.66
10.59
EC
mS cm"1
25.16
23.46
25.42
32.90
24.72
32.20
46.60
28.05
35.40
41.30
32.60
28.75
31.40
25.93
47.40
28.76
37.00
26.49
30.60
27.37
Sample ID
2559-H-SC
2568-H-SC
2512-J-SC
2515-J-SC
2517-J-SC
2519-J-SC
2482-L-SC
2484-L-SC
2486-L-SC
2488-L-SC
2490-L-SC
2601-M-SC
2605-M-SC
2609-M-SC
2613-M-SC
2492-N-SC
2494-N-SC
2496-N-SC
2498-N-SC
WHC %
15.7
43.58
30.19
21.21
24.91
19.81
40.11
43.85
41.94
37.91
69.24
43.84
59.22
69.48
47.86
23.8
29.4
2.9
63.06
MC%
1.12
0.79
0.27
0.35
1.09
0.7
0.53
1.02
0.8
2.06
0.29
1.48
0.16
1.88
0.01
0.47
0.78
0.13
0.28
pH
10.57
10.52
11.02
9.60
9.93
10.04
10.96
10.82
10.73
10.66
10.86
10.47
10.06
10.35
10.05
10.27
10.45
10.20
10.69
EC
mS cm"1
33.00
23.63
32.70
29.48
30.90
26.13
33.20
20.97
22.30
33.20
29.41
29.03
18.40
22.00
31.30
27.07
27.27
23.26
30.20
F-71
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 72 of 478
Table B-2: Major elemental composition of salt cake (EPA Method 6010C)
Sample ID
2452-B-SC
2468-B-SC
2478-B-SC
2454-B-SC
2433-C-SC
2435-C-SC
2532-D-SC
2536-D-SC
2538-D-SC
2540-D-SC
2437-E-SC
2439-E-SC
2502-F-SC
2504-F-SC
2506-F-SC
2508-F-SC
2510-F-SC
2046-H-SC
2544-H-SC
2555-H-SC
2559-H-SC
2568-H-SC
2512-J-SC
2515-J-SC
2517-J-SC
2519-J-SC
2482-L-SC
2484-L-SC
2486-L-SC
2488-L-SC
2490-L-SC
2601-M-SC
2605-M-SC
2609-M-SC
2613-M-SC
2492-N-SC
2494-N-SC
2496-N-SC
Al
8.46
10.62
13.82
11.00
11.68
12.99
9.46
11.57
9.19
10.56
12.09
11.79
16.04
12.94
9.24
12.74
14.25
21.22
17.45
16.00
15.72
12.71
17.35
15.08
10.20
13.56
11.56
11.83
16.22
13.05
13.80
21.81
21.37
41.77
31.77
6.70
6.85
8.57
Fe
0.34
0.36
0.29
0.45
0.37
0.40
0.54
0.53
0.37
0.46
0.36
0.32
1.37
0.42
0.15
0.21
0.32
0.37
0.32
0.29
0.49
0.37
2.40
1.04
1.10
0.98
0.21
0.26
0.70
0.45
0.70
0.44
0.20
0.47
0.68
1.15
1.24
0.99
Ca
€
1.15
1.72
1.04
1.16
2.07
1.67
0.56
0.47
0.52
0.64
1.98
2.15
0.56
0.79
0.37
0.72
1.41
1.08
1.13
1.17
1.29
1.00
0.91
1.15
1.00
1.26
0.32
0.50
1.13
0.69
2.40
1.01
0.40
0.84
1.18
0.51
0.51
0.43
K
/o
5.77
4.65
4.43
7.56
4.30
3.77
12.51
10.27
12.79
8.51
5.39
6.17
3.00
4.06
7.36
4.72
5.12
5.41
6.90
5.75
6.26
6.51
7.00
6.14
5.70
6.91
3.84
2.90
4.81
4.99
3.97
7.73
2.74
7.19
9.02
2.66
4.04
3.14
Mg
1.67
1.69
1.18
1.58
2.34
2.50
3.72
1.70
2.07
1.84
3.54
2.97
1.08
2.66
2.80
1.31
3.01
0.70
0.86
0.56
0.71
0.48
2.04
2.78
1.66
2.11
4.03
4.10
1.71
2.45
2.23
3.98
0.83
4.03
3.40
0.11
0.05
0.27
Na
10.02
10
9.
7.
10
11
11
9.
11
.53
36
28
.73
.45
.94
20
.73
12.07
10
10
11
11
16
12
12
7.
9.
8.
8.
7.
9.
9.
8.
9.
12
10
9.
.52
.88
.30
.49
.54
.29
.34
90
68
70
46
53
56
36
62
00
.60
.15
20
12.32
11
11
5.
6.
7.
10
10
11
.61
.70
58
20
31
.85
.40
.64
S
<163
<163
<163
915
163
465
300
210
377
458
366
411
<163
<163
<163
<163
<163
566
163
<163
<163
<163
<163
<163
<163
541
<163
<163
908
475
1415
808
222
549
547
<163
<163
<163
Zn
mg
349
376
230
367
902
1445
650
493
618
536
709
547
618
499
458
556
380
834
772
648
582
700
2451
2655
2215
2434
196
114
534
364
1054
561
509
457
645
473
478
462
Cu
kg1
217
126
88
174
1719
2028
532
417
374
511
554
377
251
153
397
183
263
557
415
381
433
370
4925
6214
3871
3859
85
94
415
273
1334
557
224
841
717
58
35
59
Mn
2766
2857
2075
1955
1034
1046
766
1136
589
1191
1322
1763
2994
2067
160
1653
2033
1427
1052
632
970
564
1400
1294
726
1012
529
1137
2263
906
1225
2497
1428
5344
2656
135
126
174
F-72
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 73 of 478
2498-N-SC 9.25 0.47 0.51 3.18 0.84 12.05 <163 479 249 342
*The MRL of total Sulfur by ICP is 163 mg Kg4.
F-73
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 74 of 478
Table B-3: Trace metal content of salt cake (EPA Method 6010C)
Sample ID
2452-B-SC
2468-B-SC
2478-B-SC
2454-B-SC
2433-C-SC
2435-C-SC
2532-D-SC
2536-D-SC
2538-D-SC
2540-D-SC
2437-E-SC
2439-E-SC
2502-F-SC
2504-F-SC
2506-F-SC
2508-F-SC
2510-F-SC
2046-H-SC
2544-H-SC
2555-H-SC
2559-H-SC
2568-H-SC
2512-J-SC
2515-J-SC
2517-J-SC
2519-J-SC
2482-L-SC
2484-L-SC
2486-L-SC
2488-L-SC
2490-L-SC
2601-M-SC
2605-M-SC
2609-M-SC
2613-M-SC
2492-N-SC
2494-N-SC
2496-N-SC
2498-N-SC
As
mg kg -1
7.0
16.6
12.8
29.9
20.9
23.6
7.4
12.9
5.7
10.1
8.6
8.6
17.7
7.9
2.8
7.0
8.4
18.5
6.9
7.6
10.6
26.8
15.2
11.7
13.0
13.1
16.7
7.5
14.8
9.6
10.8
16.3
22.6
38.3
40.8
3.0
4.5
6.8
10.4
Cd
52.9
70.9
95.1
69.1
303.9
388.9
86.2
111.7
249.9
463.9
343.5
195.4
83.4
95.3
37.8
59.9
82.4
524.6
890.8
696.7
363.0
1051.5
581.7
1048.2
588.7
502.1
92.1
74.0
533.6
79.7
526.9
342.6
318.4
849.9
817.8
64.4
26.6
19.7
217.7
Cr
mg kg -1
139.4
120.0
128.4
110.6
215.9
264.1
298.6
273.2
355.2
285.2
167.8
179.7
838.6
285.4
263.3
135.3
180.8
783.0
584.2
489.7
600.9
438.2
461.1
478.5
356.6
439.0
128.7
206.4
402.3
320.1
424.9
253.9
76.9
304.1
658.7
225.6
437.7
139.2
401.3
Pb
mg kg -1
12.8
11.0
6.9
10.0
36.4
42.1
98.8
30.0
16.1
17.8
27.1
25.5
6.9
6.8
4.9
7.4
8.0
90.6
103.7
42.6
51.9
50.9
101.4
314.1
48.0
172.7
5.5
4.7
21.2
19.2
78.4
46.4
19.2
48.4
78.1
6.0
4.6
6.0
11.3
Se
mg kg -1
18.4
4.5
30.2
14.4
2.6
4.0
3.2
13.1
4.5
4.4
5.4
5.5
20.0
9.7
3.3
7.4
22.1
7.5
8.5
8.3
8.9
6.1
10.3
8.6
4.3
9.2
7.8
11.2
16.1
10.2
9.9
14.4
12.3
25.6
24.6
2.4
1.3
2.4
3.2
F-74
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 75 of 478
16
24 32
Al Content
40
48
Figure B-l: Total Al distribution in salt cake samples
|QVP
0 0.5
1 1.5
Ca Content
Figure B-2: Total Ca distribution in salt cake samples
Table B-4: Total calcium content (%) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
1.3±0.3
1.9±0.28
0.55±0.07
2.1±0.12
0.77±0.39
l.liO.ll
1.1±0.16
1.0±0.83
0.86±0.34
0.49±0.04
1.8
4.4
0.66
3.1
1.3
1.3
1.3
2.1
1.4
0.55
1.0±1.7
1.7±2.8
0.47±0.64
1.9±2.1
0.37±1.4
1.0±1.3
0.91±1.3
0.32±2.4
0.40±1.2
0.43±0.51
F-75
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 76 of 478
Facility
Mean
UCL95
Range
All Facilities 1.0±0.53
1.2
0.32±2.4
18%
8%
15%
-0.15
13%
V 8% 8%
5%
f
^
-Q
I
-0.05
Mg Content
Figure B-3: Total Mg content distribution in salt cake samples
Table B-5: Total magnesium content (%) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
1.5±0.24
2.4±0.11
2.3±0.94
3.3±0.4
2.2±0.9
0.66±0.15
2.2±0.46
2.9±1.1
3.1±1.5
0.32±0.36
2.0±1.2
1.9
3.4
3.8
6.9
3.3
0.85
2.9
4.3
5.5
0.89
2.4
1.2-1.7
2.3-2.5
1.7-3.7
3.0-3.5
1.1-3.0
0.48-0.86
1.7-2.8
1.7-4.1
0.83-4.0
0.05-0.84
0.05-4.1
F-76
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 77 of 478
p -s-j 0% 0% 0% °
1 1.5 2 2.5
0.5
Fe Content
Figure B-4: Total Fe distribution in salt cake samples
Table B-6: Total iron content (%) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
0.36±0.07
0.39±0.02
0.48±0.08
0.34±0.03
0.49±0.5
0.37±0.08
1.9±0.7
0.46±0.2
0.45±0.2
0.96±0.3
0.58±0.4
0.47
0.58
0.60
0.59
1.1
0.46
2.5
0.75
0.76
1.5
0.72
0.29-0.45
0.37-0.4
0.37-0.54
0.32-0.36
0.15-1.4
0.29-0.49
0.98-2.4
0.21-0.7
0.20-0.68
0.47-1.2
0.15-2.4
6 8
K Content
12
14
Figure B-5: Total potassium content overall distribution
F-77
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 78 of 478
Table B-7: Total K content (%) in salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
All Facilities
5.6±1.4
4.0±0.37
11±2.0
5.8±0.55
4.9±1.6
6.1±0.59
6.4±0.63
4.1±0.84
6.7±2.7
3.3±0.57
5.9±2.4
7.9
7.4
14
11
6.9
6.9
7.4
5.1
11
4.2
6.6
4.4-7.6
3.8-4.3
8.5-13
5.4-6.2
3.0-7.4
5.4-6.9
5.7-7.0
2.9-5.0
2.7-9.0
2.7-4.0
2.7-13
8 10 12 14 16
Na Content
18
Figure B-6: Total sodium distribution in salt cake samples
Table B-8: Total Na content (%) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
9.3±1.4
11±0.51
11±1.4
11±0.25
13±2.2
8.5±0.83
9.1±0.41
11±1.5
7.7±2.8
11±0.75
10±2.1
11
16
13
13
15
9.5
9.8
13
12
12
11
7.3-11
11-12
9.2-12
10-11
11-17
7.5-9.7
8.6-9.6
9.2-13
5.6-12
10-12
5.6-17
F-78
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 79 of 478
20 30
As Content
40
50
Figure B-7: Total arsenic distribution in salt cake samples
Table B-9: Total As content (nig kg"1) in salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
All Facilities
17±9.7
22±1.9
9.0±3.2
8.6±0
8.8±5.5
14±8.5
13±1.4
12±3.8
30±12
6.2±3.2
14±8.8
32
39
14
8.6
16
25
16
17
48
11
17
7-30
21-24
5.7-13
8.0-9.0
2.8-18
6.9-27
12-15
7.5-17
16-41
3.0-10
2.8-41
-0.40
-0.30 .
-0.20
-0.10
0 200 400 600 800 1000 1200
Cd Content
F-79
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 80 of 478
Figure B-8: Total cadmium distribution in salt cake samples
Table B-10: Total Cd content (|ag kg1) in salt cake by facility
Facility
Mean
UCL9s Range
B
C
D
E
F
H
J
L
M
N
All Facilities
72±17
350±60
230±170
270±100
72±23
700±280
680±250
260±250
580±290
82±93
330±300
100
890
500
1,200
100
1,100
1,000
570
1,000
230
430
53±95
300±390
86±460
190±340
38±95
360±1,000
500±1,000
74±530
320±850
20±230
20± 1,000
-0.20
-0.15.&
-0.100-
-0.05
0 150 300 450 600 750 900
Cr Content
Figure B-9: Total chromium distribution in salt cake samples
Table B-ll: Total Cr content (mg kg"1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
130±12
240±34
300±36
170±8.4
340±280
580±130
430±54
300±130
320±240
300±140
330±190
140
550
360
250
690
740
520
450
710
530
390
110-140
220-260
270-360
170-180
140-840
440-780
360-480
130-430
76.9-660
140-440
77-840
F-80
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 81 of 478
2000 3000 4000
Total Cu content
3%
m
5000
3%
6000 7000
Figure B-10: Total copper distribution in salt cake samples
Table B-12: Total Cu content (mg kg-1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All facilities
150±60
1,900±230
460±75
470±120
250±94
430±75
4,700±1,100
440±520
590±270
100±100
880
240
3800
580
1600
370
520
6500
1100
1000
260
1300
88-220
1700-2,000
370-530
380-550
150-400
370-560
3,900-6,200
86-1,300
220-840
35-250
35-6,200
F-81
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 82 of 478
33%
21%
13%
\
8%
13%
10%
0 1000 2000 30
^^^ 3%
0% 0% 0% 0% | |
DO 4000 5000 6000
-0.35
-0.30
-0.25
-0.20l
.Q
e
-0.15°-
-0.10
-0.05
Mn Content
Figure B-ll: Total manganese distribution in salt cake samples
Table B-13: Total Mn content (mg kg-1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
2,400±460
1,000±8.3
920±290
1,500±310
1,800±1,000
930±350
1,100±300
1,200±650
3,000±1,700
190±100
1,400± 1,000
3,600
1,100
1,400
4,300
3,100
1,400
1,600
2,000
5,600
350
1,700
1,900-2,900
1,000-1,100
590-1,200
1,300-1,800
160-3,000
560-1,400
720-1,400
530-2,300
1,400-5,300
130-340
130-5,300
51%
-0.50
23%
10%
S% I 5%
10% 0% 0% 0% 0%
3%
-t-
s
S
B
o.
-0.25
50 100 150 200
Total Pb content
250
300
350
Figure B-12: Total lead distribution in salt cake samples
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 83 of 478
Table B-14: Total Pb content (mg kg"1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
10±2.5
39±4.0
41±39
26±1.1
6.8±1.2
68±27
160±120
26±30
48±24
7.0±3.0
43±58
14
76
100
36
8.2
100
340
63
86
11
62
6.9-13
36-42
16-99
25-27
4.9-8.0
42-100
48-310
4.7-78
19-78
4.6-11
4.6-310
10 15 20
Se Content
35
Figure B-13: Total selenium content distribution in salt cake samples
Table B-15: Total Se content (mg kg"1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
17±11
3.3±0.99
6.3±4.6
5.5±0.1
13±8.2
7.9±1.1
8.1±2.6
11±3.1
19±6.9
2.3±0.8
9.9±7.1
33
12
14
6.1
23
9.2
12
15
30
3.6
12
4.5-30
2.6-4.0
3.2-13
5.4-5.5
3.3-22
6.1-8.9
4.3-10
7.8-16
12-25
1.3-3.2
1.3-30
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 84 of 478
500
1000 1500 2000
Zn Content
2500
Figure B-14: Total zinc content distribution in salt cake samples
Table B-16: Total Zn content (mg kg"1) in salt cake by facility
Facility
Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
330±68
1,200±380
570±72
630±120
500±91
710±99
2,400±180
450±370
540±80
470±7.9
440
4,600
690
1,700
610
830
2,700
910
670
480
230-370
900-1,400
490-650
550-710
380-620
580-830
2,200-2,700
110-1100
460-640
460-480
All Facilities 750±620
950
110-2,600
0.00%
0.50% 1.00% 1.50%
Leachability of Al
2.50%
Figure B-15: Distribution of leachability of aluminum in salt cake samples
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 85 of 478
Table B-17: Correlation Coefficients between Metals in Salt Cakes
Metal
Pearson product moment Spearman rank order
Correlation _ , Correlation _ ,
„,.. . , P value „,.. . , P value
coefficient coefficient
As
Cd
Cr
Al Cu
Mn
Pb
Se
Zn
Cd
A Ml1
As
Pb
Se
Cr
r, Cu
Cd
Pb
Zn
Cr Pb
Zn
n Pb
Cu
Zn
Mn Se
0.72 0.000001 0.53 0.001
0.55 0.001 0.63 0.0001
0.32 0.05
0.40 0.01
0.082 0.6 0.44 0.005
0.70 0.000001 0.55 0.0003
0.23 0.2
0.53 0.0005
0.61 0.0001 0.67 0.00001
0.039 0.8
0.32 0.05
0.45 0.004 0.48 0.002
0.56 0.0002 0.44 0.005
0.10 0.5 0.39 0.02
0.46 0.003 0.40 0.01
0.51 0.001 0.60 0.00005
0.51 0.0009 0.74 0.000001
0.65 0.000001 0.82 0.000001
0.52 0.000001 0.69 0.000001
0.41 0.009 0.57 0.0002
0.32 0.05 0.60 0.000001
0.80 0.000001 0.85 0.000001
0.97 0.000001 0.78 0.000001
0.74 0.000001 0.74 0.000001
200
100 -
80
60 •
_ 40
°3> 30
LeachableAlfn
» e»0 g
4 •
3
2
9
|
e
._*
*-/**
«*/c
/
/
^^
*/
"""ft "
9.5 10 10.5 11 11.5 12
P
F-85
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 86 of 478
Figure B-16: Correlation between teachable Al and pH in leachate of salt cake
31%
1%
11%
% 3% 3%
3% 3%
rfqo%o% o% o% i
-0.60
-0.50
-0.40 £.
!Q
-0.30 |
D.
-0.20
-0.10
0.0% 10.0% 20.0% 30.0% 40.0% 50.0% 60.0% 70.0%
Leachability of Ca
Figure B-17: Distribution of leachability of calcium in salt cake samples
Table B-18: Leachable Ca (mg I/1) in salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
All Facilities
55±77
44±37
3.5±1.3
300±66
71±95
12±4.4
220±130
17±22
54±53
0.82±0.36
65-100
180
380
5.5
900
190
17
430
45
180
1.4
100
0.89-170
17-70
1.8-5.0
260-350
12-230
7.3-19
66-390
1.1-55
3.9-110
0.33-1.2
0.33-390
Table B-19: Leachable Mg (|j.g I/1) in salt cake by facility
Facility
Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
<10
210±130
70±80
<10
10±10
<10
660±880
20±10
20±10
70±120
10
1,400
190
10
20
10
2,100
30
50
260
<10
110-300
10-160
<10
10-30
<10
10-2,000
10-40
10-30
10-250
All Facilities 110±320 210
10-2,000
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 87 of 478
79%
11%
5%
10% 0% 0% 0% 0%
3%
-0.80
-0.70
-0.60
-0.50 =
-0.40 |
-0.30
-0.20
-0.10
0.00% 0.03% 0.06% 0.09% 0.12%
Leachability of Mg
0.15%
Figure B-18: Distribution of teachability of Mg in salt cake samples
Table B-20: Leachable K (mg I/1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
2,700±500
1,900±100
4,800±900
2,600±300
2,100±700
2,500±200
2,600±400
1,700±300
2,500±1,000
1,400±200
2,500±1,000
3,600
2,900
6,200
5,700
3,000
2,800
3,200
2,100
5,200
1,700
2,800
2,300-3,500
1,900-2,000
3,600-5,600
2,400-2,800
1,300-3,200
2,300-2,800
2,200-3,000
1,300-2,100
1,300-3,200
1,100-1,700
1,100-5,600
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 88 of 478
-0.20
-0.15
-0.10
-0.05
70.0% 75.0% 80.0% 85.0% 90.0% 95.0% 100.0%
Leachability of K
Figure B-19: Distribution of teachability of K in salt cake samples
Table B-21: Leachable Na (mg I/1) in salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
3,000±300
3,300±100
2,800±200
2,800±30
3,200±200
2,400±100
2,500±70
2,700±200
2,000±500
2,800±300
2,700±400
3,500
4,200
3,100
3,000
3,400
2,500
2,600
2,900
3,200
3,300
2,900
2,500-3,200
3,200-3,300
2,600-3,000
2,700-2,800
3,100-3,500
2,300-2,500
2,400-2,600
2,400-2,900
1,700-2,600
2,500-3,100
1,700-3,500
5%
r
40.0%
/\W6
21%
J
B1%
H
I
i
•
5%
48.0% 56.0%
5%
«•
IB 3%
| 0% 0% 0% 1 |
64.0%
1 ' 1 ' 1
-0.25
-0.20
S-
-0.151
-0.10°"
-0.05
72.0% 80.0% 88.0%
Leachability of Na
Figure B-20: Distribution of leachability of Na in salt cake samples
F-S
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 89 of 478
0.4 0.8
Leachability of As
1.2
Figure B-21: Distribution of teachability of As in salt cake samples
Table B-22: Leachable arsenic (|j.g I/1) in salt cake by facility
Facility
Mean
UCLgs
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
2.3±0.9
<1.8
<1.8
2.7±0.15
<1.8
<1.8
2.7±1.0
<1.8
<1.8
<1.8
2.0±
3.7
1.8
1.8
4.1
1.8
1.9
4.3
1.8
1.8
1.8
2.2
<1.
<
<
8-3.6
2.6-2.8
<
<1.
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 90 of 478
1
1
0
24%
o.c
5%
j 0% • — • 0% 0% 0% 0% • 1
)2 0.04 0.06 0.08 0.1
Leachability of Cr
-1.20
-1.00
-0.80 ^
!Q
-0.60 -|
CL
-0.40
-0.20
Figure B-22: Distribution of leachability of Cr in salt cake samples
Table B-24: Leachable Cu (iig L"1) in salt cake by facility
Facility Mean
1
|
B
C
D
E
F
H
J
L
M
N
All
%
9
ls%
10±6.2
460±640
140±13
150±10
200±24
8.9±3.9
290±490
79±110
4.2±3.1
8.7±3.8
Facilities 73±220
^^H
3% 1 • 3%
UCL95
20
6,200
34
11
50
14
1,000
220
12
15
150
3%
Range
7.1-19
7.1-91
7.1-34
7.1-22
20-61
7.1-16
16-1,000
7.1-270
<7.1
7.1-14
7.1-1,000
3%
1 J^^^^^^^S 0% 0% 0% ^^* 0% ^^H
0.0%
0.2%
0.4% 0.6% 0.8%
Leachability of Cu
1.0%
-0.80
-0.60^
1
-0.40QI
-0.20
1 1 '
1.2%
F-90
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 91 of 478
Figure B-23: Distribution of teachability of Cu in salt cake samples
Table B-25: Leachable Mn (|o.g L"1) in salt cake by facility
Facility
Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
20±0.97
20±0.42
21±3.0
18±0.14
19±1.5
19±1.4
18±1.0
19±0.88
19±1.2
19±1.2
19±1.6
22
24
26
19
21
21
19
20
23
21
20
20-22
20-21
18-25
18-18
17-21
18-21
16-19
18-20
18-21
18-20
16-25
-1.40
-1.20
-1.00
-0.80
-0.60
-0.40
-0.20
0.0%
0.2%
Leachability of Mn
0.4%
Figure B-24: Distribution of leachability of Mn in salt cake samples
Table B-26: Leachable Pb (iig I/1) in salt cake by facility
Facility
Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
4.0±1.8
<2.5
6.6±4.0
<2.5
<2.5
<2.5
2.6±0.1
2.6±0.3
4.4±3.3
<2.5
3.3±2.0
6.8
2.5
13
2.5
2.5
2.5
2.7
3.0
13
2.5
3.9
2.5-5.6
<2.5
2.5-10
<2.5
<2.5
<2.5
2.5-2.7
2.5-3.2
2.5-8.3
<2.5
2.5-10
F-91
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 92 of 478
29%
1 1
n
• 3%\
8°/
0 0.25
\. 11% 11%
, 8% 8% r~| •
I 5%
3% I |3% 3%
'0% 0% j j
0.5 0.75 1 1.25 1.5 1.75
-0.35
-0.30
-0.25^
-0.20|
8.
-0.15^
-0.10
-0.05
teachability of Lead
Figure B-25: Distribution of teachability of Pb in salt cake samples
Table B-27: Leachable Se Qg L'1) in salt cake by facility
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Mean
120±64
<10
<10
<10
27±28
10±1.0
15±8.9
10±0.36
<10
<10
24±40
UCL9s
223
10
10
10
61
12
29
11
10
10
38
Range
37-190
<10
<10
<10
10-75
10-12
10-29
10-11
<10
<10
10-190
F-92
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 93 of 478
24
Leachability of Se
Figure B-26: Distribution of teachability of Se in salt cake samples
Table B-28: Leachable Zinc (n,g L"1) in salt cake by facility
Facility
Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
<5.2
57±74
<5.2
<5.2
37±63
47±27
61±9.4
26±18
5.9±1.1
5.9±1.0
26±43
5.2
72
5.2
5.2
110
81
210
48
8.9
7.2
40
<5.2
5.2-110
<5.2
<5.2
5.2-150
11-68
5.2-200
5.2-47
5.2-7.3
5.2-7.1
5.2-200
16%
0%
0%
0%
3%
-3.00
-2.50
-2.00 i"
ID
-1.502
-1.00
-0.50
0.0% 0.2% 0.4% 0.6%
Leachability of Zn
0.8%
1.0%
Figure B-27: Distribution of leachability of Zn in salt cake samples
F-93
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 94 of 478
Table B-29: TCLP results for Al (mg I/1) by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
150±280
1.1±0.21
5.7±3.7
4.5±1.9
120±230
180±30
180±140
18±20
1.5±0.72
110±19
90±140
590
3.0
12
22
400
220
410
42
3.3
140
140
0.95-570
0.95-1.2
2.5-11
3.1-5.9
4.0-520
150-240
1.6-330
2.1-51
0.95-2.3
99-140
0.95-570
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 95 of 478
Table B-30: TCLP results for Ag (mg I/1) by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
All Facilities
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 96 of 478
Facility Mean UCLgs Range
^N 0.01±0.01 0.02 0.004-0.02
All Facilities 0.01±0.01 0.01 0.004-0.04
Table B-34: TCLP results for Cr (mg I/1) by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
0.06±0.07
0.02±0.002
0.03±0.01
0.02
0.07±0.1
0.1±0.03
0.19±0.19
0.02±0.002
0.03±0.01
0.06±0.02
0.06±0.08
0.17
0.04
0.04
0.02
0.19
0.13
0.49
0.02
0.04
0.09
0.09
0.02-0.2
0.02-0.02
0.02-0.04
0.02-0.02
0.02-0.24
0.07-0.13
0.02-0.46
0.02-0.03
0.02-0.03
0.04-0.08
0.02-0.46
Table B-35: TCLP results for Pb (mg I/1) by facility
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Mean
0.06±0.09
0.02±0.004
0.02±0.02
0.014±0.0001
0.04±0.05
0.63±0.40
2.0±1.5
0.03±0.01
0.02±0.01
0.02±0.02
0.32±0.77
UCL95
0.20
0.06
0.05
0.02
0.09
1.1
4.4
0.04
0.04
0.05
0.57
Range
0.01-0.19
0.01-0.02
0.01-0.05
0.01-0.01
0.01-0.12
0.17-1.2
0.01-3.3
0.01-0.04
0.01-0.03
0.01-0.05
0.01-3.3
Table B-36: TCLP results for Se (mg I/1) by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
0.06±0.09
0.02±0.004
0.02±0.02
O.OliO.OOOl
0.04±0.05
0.63±0.40
2.0±1.5
0.03±0.01
0.02±0.01
0.02±0.02
0.32±0.77
0.76
0.10
0.08
0.18
0.18
0.03
0.06
0.06
0.07
0.06
0.10
0.02-0.72
0.04-0.05
0.03-0.08
0.02-0.04
0.02-0.18
0.02-0.03
0.02-0.06
0.03-0.07
0.02-0.05
0.02-0.06
0.02-0.72
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 97 of 478
Table B-37: Aluminum mineral phase (%) in salt cake
sample ID
2452-B
2454-B
2468-B
2478-B
2433-C
2435-C
2532-D
2536-D
2538-D
2540-D
2437-E
243 9-E
2502-F
2504-F
2506-F
2508-F
2510-F
2046-H
2544-H
2555-H
2559-H
2568-H
2512-J
2515-J
2517-J
2519-J
2482-L
2484-L
2486-L
2488-L
2490-L
260 1-M
2505-M
2609-M
2613-M
2492-N
53
2
2
2
2
2
2
2
2
2
2
3
3
5
4
4
2
3
2
1
2
2
2
4
4
1
1
3
4
2
1
3
6
3
18
14
1
Z
4
6
4
4
5
6
0
6
2
2
5
4
5
4
1
3
5
10
7
10
9
6
3
4
4
4
5
6
9
6
5
2
4
2
3
3
VJ
0
z
J
V)
00
10
14
10
14
11
10
12
8
10
12
9
10
9
13
15
17
11
10
11
6
9
9
12
10
16
12
13
7
7
14
9
9
14
11
8
13
A12.81 Os.S6 No.44
6
10
6
10
6
6
7
5
7
8
6
6
6
8
8
11
7
6
7
5
6
6
9
6
12
8
8
4
5
10
6
6
10
8
5
9
A12.78 Os.6sNo.35
5
8
5
7
5
5
6
4
5
7
5
5
5
6
6
8
6
5
5
5
5
5
7
5
9
6
6
3
4
7
5
5
9
6
4
7
Z
53
I
6.9
10.4
6.9
8.3
8.1
8.9
3.5
8.4
5.1
5.7
7.8
6.9
7.8
7.8
5.1
8.0
8.3
12.9
10.2
12.2
11.8
8.8
6.9
6.9
9.1
7.6
8.8
8.0
11.2
10.3
7.8
4.8
8.5
5.5
5.4
7.0
6
5]
5
3
7
6
9
11
3
4
2
3
9
5
10
6
2
4
5
10
8
14
9
12
7
9
5
6
3
6
8
3
8
1
6
ND
2
23
O
10
14
8
12
9
9
10
7
10
11
7
8
8
11
13
15
9
9
9
6
7
8
12
9
15
11
11
5
7
13
8
10
14
10
7
12
q
13
"o
36.4
49.2
35.7
48.6
39.9
41.0
37.8
27.9
34.2
40.9
35.5
33.7
37.9
43.8
44.2
54.9
37.6
40.0
39.7
35.8
35.5
39.9
47.1
39.0
56.8
43.0
40.8
24.7
31.1
47.0
35.9
31.5
53.1
34.8
25.9
63.9
53
cS
z
3
3
3
2
2
2
2
3
3
4
3
3
5
4
4
2
3
3
2
3
3
3
3
4
2
2
4
6
3
2
4
4
3
6
6
1
•*
o
13
7
11
10
5
7
5
10
8
10
9
10
9
10
6
7
12
9
7
9
10
8
6
8
5
5
18
23
10
9
8
5
5
13
8
2
F-97
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 98 of 478
2494-N
2496-N
2498-N
1
1
2
3
3
6
9
16
9
7
13
6
6
10
4
6.0
8.4
8.7
33
12
12
9
17
8
64.0
68.2
39.0
1
1
3
3
3
12
F-98
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 99 of 478
Table B-38: Non-Aluminum mineral phase (%) in salt cake
Sample ID
2452-B
2454-B
2468-B
2478-B
2433-C
2435-C
2532-D
2536-D
2538-D
2540-D
2437-E
243 9-E
2502-F
2504-F
2506-F
2508-F
2510-F
2046-H
2544-H
2555-H
2559-H
2568-H
2512-J
2515-J
2517-J
2519-J
2482-L
2484-L
2486-L
2488-L
2490-L
260 1-M
2505-M
2609-M
2613-M
2492-N
2494-N
2496-N
2498-N
KC1
9
8
8
6
8
7
18
17
19
11
10
11
5
5
9
5
8
9
10
10
11
10
10
12
7
11
4
5
10
5
7
14
5
11
13
4
5
3
5
NaCl
21
12
20
17
23
21
18
15
19
16
18
20
20
20
30
19
22
16
18
12
16
15
15
21
13
15
20
16
19
19
18
20
17
11
11
17
12
14
20
CaF2
6
7
5
3
7
5
11
11
12
8
8
7
6
ND
ND
2
ND
5
6
9
8
6
5
ND
3
12
2
4
7
3
5
ND
3
ND
8
2
3
1
4
Total salt
36
27
33
26
38
33
47
43
50
35
36
38
31
25
39
26
30
30
34
31
35
31
30
33
23
38
26
25
36
27
30
34
25
22
32
23
20
18
29
MgO
2
2
2
1
1
1
1
1
1
1
2
1
1
3
2
1
4
ND
ND
ND
ND
1
1
1
1
1
4
4
1
2
2
2
1
2
2
ND
ND
1
1
CaSO4
6
ND
6
5
5
5
5
5
ND
5
6
5
6
5
ND
4
6
5
5
8
6
5
5
5
4
4
ND
6
6
5
7
ND
5
ND
6
6
8
5
7
CaCOs
ND
1
ND
ND
1
ND
ND
1
ND
ND
1
1
ND
1
ND
ND
ND
ND
1
2
ND
ND
ND
1
ND
1
ND
ND
1
ND
1
ND
ND
ND
ND
ND
ND
ND
ND
SiCh
1
3
4
ND
2
1
ND
ND
1
1
1
1
1
ND
ND
ND
ND
1
1
ND
ND
4
3
2
2
2
ND
ND
ND
ND
5
16
1
1
1
1
1
1
ND
ND: Not detected
F-99
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 100 of 478
10 15
KCI Abundance
Figure B-28: Distribution of the KCI abundance in salt cake samples
Table B-39: KCI abundance of salt cake by facility (%)
Facility
Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
7.8±1.3
7.5±0.7
16±3.6
11±0.8
6.4±1.9
10±0.7
10±2.2
6.2±2.4
11±4.0
4.3±1.0
8.8±3.8
9.8
14
22
16.9
8.8
11
13
9.2
17
5.8
10
6-9
7-8
11-19
10-11
5-9
9-11
7-12
4-10
5-14
3-5
3-19
Table B-40: NaCl abundance of salt cake by facility (%)
Facility
Mean
UCL9s Range
B
C
D
E
F
H
J
L
M
N
All Facilities
18±4.0
22±1.4
17±1.8
19±1.4
22±4.5
15±2.2
16±3.5
18±1.5
15±4.5
16±3.5
18±3.8
24
35
20
32
28
18
22
20
22
21
19
12-21
21-23
15-19
18-20
19-30
12-18
13-21
16-20
11-20
12-20
11-30
F-100
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 101 of 478
10
15 20 25
NaCI Abundance
30
35
Figure B-29: Distribution of the NaCI abundance in salt cake samples
5 10
CaF2 Abundance
15
Figure B-30: Distribution of the fluorite abundance in salt cake samples
Table B-41: Fluorite abundance of salt cake by facility (%)
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
M
N
5.3±1.7
6±1.4
11±1.7
7.5±0.7
1.6±2.6
6.8±1.6
5±5.1
4.2±1.9
2.8±3.8
2.5±1.3
8.0
19
13
14
4.8
8.8
13
6.6
8.8
4.6
3-7
5-7
8-12
7-8
ND-6
5-9
ND-12
2-7
ND-8
1-4
F-101
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 102 of 478
Facility
Mean
UCL95
Range
All Facilities 5.0±3.5
6.1
ND-12
* ND: Undetectable
Table B-42: Total salt content (%) of salt cake by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
31±4.8
31±3.5
44±6.5
37±1.4
30±5.5
32±2.2
31±6.3
29±4.4
28±5.7
23±4.8
38
67
54
50
37
35
41
34
37
30
26-36
33-38
35-50
36-38
25-39
30-35
23-38
25-36
22-34
18-29
All Facilities 31±6.9
34
18-50
10
I
0.35
0.30
0.25
0.20 =
0.10
0.05
30 40
Total salt
50
60
Figure B-31: Distribution of the total salt flux in salt cake samples
Table B-43: Metallic Al abundance (%) of salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
2±0
2±0
2±0
3±0
3.6±1.1
1.8±0.4
2.5±1.7
2.6±1.1
10±6.9
1.3±0.5
2
2
2
o
J
5.0
2.4
5.3
4.0
21
2.0
2-2
2-2
2-2
o o
J-J
2-5
1-2
1-4
1-4
3-18
1-2
F-102
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 103 of 478
Facility
Mean
UCL95 Range
All Facilities 3.1±3.3
4.2
1-18
H3*» - -
\
II
0
1
i • i • i • i
-1.00
-0.90
-0.80
-0.70
-060^
5
-0.50 1
-0.40 °~
-0.30
-0.20
-0.10
4 8 12 16 20
Metallic Al Abundance
Figure B-32: Distribution of the metallic aluminum in salt cake samples
15 -
5 -
pp
*
• «
• • • *
024
«
I •
6
(
•
a
•a
-^
10 12 14
b
15 -
5 -
0
•
i
5
• •
•
—
• *
• •<
1
K
'
» •
::
3
•
• ••
15 2
b
i
15 -
5 -
0
Ct
:
ur
5 10 15
Na
-
I
sr
2
•
m
D
25 30
b
Figure B-33: Relations between the abundance of metallic Al and salt in salt cake
Table B-44: Mineral A1N abundance (%) of salt cake by facility
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Mean
4.5±1
5.5±0.7
2.5±2.5
4.5±0.7
3.6±1.7
8.4±1.8
3.8±0.5
6.2±1.6
2.8±1.0
3.8±1.5
4.6±2.3
UCL95
6.1
12
6.5
11
5.7
11
4.5
8.2
4.3
6.1
5.4
Range
4-6
5-6
ND-6
4-5
1-5
6-10
3-4
5-9
2-4
3-6
ND-10
* ND: Undetectable
F-103
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 104 of 478
Table B-45: Ak.gsO3.4sNo.ss abundance (%) of salt cake by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
12±2.3
11±0.7
11±1.9
9.5±0.7
13±3.2
9±1.9
13±2.5
10±3.3
11±2.6
12±3.4
11±2.7
16
17
14
16
17
11
17
14
15
17
12
10-14
10-11
8-12
9-10
9-17
6-11
10-16
7-17
8-14
9-16
6-17
Table B-46: Ab.ysOs.esNo.ss abundance (%) of salt cake by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
6.3±1.5
5±0
5.5±1.3
5±0
6.2±1.1
5±0
6.8±1.7
5±1.6
6±2.2
6.8±2.5
5.8±1.5
8.6
5
7.6
5
7.6
5
9.5
7.0
9.4
10.7
6.3
5-8
5-5
4-7
5-5
5-8
5-5
5-9
3-7
4-9
4-10
3-10
Table B-47: Ab.8iO3.s6No.44 abundance (%) of salt cake by facility
Facility Mean UCLgs Range
B
C
D
E
F
H
J
L
M
N
All Facilities
8±2.3
6±0
6.8±1.3
6±0
8±1.9
6±0.7
8.8±2.5
6.6±2.4
7.3±2.2
8.8±3.1
7.3±2.1
12
6
8.8
6
10
6.9
13
9.6
11
14
8.0
6-10
6-6
5-8
6-6
6-11
5-7
6-12
4-10
5-10
6-13
4-13
F-104
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 105 of 478
0.30
0.25
0.201
0.1s|
0.10
0.05
AI2.85O3.45N0.55 Abundance
-0.30 =
0.20
-0.10
AI2.81O3.S6N0.44 Abundance
0.309
I
0.20
0.10
AI2.81O3.65N0.35 Abundance
Figure B-34: Overall distribution of the three aluminum nitride oxides in salt cake
Table B-48: Total A1N abundance (%) of salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
All Facilities
8.1±1.7
8.5±0.6
5.7±2.0
7.4±0.6
7.4±1.3
11±1.7
7.6±1.0
9.2±1.5
6.1±1.7
7.5±1.3
8.0±2.1
10.8
13.6
8.9
13
9.0
13
9.3
11
8.7
9.5
8.6
6.9-10
8.1-8.9
3.5-8.4
6.9-7.8
5.1-8.3
8.8-13
6.9-9.1
7.8-11
4.8-8.5
6-8.7
3.5-13
6
AIM Abundance
12
Figure B-35: Distribution of the aluminum nitride in salt cake samples
F-105
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 106 of 478
Table B-49: Alumina abundance (%) of salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
All Facilities
5.3-1.7
10-1.4
3-0.8
7-2.8
5.4-3.0
11-2.4
6.8-1.7
5.6-2.5
2.3-2.6
20-10
7.5-6.0
8.0
23
4.3
32
9.1
14
9.5
8.7
6.4
36
9.4
3-7
9-11
2-4
5-9
2-10
8-14
5-9
3-8
ND-6
12-33
ND-33
* ND: Undetectable
F
0 5 10 15 20 25 30 35
• •
0 4 a 12
Ca
Figure B-36: Relations between the abundance of A1N and salt in salt cake
-0.25
-0.20
5
-0.15^
£
-0.10
-0.05
10 15 20 25
AI2O3 Abundance
35
Figure B-37: Distribution of the alumina in salt cake samples
F-106
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 107 of 478
Table B-50: Alumina abundance (%) of salt cake by facility
Facility
Mean
UCL95 Range
B
C
D
E
F
H
J
L
M
N
All Facilities
5.3-1.7
10-1.4
3-0.8
7-2.8
5.4-3.0
11-2.4
6.8-1.7
5.6-2.5
2.3-2.6
20-10
7.5-6.0
* ND: Undetectable
Table B-51: Ah.eeyCh abundance
Facility
B
C
D
E
F
H
J
L
M
N
All Facilities
Mean
11±15
9±9
9.5±12
7.5±14
11±15
7.8±9.4
12±16
8.8±13
10±15
11±18
9.9±11
8.0
23
4.3
32
9.1
14
9.5
8.7
6.4
36
9.4
3-7
9-11
2-4
5-9
2-10
8-14
5-9
3-8
ND-6
12-33
ND-33
(%) of salt cake by facility
UCL95
15
9
12
14
15
9.4
16
13
15
18
11
Range
8-14
9-9
7-11
7-8
8-15
6-9
9-15
5-13
7-14
8-17
5-17
F-107
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 108 of 478
10 15
AI2.67O4 Abundance
20
Figure B-38: Distribution of Ah.eyCMn salt cake samples
Table B-52: Total abundance of Aluminum oxides (%) in salt cake by facility
Facility
Mean
UCL9s Range
B
C
D
E
F
H
J
L
M
N
All Facilities
43±7.4
41±0.8
35±5.6
35±1.3
44±7.0
38±2.3
47±7.6
36±8.6
36±12
59±13
41±10
54
47
44
46
52
41
59
47
55
80
45
36-49
40-41
28-41
34-36
38-55
36-40
39-57
25-47
26-53
39-68
25-68
F-108
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 109 of 478
30 40 50 60
Total AI2O3 Abundance
70
Figure B-39: Distribution of total aluminum oxides in salt cake samples
L
,;.tt.??,,..
10 20
0 10 20 30 40 50 60 70
total
Figure B-40: Relations between alumina oxides and metallic Al in salt cake
35 -
30 -
25-
€
10 -
5 -
l~-
_-
sbfr .
0 5 10 15
Na
20
~~|
I
25 30
30 -
25 -
"20-
§15-
10 -
^^^_
• • f *
•••£•• .
n
0 5 10 15 20
K
35 -
30 -
25 -
820-
* 15 -
5 -
0 -
(
1
• • • •
* • * *
1 • * * |
2468
Ca
I
H
10 12 14
Figure B-41: Relations between salt and alumina in salt cake
F-109
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 110 of 478
70 -
60 -
50 -
°40 -
|30-
20 -
10 -
0 -
Q
1,
-
Si • «•_«
•• • L
5 10 15
Na
20
L
i
25 30
70 -
60 -
50 -
°40 -
|30-
20 -
10 -
0 -
Q
r-TKl
1 •
.:•/::,
. •" .' • *
]
I
5 10 15 20
K
70 -
60 -
50 -
°40 -
|30-
20 -
10 -
0 -
n
•
•
i •
0 2
•
2
t
i
ii
—
•
;:
•
4 6 i
Ca
— i
|
•:
L
i
10 12 14
Figure B-42: Relations between salt and total aluminum oxides in salt cake
246
K2NaAIF6 Abundance
Figure B-43: Distribution of the elpasolite abundance in salt cake samples
Table B-53: Elpasolite abundance (%) of salt cake by facility
Facility
Mean
UCL95
Range
B
C
D
E
F
H
J
L
2.8±0.5
2±0
3±0.8
3±0
3.6±1.1
2.8±0.4
2.8±1.0
3.8±1.5
3.5
2
4.3
o
J
5.0
3.4
4.3
5.6
2-3
2-2
2-4
3-3
2-5
2-3
2-4
2-6
F-110
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 111 of 478
Facility
M
N
All Facilities
Mean
4.8±1.5
1.5±1
3.1±1.2
UCL95
7.1
3.1
3.5
Range
3-6
1-3
1-6
Table B-54: Spinel abundance (%) of salt cake by facility
Facility
Mean
UCL95
Range
B 10±2.5 14.2 7-13
C 6±1.4 18.7 5-7
D 8.3±2.4 12.0 5-10
E 9.5±0.7 15.9 9-10
F 8.8±2.4 11.8 6-12
H 8.6±1.1 10.0 7-10
J 6±1.4 8.3 5-8
L 14±6.6 21.8 8-23
M 7.8±3.8 13.8 5-13
N 5±4.7 12.4 2-12
All Facilities 8.6±3.9 9.9 2-23
, ,
1 .J--— --B^ 1 i
| *T -^"1 1
i
0 5 10 15 20 25
MgAI2O4 Abundance
-0.35
-0.30
-0.25
t
-0.20 ji
-0.15°-
-0.10
-0.05
Figure B-44: Distribution of the spinel abundance in salt cake samples
£10-
Figure B-45: Relations between metallic Al, elpasolite and spinel in salt cake
F-lll
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 112 of 478
F-112
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 113 of 478
Secondary Aluminum Processing Waste: Salt Cake Characterization and Reactivity
9. APPENDIX C: XRD Data
FACILITY B 115
1.1:2452-B-SC 115
1.2: 2454-B-SC 121
1.3:2468-B-SC 128
1.4: 2478-B-SC 134
FACILITY C 140
2.L2433-C-SC 140
2.2: 2435-C-SC 147
FACILITY D 153
3.L2532-D-SC 153
3.2: 2536-D-SC 159
3.3:2538-D-SC 166
3.4: 2540-D-SC 172
FACILITY E 180
4.L2437-E-SC 180
4.2: 2439-E-SC 187
FACILITY F 194
5.L2502-F-SC 194
5.2: 2504-F-SC 201
5.3:2506-F-SC 207
5.4: 2508-F-SC 213
5.5: 2510-F-SC 219
FACILITY H 226
6.L2046-H-SC 226
6.2: 2544-H-SC 232
6.3:2555-H-SC 239
6.4: 2559-H-SC 246
6.5: 2568-H-SC 252
FACILITY! 259
7.L2512-J-SC 259
7.2: 2515-J-SC 265
7.3:2517-J-SC 272
7.4:2519-J-SC 279
FACILITY L 286
8.L2482-L-SC 286
8.2: 2484-L-SC 292
8.3:2486-L-SC 298
8.4: 2488-L-SC 305
8.5: 2490-L-SC 311
FACILITY M 318
9.L2601-M-SC 318
9.2: 2605-M-SC 324
9.3:2609-M-SC 330
9.4: 2613-M-SC 336
FACILITY N 342
10.L2492-N-SC 342
10.2: 2494-N-SC 349
F-113
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 114 of 478
10.3:2496-N-SC 356
10.4: 2498-N-SC 362
F-114
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 115 of 478
FACILITY B
1.1: 2452-B-SC
1.1.1 Measurement Conditions
Dataset Name
File name
no cover_002.sd
Sample Identification 2452-B-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2452-B-SC, no cover_002
C:\DocumentsandSettings\xhuang\Desktop\SAP-xrd\9-24-10\2452-B-sc,
Measurement Date / Time
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
9/13/2010 9:26:00 AM
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
1.1.2: Main Graphics, Analyze View of 2452-B
F-115
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 116 of 478
V VV
2452-B-sc, no cover_002
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Periclase, syn (00-043-1022)
50 60 70 80
Position [°2Theta] (Copper (Cu))
Magnesium Aluminum Oxide 12.6 % |
Aluminum Oxide Nitride 9.7 %
Aluminum Oxide 9.7 %
Sylvite, syn 8.7 %
Fluorite, syn 5.8 %
Aluminum Oxide Nitride 5.8 %
\
Sodium Chloride 20.4 %|
Aluminum Nitririp 39%
Aluminum 1 .9 % | %
AIIJI-T IU ..... JI-.
Aluminum Oxide 4.9 %
1.1.3: Pattern List of 2452-B
F-116
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 117 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
54
49
51
55
32
17
19
19
22
34
17
25
21
19
14
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
5
9
21
13
4
10
6
5
2
2
6
3
6
10
1
20
10
9
14
8
12
12
12
5
7
6
16
39
12
18
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
1.1.4: Peak List of 2452-B
F-117
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 118 of 478
Pos. [°2Th.]
16.3120
18.9666
21.9210
23.0550
23.8802
24.4954
25.5660
26.6574
27.3460
28.3548
29.7838
31.2722
31.6806
33.2189
34.3249
35.1383
35.6056
36.0140
36.8589
37.7908
38.4973
40.4885
41.8142
42.9022
43.3116
44.8249
45.4042
45.5424
Height [cts]
97.75
3551.60
135.51
182.34
163.97
315.41
2302.18
727.14
6982.14
28990.78
676.66
7215.31
71247.75
3129.19
661.14
4146.22
1514.56
2690.27
16383.13
3649.17
1993.74
14140.14
420.56
2295.15
3822.06
10652.60
38085.40
21621.73
FWHM
[°2Th.]
0.2362
0.0492
0.2362
0.3149
0.2362
0.1574
0.1181
0.1378
0.0984
0.1673
0.2362
0.1181
0.1673
0.2362
0.3149
0.0984
0.1181
0.1771
0.1574
0.1968
0.1771
0.1279
0.2362
0.0689
0.0492
0.1574
0.1680
0.0960
d-spacing [A]
5.43416
4.67914
4.05473
3.85781
3.72633
3.63412
3.48431
3.34409
3.26143
3.14765
2.99980
2.86034
2.82439
2.69703
2.61262
2.55398
2.52153
2.49387
2.43862
2.38060
2.33852
2.22799
2.16037
2.10807
2.08909
2.02202
1.99590
1.99511
Rel. Int. [%]
0.14
4.98
0.19
0.26
0.23
0.44
3.23
1.02
9.80
40.69
0.95
10.13
100.00
4.39
0.93
5.82
2.13
3.78
22.99
5.12
2.80
19.85
0.59
3.22
5.36
14.95
53.45
30.35
Matched by
01-074-1132;
00-022-1235;
01-086-2270
00-022-1235
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-086-2270
F-118
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 119 of 478
Pos. [°2Th.]
46.9563
50.1396
50.2852
52.5329
53.8203
55.6047
56.4188
56.6081
57.4488
57.6144
58.6033
59.3284
59.5020
61.2636
62.2711
65.2078
65.3831
66.1455
66.3426
68.1612
68.3279
71.3612
Height [cts]
919.84
3520.41
3415.84
1476.12
1211.78
1188.15
10160.12
4642.62
3054.41
1930.18
1917.57
6090.31
4972.67
392.20
785.63
9262.63
8345.74
5669.36
6344.42
1637.29
1028.13
533.31
FWHM
[°2Th.]
0.1440
0.0720
0.0960
0.1200
0.1440
0.2400
0.1440
0.0960
0.1080
0.1200
0.1920
0.0840
0.0960
0.1920
0.1440
0.1440
0.1440
0.1200
0.1080
0.0960
0.1200
0.3360
d-spacing [A]
1.93348
1.81794
1.81301
1.74061
1.70197
1.65150
1.62959
1.62863
1.60280
1.60255
1.57394
1.55642
1.55230
1.51182
1.48975
1.42958
1.42617
1.41157
1.40785
1.37465
1.37170
1.32067
Rel. Int. [%]
1.29
4.94
4.79
2.07
1.70
1.67
14.26
6.52
4.29
2.71
2.69
8.55
6.98
0.55
1.10
13.00
11.71
7.96
8.90
2.30
1.44
0.75
Matched by
00-004-0864;
01-086-2270
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
00-004-0587;
00-022-1235;
01-085-0930
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862;
01-074-1132
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
00-022-1235;
01-085-0930
01-075-1620;
01-080-2173;
01-086-2270
F-119
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 120 of 478
Pos. [°2Th.]
72.9777
73.6559
73.8772
75.2014
75.4178
76.8160
77.3334
78.5381
80.6147
82.5810
83.8916
84.1223
85.7082
87.5936
88.9296
90.3108
91.1115
94.0246
94.4253
95.1920
99.2739
101.0309
101.3775
107.6507
108.4939
109.9051
Height [cts]
579.10
1876.08
1603.46
8497.75
4816.08
657.98
1163.95
431.31
188.64
781.08
5373.96
2972.52
222.27
432.41
152.29
399.76
561.85
1456.77
1733.85
797.04
646.35
1804.01
1421.00
599.29
506.49
2986.73
FWHM
[°2Th.]
0.1200
0.1920
0.1440
0.1560
0.1080
0.1200
0.1680
0.6720
0.1440
0.1920
0.1440
0.1560
0.2400
0.2400
0.1920
0.1200
0.1920
0.1200
0.1440
0.1680
0.2400
0.1680
0.0960
0.1680
0.2400
0.0600
d-spacing [A]
1.29535
1.28509
1.28497
1.26247
1.26251
1.23990
1.23289
1.21697
1.19078
1.16734
1.15241
1.15269
1.13257
1.11298
1.09969
1.08642
1.07895
1.05304
1.05223
1.04319
1.01095
0.99806
0.99806
0.95426
0.94918
0.94091
Rel. Int. [%]
0.81
2.63
2.25
11.93
6.76
0.92
1.63
0.61
0.26
1.10
7.54
4.17
0.31
0.61
0.21
0.56
0.79
2.04
2.43
1.12
0.91
2.53
1.99
0.84
0.71
4.19
Matched by
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
01-077-2064
01-075-1862
01-074-1132
01-074-1132;
00-043-1022;
01-086-2270
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-085-0930
01-074-1132;
01-075-1620;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862
00-022-1235
00-043-1022;
00-004-0864
00-004-0587
00-043-1022
F-120
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 121 of 478
1.2: 2454-B-SC
1. 2.1: Measurement Conditions
Dataset Name
File name
no cover.sd
Sample Identification 2454-B-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2454-B-SC, no cover
C:\DocumentsandSettings\xhuang\Desktop\SAP-xrd\9-24-10\2454-B-sc,
Measurement Date / Time
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
9/6/2010 1:22:00 PM
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
F-121
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 122 of 478
1.2.2: Main Graphics, Analyze View of 2454-B
'V V V V
V V V
2454-B-sc, no cover
Aluminum Oxide (01-075-1865)
Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
Periclase, syn (00-043-1022)
Silicon Oxide (01-081-0069)
20 30 40
50 60 70
Position [°2Theta] (Copper (Cu))
Sodium Chloride 12 %
Aluminum Oxide Nitride 10 %
Sylvite, syn 3 % |
Aluminum Oxide Nitride 8 %
Aluminum Oxide Nitride 14 %\
Aluminum Oxide 14 % |
Magnesium Aluminum Oxide 7 %
F-122
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 123 of 478
1.2.3: Pattern List of 2454-B
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-080-
1385
01-086-
2339
01-085-
0930
Score
31
34
50
42
40
17
15
15
36
31
18
19
18
11
19
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Aluminum
Oxide
Calcite
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
A12.667 O4
Ca ( C O3 )
Si O2
3
8
12
7
6
14
10
8
2
2
7
3
14
1
3
Matched
Lines
12
8
9
12
9
11
8
8
5
6
5
12
11
18
19
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-123
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 124 of 478
1.2.4: Peak List of 2454-B
Pos. [°2Th.]
10.2784
10.4044
13.4431
14.2128
18.7440
18.9789
21.0267
23.0794
23.4920
25.7348
26.9236
27.5135
28.4217
29.5465
30.1848
30.5222
31.8431
32.8052
33.3599
33.8444
35.2872
36.1919
37.0224
37.8560
38.0985
38.3765
38.6382
38.7162
39.5989
40.5539
41.3321
43.0894
43.4685
43.9575
Height [cts]
390.75
185.69
339.24
176.64
787.33
1203.08
708.16
3062.55
3644.38
1359.51
10617.56
3776.52
14884.73
1847.40
4804.33
2648.80
27845.93
2430.35
4986.85
2233.43
2610.30
3577.15
6185.25
4278.89
4302.12
5174.65
5509.81
4859.92
1495.30
8990.61
1316.22
3007.54
2529.91
1452.44
FWHM
[°2Th.]
0.0394
0.2362
0.0984
0.1968
0.1378
0.1574
0.1082
0.1181
0.1476
0.1378
0.1574
0.1771
0.1870
0.1574
0.1673
0.1181
0.1870
0.1574
0.0886
0.1574
0.0689
0.1574
0.1771
0.1378
0.1181
0.0590
0.0720
0.0787
0.1968
0.2165
0.1771
0.1968
0.1378
0.1574
d-spacing [A]
8.60653
8.50257
6.58669
6.23170
4.73422
4.67613
4.22513
3.85378
3.78703
3.46184
3.31163
3.24195
3.14039
3.02335
2.96085
2.92889
2.81035
2.73009
2.68595
2.64860
2.54355
2.48202
2.42822
2.37665
2.36208
2.34561
2.32839
2.32581
2.27597
2.22455
2.18445
2.09935
2.08191
2.05988
ReLIntM
1.40
0.67
1.22
0.63
2.83
4.32
2.54
11.00
13.09
4.88
38.13
13.56
53.45
6.63
17.25
9.51
100.00
8.73
17.91
8.02
9.37
12.85
22.21
15.37
15.45
18.58
19.79
17.45
5.37
32.29
4.73
10.80
9.09
5.22
Matched by
01-074-1132;
00-022-1235
01-085-0930
01-086-2339
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1620
00-043-1022
01-075-1862;
01-075-1620
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327
01-074-1132
01-085-0930
00-004-0587
01-086-2339
01-075-1862
F-124
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 125 of 478
Pos. [°2Th.]
44.8756
44.9739
45.5400
46.9979
47.3992
47.8035
50.0933
52.6538
53.5981
53.9522
55.2167
55.7756
56.5532
56.7183
57.6014
58.4981
59.4039
60.4525
61.6659
62.4354
62.6176
Height [cts]
5583.01
6267.31
17662.02
1732.91
1747.98
1502.86
2787.10
901.62
551.35
886.86
809.27
864.83
4448.87
2722.19
1580.00
1312.51
2759.75
1320.53
935.47
2598.96
1972.68
FWHM
[°2Th.]
0.1200
0.0787
0.1476
0.0984
0.1181
0.1968
0.1968
0.1181
0.2165
0.0984
0.2362
0.1968
0.1560
0.0960
0.1680
0.3840
0.0960
0.3360
0.2880
0.1080
0.0960
d-spacing [A]
2.01818
2.01566
1.99192
1.93347
1.91803
1.90275
1.82101
1.73833
1.70991
1.69953
1.66356
1.64821
1.62604
1.62572
1.59891
1.57652
1.55463
1.53014
1.50292
1.48623
1.48602
Rel. Int. [%]
20.05
22.51
63.43
6.22
6.28
5.40
10.01
3.24
1.98
3.18
2.91
3.11
15.98
9.78
5.67
4.71
9.91
4.74
3.36
9.33
7.08
Matched by
01-074-1132;
01-085-1327
01-074-1132
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
00-004-0864;
01-086-2339
01-086-2339
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862
01-077-2064
00-022-1235;
01-085-0930
01-074-1132;
00-004-0864
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385;
01-086-2339
01-075-1862;
01-086-2339
00-004-0587
01-074-1132;
01-075-1620
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
00-043-1022
65.3023
3305.02
0.1920
1.42774
11.87
F-125
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 126 of 478
Pos. [°2Th.]
66.2862
68.2234
68.4538
69.8436
71.5024
73.6157
75.3213
75.5442
77.3920
78.3673
81.1542
82.6366
83.9921
84.2693
87.4461
90.3922
91.2532
94.0614
Height [cts]
5041.53
1106.38
995.48
689.60
746.29
1026.75
3569.44
2055.08
399.60
613.64
90.45
262.04
2248.31
1128.10
185.23
126.99
108.72
724.19
FWHM
[°2Th.]
0.1440
0.1320
0.1440
0.2400
0.2400
0.5280
0.1440
0.0840
0.5760
0.1920
0.7680
0.4800
0.1440
0.1440
0.4800
0.1920
0.5760
0.1920
d-spacing [A]
1.40892
1.37355
1.36949
1.34560
1.31840
1.28569
1.26075
1.26071
1.23211
1.21920
1.18422
1.16669
1.15128
1.15105
1.11448
1.08566
1.07765
1.05273
Rel. Int. [%]
18.11
3.97
3.57
2.48
2.68
3.69
12.82
7.38
1.44
2.20
0.32
0.94
8.07
4.05
0.67
0.46
0.39
2.60
Matched by
01-074-1132;
01-086-2339
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-085-0930
01-074-1132;
01-075-1620;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
00-004-0587;
00-022-1235;
01-086-2339;
01-085-0930
01-077-2064
01-074-1132
01-074-1132;
01-085-1327;
01-086-2339
01-075-1620;
01-086-2339;
01-085-0930
01-074-1132;
01-085-1327
01-077-2064;
01-086-2339;
01-085-0930
00-004-0587;
01-080-2171;
00-004-0864;
01-080-1385;
01-085-0930
00-022-1235
00-043-1022;
00-004-0864
95.2223
442.30
0.2880
1.04294
1.59
F-126
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 127 of 478
Pos. [°2Th.]
99.3158
101.1450
101.4681
107.7364
Height [cts]
225.82
1057.89
565.82
329.63
FWHM
[°2Th.]
0.6720
0.1680
0.1440
0.1440
d-spacing [A]
1.01064
0.99724
0.99741
0.95374
Rel. Int. [%]
0.81
3.80
2.03
1.18
Matched by
F-127
-------
1.3: 2468-B-SC
1.3.1: Measurement Conditions
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 128 of 478
Dataset Name
File name
SC_003.sd
Sample Identification 2468-B-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 7/29/2010 3:37:00 PM
2468-B-SC_003
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2468-B-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
10.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
30 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
1.3.2: Main Graphics, Analyze View of 2468-B
F-128
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 129 of 478
V V V
2468-B-SC_003
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-0;
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
_ Aluminum (01-085-1327)
Periclase, syn (00-043-1022)
50 60 70 80
Position [°2Theta] (Copper (Cu))
Magnesium Aluminum Oxide 10.9 % |
Aluminum Oxide Nitride 9.9 %
Aluminum Oxide Nitride 5.9 %
Sodium Chloride 19.13%
Ah imirM im "l Of. I
Periclase, syn 2 % |
mw t- 70 |
h ~ Elpasolite, syn 3 % |
Aluminum Nitride 4 %~h
Anhydrite 5.9 %|
F-129
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 130 of 478
1.3.3: Pattern List of 2468-B
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0335
Score
50
49
49
51
32
11
14
17
37
31
19
28
20
15
15
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz low
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
7
8
20
11
4
10
6
5
2
2
5
3
6
8
4
Matched
Lines
20
10
9
14
7
12
12
12
5
7
5
16
36
12
16
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
1.3.4: Peak List of 2468-B
F-130
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 131 of 478
Pos. [°2Th.]
10.0403
10.3123
19.0004
23.1552
24.5151
25.5733
26.6567
27.3508
28.3610
31.2664
31.6901
33.2422
35.1549
36.0909
36.8766
37.7567
38.5389
40.5365
42.8944
43.3314
44.8351
45.4287
45.5795
46.9633
50.2171
Height [cts]
10.52
3.46
1029.62
42.46
60.76
1071.03
199.97
2516.35
8719.33
2050.53
27339.12
1165.07
1985.50
983.72
5135.61
1474.16
1403.17
5717.19
1085.38
2139.68
4219.70
18574.98
10356.30
326.66
1888.06
FWHM
[°2Th.]
0.0492
0.3149
0.0689
0.3149
0.2362
0.0787
0.1574
0.1082
0.1673
0.1181
0.1673
0.2165
0.1279
0.1378
0.0886
0.1082
0.0984
0.1574
0.2165
0.1082
0.1574
0.1560
0.0960
0.2880
0.1320
d-spacing [A]
8.81012
8.57829
4.67090
3.84133
3.63125
3.48334
3.34417
3.26086
3.14697
2.86085
2.82357
2.69519
2.55282
2.48873
2.43749
2.38267
2.33609
2.22547
2.10844
2.08818
2.02158
1.99488
1.99358
1.93321
1.81531
Rel. Int. [%]
0.04
0.01
3.77
0.16
0.22
3.92
0.73
9.20
31.89
7.50
100.00
4.26
7.26
3.60
18.78
5.39
5.13
20.91
3.97
7.83
15.43
67.94
37.88
1.19
6.91
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-085-0335
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
01-086-2270
00-004-0587
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-080-2171;
01-086-2270
00-004-0864;
01-086-2270
00-004-0587;
01-080-2173;
00-022-1235;
01-085-0335
F-131
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 132 of 478
Pos. [°2Th.]
52.5787
53.8436
55.7076
56.4772
56.6219
57.4625
57.6666
58.6533
59.3408
59.5164
61.3029
62.3138
65.2416
65.4325
66.1994
66.3933
68.2203
68.4160
71.4037
73.0495
73.7501
75.2812
75.4880
76.8860
77.3997
78.2905
Height [cts]
1008.67
642.34
559.72
5828.70
3318.28
1955.35
1403.51
1081.97
2605.25
2553.63
281.52
636.22
4354.30
4408.67
3858.98
4154.84
1451.22
898.64
410.79
464.25
1338.86
6154.45
3432.17
643.57
770.13
511.20
FWHM
[°2Th.]
0.1320
0.1440
0.3360
0.1440
0.0960
0.1200
0.0720
0.1680
0.1440
0.1440
0.3840
0.1680
0.2400
0.1440
0.0720
0.0720
0.1560
0.0720
0.1920
0.0960
0.1680
0.1560
0.1320
0.1200
0.2880
0.1920
d-spacing [A]
1.73920
1.70129
1.64870
1.62804
1.62826
1.60245
1.60123
1.57272
1.55613
1.55196
1.51094
1.48884
1.42892
1.42876
1.41055
1.41040
1.37361
1.37356
1.31998
1.29425
1.28368
1.26132
1.26151
1.23895
1.23200
1.22020
Rel. Int. [%]
3.69
2.35
2.05
21.32
12.14
7.15
5.13
3.96
9.53
9.34
1.03
2.33
15.93
16.13
14.12
15.20
5.31
3.29
1.50
1.70
4.90
22.51
12.55
2.35
2.82
1.87
Matched by
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064;
01-080-2171
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862;
01-074-1132
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
00-004-0587;
01-077-2064;
01-075-1620
01-075-1862;
00-022-1235;
01-085-0335
01-075-1620;
01-080-2173;
01-086-2270
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
01-077-2064
01-075-1862;
01-086-2270
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
F-132
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 133 of 478
Pos. [°2Th.]
80.6919
82.6461
83.9430
84.2356
86.4409
87.6940
89.0359
90.3862
91.2057
94.1166
94.6062
95.2340
99.3576
101.1117
101.4810
107.7887
108.6402
109.8065
Height [cts]
156.67
461.30
3797.68
2159.89
126.42
294.07
123.12
301.15
364.76
780.22
1123.76
659.80
357.01
1385.90
1020.68
434.32
404.41
980.25
FWHM
[°2Th.]
0.1440
0.2880
0.1920
0.1320
0.5760
0.1920
0.1680
0.1200
0.1920
0.2400
0.1920
0.2160
0.2880
0.1080
0.1680
0.1200
0.2400
0.0600
d-spacing [A]
1.18983
1.16658
1.15183
1.15143
1.12484
1.11197
1.09865
1.08571
1.07808
1.05225
1.04810
1.04284
1.01032
0.99748
0.99732
0.95342
0.94831
0.94148
Rel. Int. [%]
0.57
1.69
13.89
7.90
0.46
1.08
0.45
1.10
1.33
2.85
4.11
2.41
1.31
5.07
3.73
1.59
1.48
3.59
Matched by
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-085-0335
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-022-1235
00-043-1022;
00-004-0864
00-004-0587
00-004-0587
00-043-1022
F-133
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 134 of 478
1.4: 2478-B-SC
1.4.1: Measurement Conditions
Dataset Name
File name
SC_002.sd
Sample Identification 2478-B-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 7/3 0/2010 8:25:00 AM
2478-B-SC_002
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2478-B-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
10.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
30 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
F-134
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 135 of 478
1.4.2: Main Graphics, Analyze View of 2478-B
W f
2478-B-SC_002
| Aluminum Oxide (01-075-1865
j Potassium Chloride (01-075-0:
j Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
I Periclase, syn (00-043-1022)
96)
fllnlfl
50 60 70 80
Position [°2Theta] (Copper (Cu))
Aluminum Oxide 12.1 % |
Magnesium Aluminum Oxide 10.1 %
Aluminum Oxide Nitride 14.1 %
Sodium Chloride 17.2 % |
[AJ Aluminum 2 %
Aluminum Oxide Nitride 10.1 % ]
| Aluminum Oxide Nitride 7.1 %"| | Aluij Aluminum Nitride 4 % |
| Sylvite, syn 6.1 % |
F-135
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 136 of 478
1.4.3: Pattern List of 2478-B
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
42
43
57
54
42
11
13
14
32
30
29
19
17
12
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
6
6
17
10
4
14
10
7
2
1
3
2
5
12
Matched
Lines
18
10
9
15
11
12
11
12
5
8
7
16
36
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-136
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 137 of 478
1.4.4: Peak List of 2478-B
Pos. [°2Th.]
10.0576
10.3307
19.0022
23.0859
24.4631
25.5476
26.6517
27.3192
27.3765
28.3336
31.2777
31.6818
33.2245
35.1243
36.0356
36.8612
37.7721
37.8979
38.4850
40.4934
42.9084
43.3102
44.7724
44.8594
45.4150
45.5569
47.0521
Height [cts]
15.45
14.95
1000.33
46.04
67.98
1184.48
224.65
2288.32
2188.93
9200.78
2346.68
25630.47
1503.35
2452.23
1200.77
5264.69
1849.22
1720.76
1460.94
5517.34
1056.78
2630.53
4014.61
4428.71
17245.00
9699.77
686.54
FWHM
[°2Th.]
0.0492
0.4723
0.0886
0.2362
0.2362
0.0590
0.1378
0.0720
0.0492
0.1476
0.0984
0.1870
0.1968
0.0984
0.1378
0.0984
0.1440
0.0984
0.1082
0.2165
0.1771
0.1279
0.0840
0.0787
0.1440
0.1080
0.2160
d-spacing [A]
8.79502
8.56306
4.67047
3.85271
3.63885
3.48679
3.34480
3.26186
3.25786
3.14995
2.85985
2.82429
2.69659
2.55497
2.49242
2.43847
2.37977
2.37412
2.33924
2.22774
2.10778
2.08915
2.02259
2.02054
1.99545
1.99451
1.92977
ReLIntM
0.06
0.06
3.90
0.18
0.27
4.62
0.88
8.93
8.54
35.90
9.16
100.00
5.87
9.57
4.68
20.54
7.21
6.71
5.70
21.53
4.12
10.26
15.66
17.28
67.28
37.84
2.68
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064;
01-080-2171;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-085-1327
01-077-2064;
01-086-2270
00-004-0864
F-137
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 138 of 478
Pos. [°2Th.]
49.8053
50.1790
52.5176
53.8433
55.7136
56.4235
56.6069
57.4679
57.6502
58.6449
59.3613
61.2953
62.3003
65.2546
66.1827
66.3965
68.2085
68.3884
69.7442
71.4048
72.6353
73.0361
73.7098
73.9494
75.2526
75.4612
76.8496
77.4320
Height [cts]
709.19
1979.75
1300.32
766.04
798.80
5318.79
3140.71
2656.67
1706.46
1242.70
3234.40
525.96
614.05
5043.88
3839.14
4203.73
1879.13
1167.39
268.80
656.44
389.42
537.91
1471.58
1079.30
5767.23
3373.95
863.49
845.76
FWHM
[°2Th.]
0.1920
0.1680
0.0960
0.1200
0.2880
0.1320
0.1200
0.1200
0.1200
0.1440
0.2160
0.0720
0.1200
0.0840
0.0720
0.0840
0.1080
0.0720
0.2880
0.2880
0.1920
0.1200
0.1200
0.1440
0.1440
0.0720
0.1680
0.6240
d-spacing [A]
1.82935
1.81660
1.74108
1.70130
1.64853
1.62946
1.62866
1.60231
1.60164
1.57292
1.55564
1.51111
1.48913
1.42867
1.41087
1.41034
1.37382
1.37405
1.34727
1.31996
1.30061
1.29445
1.28428
1.28071
1.26173
1.26189
1.23945
1.23157
Rel. Int. [%]
2.77
7.72
5.07
2.99
3.12
20.75
12.25
10.37
6.66
4.85
12.62
2.05
2.40
19.68
14.98
16.40
7.33
4.55
1.05
2.56
1.52
2.10
5.74
4.21
22.50
13.16
3.37
3.30
Matched by
01-075-1620;
01-080-2171
00-004-0587;
01-080-2173;
00-022-1235
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620
01-075-1620;
01-080-2173;
01-086-2270
01-075-1620
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
01-074-1132
01-077-2064
01-075-1862
01-074-1132;
01-086-2270
F-138
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 139 of 478
Pos. [°2Th.]
78.2499
80.6851
82.6306
83.9763
84.2204
85.7975
86.4419
87.6478
88.9804
90.3980
90.6708
91.1740
94.1149
94.5452
94.8575
95.2504
98.3305
99.3856
101.1231
101.4726
104.8618
107.7264
108.1340
108.6025
109.7705
Height [cts]
607.37
264.00
540.28
3855.69
2151.68
175.76
183.07
366.95
253.60
333.79
292.57
461.77
875.08
1196.74
883.34
844.09
113.66
428.34
1480.69
1129.09
110.31
641.49
608.11
724.27
999.16
FWHM
[°2Th.]
0.1920
0.1920
0.2880
0.1440
0.1320
0.2880
0.3840
0.1200
0.1680
0.1680
0.1440
0.1920
0.2400
0.1200
0.1440
0.1920
0.2880
0.2880
0.1920
0.1440
0.5760
0.1440
0.1440
0.2400
0.0480
d-spacing [A]
1.22073
1.18992
1.16676
1.15146
1.15160
1.13162
1.12483
1.11243
1.09919
1.08560
1.08305
1.07838
1.05227
1.05122
1.04598
1.04270
1.01811
1.01011
0.99740
0.99738
0.97184
0.95380
0.95133
0.94853
0.94168
Rel. Int. [%]
2.37
1.03
2.11
15.04
8.40
0.69
0.71
1.43
0.99
1.30
1.14
1.80
3.41
4.67
3.45
3.29
0.44
1.67
5.78
4.41
0.43
2.50
2.37
2.83
3.90
Matched by
01-074-1132;
01-085-1327
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-022-1235
00-043-1022;
00-004-0864
00-004-0587
00-043-1022
F-139
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 140 of 478
FACILITY C
2.1: 2433-C-SC
2.1.1: Measurement Conditions
Dataset Name
File name
Sample Identification
Comment
Generated by todd in project Ft.
Measurement Date / Time
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
2433-C-SC, no cover
D:\SAP\2433-c-sc, no cover.sd
2433-C-SC, no cover
Exported by X'Pert SW
Devens.
9/7/2010 6:35:00 AM
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
2.1.1: Main Graphics, Analyze View of 2433-C
F-140
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 141 of 478
V V
2433-c-sc, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
• Periclase, syn (00-043-1022)
I
20 30 40 50 60 70 80 90
Position [°2Theta] (Copper (Cu))
100 110
Aluminum Oxide Nitride 10.9 % ]
Aluminum Oxide 8.9 %
Aluminum Oxide 8.9 %
Sylvite, syn 7.9 %
Sodium Chloride 22.3 %|
Fluor Aluminum Nitride 5
Aluminum Qxide Nitride 5.9 % |
—
I Ani Aluminum 2 %
Magnesium Aluminum Oxide 5 % |
F-141
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 142 of 478
2.1.3: Pattern List of 2433-C
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
01-085-
0930
Score
59
39
48
45
39
20
18
20
39
29
24
20
22
18
17
32
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
9
8
23
5
5
11
6
5
2
1
7
2
5
9
1
2
Matched
Lines
20
10
9
13
10
13
12
13
5
6
7
14
37
12
18
22
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-142
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 143 of 478
2.1.4: Peak List of 2433-C
Pos. [°2Th.]
1L0641
18.9670
20.8140
22.0522
23.1096
24.4977
25.5120
26.5836
27.3204
28.2767
29.4178
30.1487
31.6455
33.1579
33.7175
35.0699
35.9821
36.8228
37.7185
37.8212
38.4372
39.4031
40.3643
41.7470
42.8567
43.2972
Height [cts]
18L83
1342.79
855.31
309.92
388.96
399.19
3939.31
4731.94
7548.82
23928.78
1835.06
1939.02
75016.20
4517.37
1233.90
7041.67
3395.74
6273.39
5185.56
5140.08
4036.61
1275.59
10370.73
831.25
2506.25
7443.45
FWHM
[°2Th.]
0.3936
0.1574
0.1181
0.4723
0.1574
0.1771
0.0984
0.1181
0.1279
0.1968
0.1771
0.1574
0.1771
0.0787
0.2362
0.0886
0.1574
0.1181
0.0840
0.1574
0.0886
0.0984
0.1771
0.3149
0.1574
0.1800
d-spacing [A]
799706
4.67904
4.26783
4.03092
3.84881
3.63378
3.49157
3.35320
3.26442
3.15616
3.03629
2.96432
2.82745
2.70186
2.65829
2.55881
2.49601
2.44093
2.38303
2.37876
2.34204
2.28683
2.23457
2.16370
2.11020
2.08802
Rel. Int. [%]
024
1.79
1.14
0.41
0.52
0.53
5.25
6.31
10.06
31.90
2.45
2.58
100.00
6.02
1.64
9.39
4.53
8.36
6.91
6.85
5.38
1.70
13.82
1.11
3.34
9.92
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-086-2340
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-077-2064;
01-080-2171
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-080-2173
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
01-080-2172;
01-080-2173;
01-080-1385;
01-086-2340;
01-085-0930
00-004-0587;
01-085-0930
01-075-1862
00-043-1022
01-075-1862;
01-086-2270;
01-086-2340
F-143
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 144 of 478
as. [°2Th.]
43.3942
44.7004
45.3509
45.4687
46.9494
47.2601
48.5777
50.0608
50.1814
52.4661
52.6227
53.7838
54.8111
55.6566
56.3906
56.5291
57.3875
57.5805
58.5122
59.2981
59.8563
Height [cts]
5128.43
5009.68
37722.89
27805.09
1985.17
1839.34
610.99
3914.59
3384.93
2901.20
1912.50
1421.99
468.27
1045.30
10042.72
6334.87
5341.81
3682.21
1710.64
3321.62
1548.59
FWHM
[°2Th.]
0.0720
0.1080
0.1680
0.0960
0.0960
0.0960
0.3360
0.0720
0.1440
0.1680
0.0720
0.1680
0.1680
0.2400
0.1080
0.0960
0.1320
0.0480
0.1680
0.2400
0.1920
d-spacing [A]
2.08876
2.02568
1.99812
1.99818
1.93375
1.92176
1.87267
1.82061
1.81652
1.74267
1.74217
1.70304
1.67352
1.65009
1.63034
1.63071
1.60436
1.60342
1.57618
1.55715
1.54395
Rel. Int. [%]
6.84
6.68
50.29
37.07
2.65
2.45
0.81
5.22
4.51
3.87
2.55
1.90
0.62
1.39
13.39
8.44
7.12
4.91
2.28
4.43
2.06
Matched by
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
01-086-2270;
01-086-2340
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-085-0930
01-075-1862
01-077-2064
01-085-0930
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-085-0930
F-144
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 145 of 478
Pos. [°2Th.]
61.2098
62.2137
65.1601
65.3249
66.0913
66.4297
68.1221
68.3018
69.6623
71.3348
72.9440
73.4951
75.1575
75.3628
76.7639
77.0589
78.1945
79.8570
80.5810
Height [cts]
986.67
990.60
3887.30
3634.10
6417.80
5276.45
3304.34
2052.88
372.69
995.09
757.38
1553.32
8043.10
4998.66
1140.09
973.82
844.03
154.35
360.82
FWHM
[°2Th.]
0.1200
0.1440
0.1920
0.1680
0.1440
0.1680
0.1320
0.1200
0.2880
0.2400
0.1440
0.1200
0.1560
0.1320
0.1680
0.2400
0.2160
0.3840
0.1440
d-spacing [A]
1.51302
1.49099
1.43051
1.42730
1.41260
1.40622
1.37535
1.37558
1.34866
1.32109
1.29586
1.28750
1.26309
1.26329
1.24062
1.23660
1.22146
1.20016
1.19119
Rel. Int. [%]
1.32
1.32
5.18
4.84
8.56
7.03
4.40
2.74
0.50
1.33
1.01
2.07
10.72
6.66
1.52
1.30
1.13
0.21
0.48
Matched by
01-075-1862;
01-086-2270;
01-086-2340
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-075-1620;
01-086-2340
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-077-2064;
01-086-2270
01-086-2340;
01-085-0930
01-077-2064
01-075-1862;
01-086-2340
01-075-1862;
01-086-2270
01-085-1327
01-080-2171;
01-080-2172;
01-086-2270;
01-080-1385;
01-075-1862;
01-086-2340
F-145
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 146 of 478
Pos. [°2Th.]
82.4323
83.8759
84.1108
86.2547
87.4406
87.9660
88.8703
90.2620
91.0518
93.9474
94.3057
95.1346
95.4626
98.2217
99.1206
100.9826
101.3586
104.6909
107.6213
108.1660
109.8493
Height [cts]
346.99
4926.52
2868.13
259.32
404.64
257.58
310.22
353.61
538.49
632.05
1077.79
1145.67
495.48
147.61
215.41
2056.43
1176.78
35.03
316.21
160.99
1397.73
FWHM
[°2Th.]
0.3840
0.1320
0.1200
0.2880
0.4320
0.1440
0.1920
0.1920
0.1440
0.1440
0.2400
0.1920
0.1680
0.2880
0.4800
0.0840
0.1920
0.5760
0.1920
0.4800
0.1080
d-spacing [A]
1.16907
1.15258
1.15282
1.12679
1.11454
1.11199
1.10027
1.08689
1.07950
1.05370
1.05064
1.04367
1.04353
1.01894
1.01210
0.99841
0.99819
0.97296
0.95444
0.95114
0.94123
Rel. Int. [%]
0.46
6.57
3.82
0.35
0.54
0.34
0.41
0.47
0.72
0.84
1.44
1.53
0.66
0.20
0.29
2.74
1.57
0.05
0.42
0.21
1.86
Matched by
01-074-1132;
01-085-1327
01-077-2064;
01-086-2340;
01-085-0930
01-075-1862;
01-086-2340
00-004-0587;
01-080-2171;
01-080-2172;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-043-1022
00-004-0587;
00-004-0864
00-043-1022
F-146
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 147 of 478
2.2: 2435-C-SC
2.2.1: Measurement Conditions
Dataset Name
File name
Sample Identification
Comment
2435-C-SC-no cover
D:\SAP\2435-C-SC-no cover.sd
2435-C-SC-no cover
Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 7/10/2010 5:54:00 AM
Raw Data Origin PHILIPS-binary (scan) (.SD)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 0.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPert MPD
Diffractometer Number 1
Goniometer Radius [mm] 200.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning Yes
F-147
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 148 of 478
2.2.2: Main Graphics, Analyze View of 2435-C
|2435-C-SC-no cover
•Aluminum Oxide (01-075-1865
|potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
lAluminum Nitride (01-076-056!
Aluminum (01-085-1327)
iQuartz, syn (01-083-2467)
[Periclase, syn (00-043-1022)
96)
TTTT
20 30
50 60 70
Position [°2"meta] (Copper (Cu))
90 100 110
sodium Chloride 21.4 % |
Aluminum Oxide 11.2 %
Aluminum Oxide Nitride 10.2 %
Magnesium Aluminum Oxide 7.1 %
["Aluminum Oxide Nitride 6.1 % |
Ruorite. syn 5.1 % I
TjTj^Jl Anhydrite 5.1 %
2.2.3: Pattern List of 2435-C
F-148
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 149 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
59
42
44
42
38
14
16
19
41
29
14
23
17
17
9
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
11
7
21
7
6
10
6
5
2
1
5
2
5
9
1
20
10
9
13
10
12
12
12
5
6
5
12
36
12
17
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-149
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 150 of 478
2.2.4: Peak List of 2435-C
as. [°2Th.]
"101523
10.7137
18.9908
20.8139
23.0997
24.4843
25.5721
26.5893
27.3429
28.2919
30.1574
31.6610
33.1801
35.1157
35.9872
36.8284
37.7503
38.4910
40.3895
40.4531
41.7896
42.9212
43.2738
44.7209
45.3709
47.2497
Height [cts]
10529
29.86
612.16
114.88
131.34
167.49
1687.94
595.77
3207.29
9209.78
909.86
34880.69
2800.47
3938.07
2009.85
3352.82
3069.79
2470.43
5096.87
6198.69
557.55
1418.03
4015.35
3380.55
23160.42
1340.12
FWHM
[°2Th.]
0.0492
0.9446
0.0886
0.1181
0.2362
0.1968
0.1378
0.1771
0.1378
0.1968
0.1771
0.1968
0.1279
0.1279
0.1968
0.0886
0.2362
0.1968
0.0840
0.1082
0.3149
0.1574
0.1574
0.1082
0.1378
0.0787
d-spacing [A]
8771319
8.25782
4.67324
4.26785
3.85045
3.63574
3.48349
3.35249
3.26179
3.15450
2.96348
2.82609
2.70009
2.55557
2.49567
2.44057
2.38306
2.33889
2.23138
2.22986
2.16159
2.10718
2.09083
2.02648
1.99895
1.92375
Rel. Int. [%]
O30
0.09
1.76
0.33
0.38
0.48
4.84
1.71
9.20
26.40
2.61
100.00
8.03
11.29
5.76
9.61
8.80
7.08
14.61
17.77
1.60
4.07
11.51
9.69
66.40
3.84
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587;
01-085-0930
00-004-0587;
01-085-0930
01-075-1862
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-086-2270
F-150
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 151 of 478
Pos. [°2Th.]
49.7409
50.1076
52.4953
53.8073
55.6462
56.3927
56.5586
57.4383
57.6076
58.5182
59.3019
61.2766
62.2622
65.1796
66.1244
66.4736
68.1494
Height [cts]
1296.75
2555.80
2245.80
1117.94
761.60
7541.18
4492.07
4494.55
2900.02
1263.14
3093.38
772.69
732.36
3358.10
5760.32
3893.54
2771.55
FWHM
[°2Th.]
0.1181
0.1082
0.1378
0.0984
0.1574
0.1320
0.0720
0.1560
0.0840
0.1920
0.1680
0.1680
0.3360
0.3120
0.1320
0.2640
0.1680
d-spacing [A]
1.83309
1.82053
1.74321
1.70376
1.65174
1.63028
1.62993
1.60306
1.60273
1.57603
1.55706
1.51153
1.48995
1.43013
1.41197
1.40540
1.37486
Rel. Int. [%]
3.72
7.33
6.44
3.21
2.18
21.62
12.88
12.89
8.31
3.62
8.87
2.22
2.10
9.63
16.51
11.16
7.95
Matched by
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
68.3403
1723.68
0.1200
1.37489
4.94
F-151
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 152 of 478
Pos. [°2Th.]
69.6883
71.3729
72.5367
72.9402
73.5442
75.1640
75.4254
76.7411
77.2211
78.2042
80.6353
82.5522
83.8380
84.1307
86.2338
87.4526
87.9569
88.8949
90.2658
90.5912
91.1070
94.3196
95.1079
98.2183
99.1956
101.0254
Height [cts]
429.92
1151.18
598.53
767.17
1400.34
7405.85
4115.02
1050.95
896.79
835.51
399.33
452.94
4680.91
2785.04
244.17
315.99
277.14
298.87
344.33
315.47
466.74
1061.20
1077.91
191.12
239.18
2080.65
FWHM
[°2Th.]
0.2880
0.2160
0.2880
0.1680
0.3360
0.1920
0.1440
0.1560
0.3840
0.2400
0.1920
0.3840
0.1440
0.1200
0.2880
0.3360
0.1440
0.1920
0.1440
0.1440
0.1920
0.1920
0.1680
0.1440
0.4800
0.1080
d-spacing [A]
1.34822
1.32048
1.30213
1.29914
1.28676
1.26300
1.26240
1.24093
1.23441
1.22133
1.19052
1.16767
1.15301
1.15260
1.12701
1.11441
1.11208
1.10003
1.08685
1.08379
1.07899
1.05052
1.04389
1.01897
1.01154
0.99810
Rel. Int. [%]
1.23
3.30
1.72
2.20
4.01
21.23
11.80
3.01
2.57
2.40
1.14
1.30
13.42
7.98
0.70
0.91
0.79
0.86
0.99
0.90
1.34
3.04
3.09
0.55
0.69
5.97
Matched by
01-074-1132;
01-075-1620
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-075-1620
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-004-0587;
00-004-0864
F-152
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 153 of 478
Pos. [°2Th.] Height [cts]
101.3506
103.2407
104.6543
107.6227
FACILITY D
3.1: 2532-D-SC
3.1:1: Measurement
1379.02
71.20
63.05
328.91
Conditions
FWHM
[°2Th.]
0.1200
0.5760
0.5760
0.1920
d-spacing [A]
0.99825
0.98263
0.97320
0.95443
Rel. Int. [%] Matched by
3.95
0.20
0.18
0.94
Dataset Name
File name
cover\2532-D-SC, no cover.udf
Sample Identification
Comment
2532-D-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no
2532-D-SC
Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
3.1.2: Main Graphics, Analyze View of 2532-D
F-153
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 154 of 478
2532-D-SC, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072 1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076
_ Aluminum (01-085-1327)
Periclase, syn (00-043-10^2)
50 60 70
Position [°2Theta] (Copper (Cu))
Aluminum Oxide 10 %
Sodium Chloride 18 %H
Aluminum Oxide Nitride 12%
Aluminum Oxide Nitride 7 % | I Aluminum Oxide Nrtride 6 % |
F-154
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 155 of 478
3.1.3: Pattern List of 2532-D
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
27
59
52
43
13
14
15
39
31
24
21
12
15
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
3
18
18
5
12
7
6
2
1
11
2
5
10
Matched
Lines
15
10
9
12
11
11
11
5
7
6
14
30
11
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
F-155
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 156 of 478
3.1.4: Peak List of 2532-D
Pos. [°2Th.]
18.9620
24.4706
25.5090
27.3010
28.3018
31.6318
35.1231
36.7827
38.4670
40.4879
42.8771
43.3329
44.8077
45.3865
45.5086
46.9751
47.9542
50.1295
50.1790
52.5190
53.8148
56.3843
56.5722
Height [cts]
283.00
122.09
88.77
2409.85
24409.16
26462.19
307.84
2074.55
1312.56
17045.68
1056.54
736.89
3414.93
19102.73
12176.62
362.82
145.28
4763.70
5467.11
126.74
694.99
5528.13
3411.56
FWHM
[°2Th.]
0.1378
0.1378
0.1574
0.1082
0.1771
0.1378
0.1181
0.1378
0.0787
0.1181
0.1378
0.1181
0.2755
0.1440
0.0960
0.2400
0.2880
0.0600
0.0960
0.2880
0.1440
0.1680
0.1200
d-spacing [A]
4.68028
3.63776
3.49197
3.26671
3.15342
2.82863
2.55506
2.44349
2.34030
2.22803
2.10925
2.08811
2.02275
1.99664
1.99652
1.93276
1.89555
1.81828
1.81660
1.74104
1.70213
1.63050
1.62957
ReLIntM
1.07
0.46
0.34
9.11
92.24
100.00
1.16
7.84
4.96
64.42
3.99
2.78
12.90
72.19
46.02
1.37
0.55
18.00
20.66
0.48
2.63
20.89
12.89
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171
01-075-1862
01-074-1132;
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235
01-075-1862
01-077-2064
01-077-2064
F-156
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 157 of 478
Pos. [°2Th.]
57.4467
58.6285
58.7671
59.2988
59.5350
62.2337
65.1837
65.3070
66.1492
66.3612
66.5690
68.1812
73.0062
73.6878
73.9073
75.2245
75.4641
77.4327
78.2188
82.4724
83.9441
84.1675
87.6582
Height [cts]
339.56
2657.62
2213.99
1026.67
885.53
490.00
3174.83
3311.24
3633.61
7242.26
4347.90
236.29
436.85
3786.38
2754.43
6272.04
3381.13
297.82
537.54
298.68
4015.57
2293.14
908.79
FWHM
[°2Th.]
0.2880
0.1320
0.1200
0.2160
0.3840
0.3840
0.1920
0.1680
0.0960
0.1320
0.1080
0.1920
0.1920
0.1320
0.1200
0.1680
0.1200
0.4800
0.1920
0.2880
0.1440
0.0840
0.1440
d-spacing [A]
1.60285
1.57332
1.56994
1.55713
1.55152
1.49056
1.43005
1.42765
1.41150
1.40750
1.40710
1.37430
1.29491
1.28461
1.28452
1.26213
1.26185
1.23156
1.22114
1.16860
1.15182
1.15219
1.11233
Rel. Int. [%]
1.28
10.04
8.37
3.88
3.35
1.85
12.00
12.51
13.73
27.37
16.43
0.89
1.65
14.31
10.41
23.70
12.78
1.13
2.03
1.13
15.17
8.67
3.43
Matched by
01-075-1862
00-004-0587
00-004-0587
01-074-1132;
01-086-2270
01-075-1862;
01-074-1132
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1862;
00-022-1235
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
01-077-2064
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-085-1327
01-077-2064
00-004-0587;
01-080-2171;
F-157
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 158 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
87.9440
620.76
0.1440
1.11221
2.35
01-080-2172;
01-080-2173;
01-080-1385
90.3685
94.4877
94.8264
99.2268
101.0832
101.4460
101.8271
107.7595
108.6038
108.9826
109.7756
304.75
1867.63
1349.97
216.51
1140.37
1675.18
804.55
618.28
1397.59
1107.36
1443.59
0.1440
0.0960
0.1440
0.7680
0.0840
0.1680
0.1920
0.1920
0.0960
0.1920
0.0480
1.08588
1.04910
1.04884
1.01130
0.99768
0.99510
0.99487
0.95360
0.94852
0.94863
0.94165
1.15
7.06
5.10
0.82
4.31
6.33
3.04
2.34
5.28
4.18
5.46
00-022-1235
00-004-0587;
00-004-0864
00-004-0587
00-004-0587
00-043-1022
F-158
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 159 of 478
3.2: 2536-D-SC
3.2.1: Measurement Conditions
Dataset Name
File name
d-sc, no cover.udf
Sample Identification 2536-D-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2536-D-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2536-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-ASCII (.UDF)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
3.2.2: Main Graphics, Analyze View of 2536-D
F-159
-------
2536-d-sc, no cover
• Aluminum Oxide (01-075-
| Potassium Chloride (01-0
Sodium Chloride (01-1
Spinel (01-086-2258)
• Aluminum Nitride (01-076
Aluminum (01-085-1327)
• Periclase, syn (00-043-10
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 160 of 478
VV V
10 20 30 40 50 60 70 80 90 100 110
Position [°2Theta] (Copper (Cu))
Fluorite, syn 11.1 % |
Magnesium Aluminum Oxide 10.1 %
Aluminum Oxide Nitride 8.1 %
Aluminum Oxide 7.1 %\
| Aluminum Nitride 6.1 % |
Sodium Chloride 15.2%
5ylvite,syn17.2% |
Calcite 1 %
Periclase, syn 1 % |
blpasolite, syn J % |
Alur
Aluminum Oxide Nitride 4 % |
F-160
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 161 of 478
3.2.3: Pattern List of 2536-D
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
Score
45
52
47
49
46
16
17
17
34
31
22
27
20
18
9
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
4
17
15
10
6
8
5
4
2
1
11
3
5
7
1
Matched
Lines
18
10
9
15
11
13
12
12
5
7
6
17
35
12
14
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
3.2.4: Peak List of 2536-D
F-161
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 162 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
18.9648
23.0226
24.4323
25.4958
26.5895
27.2825
28.3136
31.1963
31.6035
33.1246
35.0680
35.9822
36.7945
37.8534
38.4538
40.4392
40.5475
42.8443
43.2691
44.7702
45.3504
45.4570
46.9514
47.9232
49.7134
2326.35
84.84
237.65
1324.73
456.64
4671.33
47715.23
5728.80
46034.18
5396.51
2643.60
3739.81
10538.25
4563.95
3798.12
25620.43
21963.80
2058.79
2815.07
8676.52
25190.44
17604.60
933.14
349.55
1513.63
0.0492
0.2362
0.1574
0.0787
0.1574
0.1574
0.1476
0.0787
0.1771
0.1082
0.0590
0.1771
0.0590
0.1082
0.0689
0.1800
0.0720
0.2160
0.1680
0.1200
0.1560
0.0600
0.2880
0.2880
0.1440
4.67959
3.86317
3.64336
3.49375
3.35247
3.26888
3.15213
2.86712
2.83110
2.70450
2.55894
2.49600
2.44274
2.37681
2.34107
2.22875
2.22857
2.10904
2.08931
2.02268
1.99815
1.99866
1.93367
1.89671
1.83252
4.88
0.18
0.50
2.78
0.96
9.79
100.00
12.01
96.48
11.31
5.54
7.84
22.09
9.56
7.96
53.69
46.03
4.31
5.90
18.18
52.79
36.90
1.96
0.73
3.17
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270;
01-086-2340
01-077-2064
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587
00-043-1022
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
01-075-1620
F-162
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 163 of 478
Pos. [°2Th.]
50.0670
50.1136
52.4402
53.7472
55.5928
56.3777
56.5263
57.4123
58.5508
59.2293
61.1997
62.2188
65.1245
65.3501
66.1005
66.3045
66.4853
68.0903
69.6438
71.3081
72.4984
Height [cts]
6114.06
7203.32
999.57
891.88
1068.06
6536.13
3831.04
2011.73
3167.49
5045.98
492.80
831.05
6427.84
5999.05
5358.49
8312.54
5689.75
1191.87
396.47
1211.83
589.27
FWHM
[°2Th.]
0.0600
0.0480
0.1440
0.1440
0.2880
0.1320
0.0960
0.0720
0.0960
0.2160
0.3840
0.1680
0.2640
0.0960
0.0720
0.1440
0.1200
0.1440
0.2400
0.1920
0.2400
d-spacing [A]
1.82040
1.82334
1.74346
1.70411
1.65183
1.63068
1.63079
1.60373
1.57523
1.55879
1.51324
1.49088
1.43121
1.43036
1.41242
1.40857
1.40867
1.37591
1.34897
1.32152
1.30273
Rel. Int. [%]
12.81
15.10
2.09
1.87
2.24
13.70
8.03
4.22
6.64
10.58
1.03
1.74
13.47
12.57
11.23
17.42
11.92
2.50
0.83
2.54
1.23
Matched by
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
01-075-1862;
01-086-2270
01-077-2064
01-074-1132;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270;
01-086-2340
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620;
01-086-2340
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-075-1620
F-163
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 164 of 478
Pos. [°2Th.]
72.9586
73.5986
73.8301
75.1386
75.3800
76.7518
77.2363
78.1901
80.9528
82.5211
83.8290
84.1277
85.7247
87.5423
87.8473
88.8869
90.2701
91.0829
93.9785
94.4035
94.7157
98.1470
99.1917
100.9868
101.3529
Height [cts]
644.45
3539.41
2774.28
5372.07
3065.32
501.40
831.44
831.94
170.81
651.59
3135.95
1668.49
142.97
755.11
537.56
82.77
263.32
293.16
975.10
2085.79
1610.23
147.54
475.19
1278.47
1538.47
FWHM
[°2Th.]
0.1440
0.1320
0.1200
0.1320
0.0720
0.1920
0.2880
0.1920
0.3840
0.1920
0.0840
0.1440
0.3840
0.2160
0.1440
0.3840
0.1680
0.3840
0.1680
0.1680
0.1440
0.2880
0.1440
0.1920
0.1920
d-spacing [A]
1.29564
1.28595
1.28567
1.26336
1.26305
1.24078
1.23420
1.22152
1.18666
1.16803
1.15311
1.14977
1.13239
1.11350
1.11318
1.10011
1.08681
1.07922
1.05343
1.04981
1.04977
1.01952
1.01157
0.99838
0.99576
Rel. Int. [%]
1.35
7.42
5.81
11.26
6.42
1.05
1.74
1.74
0.36
1.37
6.57
3.50
0.30
1.58
1.13
0.17
0.55
0.61
2.04
4.37
3.37
0.31
1.00
2.68
3.22
Matched by
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-086-2340
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327
01-075-1620
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-086-2340
01-075-1862;
01-077-2064;
01-080-2171;
01-086-2270
01-074-1132;
01-075-1620;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385
01-075-1862;
01-086-2270
00-022-1235
00-043-1022
00-004-0587;
00-004-0864
00-004-0587
F-164
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 165 of 478
Pos. [°2Th.]
101.6689
104.7063
107.6206
Height [cts]
769.34
85.99
400.24
FWHM
[°2Th.]
0.1440
0.4800
0.1920
d-spacing [A]
0.99599
0.97286
0.95444
Rel. Int. [%]
1.61
0.18
0.84
Matched by
108.4821 987.04 0.2160 0.94925 2.07 00-004-0587
108.8723 747.80 0.1920 0.94929 1.57
109.8756 1873.64 0.1080 0.94108 3.93 00-043-1022
109.9382 1599.01 0.0360 0.94072 3.35 00-043-1022
F-165
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 166 of 478
3.3: 2538-D-SC
3.3.1: Measurement Conditions
Dataset Name
File name
d-sc, no cover_002.udf
Sample Identification 2538-D-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2538-D-SC, no cover_002
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2538-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-ASCII (.UDF)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
F-166
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 167 of 478
3.3.2: Main Graphics, Analyze View of 2538-D
2538-d-sc, no cover_002
Aluminum Oxide (01-075-
Potassium Chloride (01-0
Sodium Chloride (01-072
Spinel (01-086-2258)
Aluminum Nitride (01-076
Aluminum (01-085-1327)
Quartz, syn (01-083-2467
Periclase, syn (00-043-10
865
5-0;
1668
96)
rrm
50 60 70 80
Position [°2Theta] (Copper (Cu))
5vlvite,syn1S.8% |
Fluorite, syn 11.9 %
Aluminum Oxide Nitride 9.9 %
Aluminum Oxide 9.9 %
Sodium Chloride 18.S %|
Periclase, syn 1 % |r|
— "_%j
Aluminum Oxide 2 %
"
- ' "'" ...... "'" "•"•'"" ---_^j - I Aluminum Cixide Nitride 6.9 % I
Magnesium Aluminum C'xide 7.9% | -
F-167
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 168 of 478
3.3.3: Pattern List of 2538-D
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-080-
1385
01-085-
0930
Score
36
61
56
48
22
18
19
20
29
21
24
24
20
26
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Aluminum
Oxide
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
A12.667 O4
Si O2
2
19
19
8
2
10
7
5
2
1
12
3
10
1
Matched
Lines
15
10
9
14
7
11
11
11
5
7
7
15
11
19
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-168
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 169 of 478
3.3.4: Peak List of 2538-D:
Pos. [°2Th.]
18.9438
20.7704
24.4085
25.5050
26.5997
27.2737
28.2561
31.6053
33.1502
35.0525
36.7631
37.6912
38.3839
40.4439
42.8426
43.2395
44.7347
45.3114
45.4595
46.9476
47.8585
50.0744
50.2556
52.4082
53.7391
55.5823
56.3258
56.5058
Height [cts]
1231.34
257.58
210.45
310.69
1330.72
5273.95
52942.88
54434.18
424.05
783.02
6715.17
901.41
1862.09
30658.58
662.64
875.46
6804.80
27833.49
16862.22
387.51
183.54
7577.27
4956.66
204.57
843.02
639.63
7178.94
4251.19
FWHM
[°2Th.]
0.2558
0.1181
0.1378
0.1181
0.0689
0.0787
0.1968
0.1574
0.1378
0.1378
0.2165
0.1968
0.0984
0.1378
0.1968
0.1378
0.2558
0.1920
0.0840
0.3840
0.1920
0.1200
0.0840
0.1440
0.0960
0.2880
0.1560
0.0960
d-spacing [A]
4.68473
4.27669
3.64686
3.49251
3.35122
3.26991
3.15842
2.83095
2.70246
2.56004
2.44475
2.38666
2.34517
2.23035
2.11087
2.09241
2.02588
1.99978
1.99856
1.93382
1.89912
1.82015
1.81852
1.74445
1.70435
1.65212
1.63206
1.63133
Rel. Int. [%]
2.26
0.47
0.39
0.57
2.44
9.69
97.26
100.00
0.78
1.44
12.34
1.66
3.42
56.32
1.22
1.61
12.50
51.13
30.98
0.71
0.34
13.92
9.11
0.38
1.55
1.18
13.19
7.81
Matched by
01-074-1132;
00-022-1235
01-085-0930
01-075-1862
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064
01-075-1620
01-075-1862
01-074-1132;
00-043-1022
01-075-1862;
01-080-2172;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0930
00-043-1022
01-075-1862
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064
00-004-0864
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862
01-077-2064
01-074-1132;
00-004-0864
01-077-2064
F-169
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 170 of 478
Pos. [°2Th.]
57.3704
58.5603
58.6915
59.3577
62.2232
65.1813
65.3088
66.0710
66.2792
66.4828
68.0791
72.9172
73.6113
75.1321
75.3609
77.3320
78.1427
82.5149
83.8531
84.0919
85.7202
87.5360
87.8267
90.2347
Height [cts]
702.70
3572.44
2971.99
2284.94
227.60
5821.19
5183.02
4505.38
8559.06
5252.83
503.49
460.53
4124.26
6081.39
3473.34
486.45
443.77
464.18
3658.78
2017.07
48.86
869.56
585.14
273.20
FWHM
[°2Th.]
0.1920
0.1080
0.1200
0.1440
0.2880
0.3120
0.1680
0.1200
0.1080
0.1200
0.1920
0.1440
0.1320
0.1680
0.0960
0.5760
0.2400
0.5280
0.1200
0.1440
0.5760
0.1440
0.1200
0.1440
d-spacing [A]
1.60480
1.57500
1.57179
1.55573
1.49079
1.43010
1.43116
1.41298
1.40905
1.40872
1.37611
1.29627
1.28575
1.26346
1.26332
1.23291
1.22214
1.16810
1.15284
1.15303
1.13244
1.11357
1.11339
1.08714
Rel. Int. [%]
1.29
6.56
5.46
4.20
0.42
10.69
9.52
8.28
15.72
9.65
0.92
0.85
7.58
11.17
6.38
0.89
0.82
0.85
6.72
3.71
0.09
1.60
1.07
0.50
Matched by
01-075-1862;
01-085-0930
00-004-0587
00-004-0587
01-074-1132;
01-075-1620
00-043-1022
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171
01-075-1862;
00-022-1235;
01-085-0930
01-077-2064
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-075-1862;
01-074-1132
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327
01-077-2064;
01-085-0930
01-074-1132;
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
00-022-1235
F-170
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 171 of 478
Pos. [°2Th.] Height [cts] FWHM d-spacing [A] Rel. Int. [%] Matched by
94.3880
94.7214
2060.87
1321.76
0.0840
0.1920
1.04994
1.04712
3.79
2.43
00-004-0587;
00-004-0864
00-004-0587
99.2790 362.75 0.8640 1.01091 0.67
100.9866 1100.77 0.1440 0.99838 2.02
101.3540 1632.38 0.1200 0.99575 3.00 00-004-0587
101.7437 739.52 0.1440 0.99546 1.36
107.5972 398.67 0.2400 0.95459 0.73
108.4551 1007.98 0.1680 0.94941 1.85 00-004-0587
108.8391 772.45 0.1920 0.94713 1.42 00-004-0587
109.9171 1666.59 0.0600 0.94084 3.06 00-043-1022
F-171
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 172 of 478
3.4: 2540-D-SC
3.4.1: Measurement Conditions
Dataset Name
File name
D-SC, no cover.udf
Sample Identification 2540-D-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
2540-D-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2540-
3.4.2: Main Graphics, Analyze View of 2540-D
F-172
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 173 of 478
2540-D-SC, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0;
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Periclase, syn (00-043-1022)
TTTT
50 60 70
Position [°2Theta] (Copper (Cu))
Sylvite,syn10.9%
Aluminum Oxide 10.9 % |
Magnesium Aluminum Oxide 9.9 %
Aluminum Oxide Nitride 7.9 %
| Fluorite, syn 7.9
Aluminum Oxide Nitride 11.9 % |
Sodium Chloride 15.8 %"|
Aluminum Nitride 2 %
. - -.- II *•:-. I
Periclase, syn 1 %[]
Aluminum Oxide Nitride 6.9 %
3.4.3: Pattern List of 2540-D
F-173
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 174 of 478
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
Score
35
55
56
54
26
17
17
19
27
21
22
27
25
19
6
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
Chemical
Formula
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
Semi Quant
[%]
3
11
16
10
2
12
8
7
2
1
8
4
5
11
1
Matched
Lines
15
10
9
14
8
11
11
11
5
7
7
17
35
11
19
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-174
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 175 of 478
3.4.4: Peak List of 2540-D
Pos. [°2Th.]
18^9959
20.8595
24.4649
25.4704
26.5081
27.2415
28.2125
28.2798
28.3219
31.5645
31.6435
33.1508
35.0589
36.8349
37.7911
38.5195
40.4530
42.8461
43.3227
Height [cts]
59228
27.22
31.89
138.62
130.71
1928.81
10839.66
13482.11
13170.16
21506.33
23927.71
458.02
429.67
3990.17
601.90
942.09
9813.46
433.76
571.45
FWHM
[°2Th.]
0.3149
0.4723
0.7872
0.1574
0.2362
0.0787
0.1320
0.0480
0.0960
0.1560
0.1800
0.3840
0.1200
0.3360
0.2880
0.2880
0.3000
0.2400
0.2880
d-spacing [A]
4767200
4.25862
3.63859
3.49718
3.36258
3.27370
3.16058
3.16104
3.14862
2.83217
2.82528
2.70018
2.55747
2.43814
2.37861
2.33529
2.22802
2.10896
2.08685
Rel. Int. [%]
248
0.11
0.13
0.58
0.55
8.06
45.30
56.35
55.04
89.88
100.00
1.91
1.80
16.68
2.52
3.94
41.01
1.81
2.39
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
00-004-0587;
00-004-0864;
01-086-2270
01-077-2064;
01-080-2171;
01-086-2270;
01-080-1385
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-074-1132;
00-043-1022;
01-085-0930
01-075-1862;
01-075-1620;
01-080-2172;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587;
01-085-0930
00-043-1022
01-075-1862;
01-086-2270
F-175
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 176 of 478
Pos. [°2Th.]
44.8161
45.2848
45.4432
46.9174
50.1702
52.5524
53.8012
55.6695
56.4889
57.4671
58.6422
59.3717
62.3105
65.1584
65.2785
Height [cts]
4661.75
13747.59
17065.36
294.86
3537.08
182.01
644.38
513.70
5305.53
519.70
1937.51
2314.01
187.70
4817.07
5470.85
FWHM
[°2Th.]
0.3120
0.0840
0.1920
0.3840
0.0720
0.3360
0.1680
0.2880
0.1200
0.3360
0.2880
0.2160
0.3840
0.2160
0.1200
d-spacing [A]
2.02072
2.00089
1.99428
1.93500
1.81690
1.74001
1.70253
1.64973
1.62773
1.60233
1.57299
1.55539
1.48891
1.43055
1.43175
Rel. Int. [%]
19.48
57.45
71.32
1.23
14.78
0.76
2.69
2.15
22.17
2.17
8.10
9.67
0.78
20.13
22.86
Matched by
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
00-004-0864;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
F-176
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 177 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
66.3890 5430.32 0.3840 1.40698
68.1319 337.34 0.2880 1.37517
71.4634 156.25 0.6720 1.31903
72.9819 421.88 0.2400 1.29528
73.6844 2493.45 0.1440 1.28466
75.2201 6098.28 0.1920 1.26220
75.2935 5760.19 0.0960 1.26115
75.5022 2835.23 0.1440 1.26131
77.3433 603.41 0.5760 1.23276
78.2884 524.70 0.3840 1.22023
82.5959 505.60 0.3360 1.16716
22.69 01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
1.41 01-075-1862;
00-022-1235;
01-085-0930
0.65 01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
1.76 01-077-2064;
01-086-2270
10.42 00-004-0587;
00-022-1235;
01-085-0930
25.49 01-077-2064
24.07 01-077-2064;
01-080-2171;
01-080-1385
11.85
2.52 01-075-1862;
01-074-1132;
01-086-2270
2.19 01-074-1132;
01-085-1327;
00-043-1022;
00-022-1235;
01-086-2270
2.11 01-074-1132;
01-085-1327;
01-086-2270
F-177
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 178 of 478
Pos. [°2Th.]
83.9310
84.2426
85.8171
87.6250
90.3502
94.4590
94.8377
99.3814
101.0748
101.4645
101.8343
107.6740
108.5525
108.9883
109.7606
Height [cts]
4080.90
1841.67
77.16
607.09
331.65
1600.49
1127.45
449.38
1311.73
1473.39
575.51
658.20
1091.08
995.15
1510.33
FWHM
[°2Th.]
0.1080
0.1920
0.5760
0.1680
0.2400
0.1200
0.2160
0.8640
0.1920
0.1920
0.1440
0.1920
0.2160
0.1440
0.0480
d-spacing [A]
1.15196
1.14850
1.13141
1.11267
1.08605
1.04934
1.04615
1.01014
0.99775
0.99497
0.99482
0.95412
0.94883
0.94860
0.94174
Rel. Int.[%]
17.06
7.70
0.32
2.54
1.39
6.69
4.71
1.88
5.48
6.16
2.41
2.75
4.56
4.16
6.31
Matched by
01-075-1862;
01-077-2064;
01-086-2270;
01-085-0930
01-075-1862;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-074-1132;
01-075-1620;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
00-022-1235
00-004-0587;
00-004-0864
00-004-0587
00-004-0587
00-004-0587;
00-022-1235
00-004-0587
00-043-1022
F-178
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 179 of 478
F-179
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 180 of 478
FACILITY E
4.1: 2437-E-SC
4.1.1: Measurement Conditions
Dataset Name
File name
SC.sd
Sample Identification 2437-E-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 8/1/2010 10:50:00 AM
2437-E-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2437-E-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
10.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
30 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
4.1.2: Main Graphics, Analyze View
F-180
-------
V
2437-E-SC
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
I Quartz, syn (01-083-2467)
I Periclase, syn (00-043-1022)
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 181 of 478
V V
TTTT
jt.
™
10 20 30 40 50 60 70 80 90 100
Position [°2Theta] (Copper (Cu))
Magnesium Aluminum Qxide 8.8 % | | Sylvite, syn 9.8 % |
Aluminum Oxide Nitride S.6 % |
Aluminum Oxide 8.8 %
Fluorite.syn 7.8%
Aluminum Oxide 6.9 %
Sodium Chloride 17.6 %|
Anhydrite 5.9 %|
Alui) Aluminum 2.9 % I. I
^=i—i — '-i 1
Alumj Aluminum Qxide Nitride 4.9 % |
4.1.3: Pattern List of 2437-E-SC
F-181
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 182 of 478
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
01-085-
0930
Score
52
34
39
39
32
12
12
14
34
35
16
25
23
13
20
20
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
9
10
18
9
5
9
6
5
3
2
8
3
6
7
1
1
Matched
Lines
19
9
9
13
8
11
11
10
5
7
5
14
33
11
14
18
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-182
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 183 of 478
4.1.4: Peak List of 2437-E-SC
DS. [°2Th.]
ia0318
10.1612
10.9525
16.3556
18.9770
20.8380
21.9560
23.0907
24.4887
25.5399
26.6231
27.3109
28.3037
29.4108
31.6833
33.2117
35.1041
35.1712
35.9923
36.8398
37.7502
37.9015
38.4849
39.4859
40.4900
Height [cts]
9~82
41.32
77.56
34.02
616.76
237.92
132.00
154.82
186.25
1054.86
1162.05
2322.63
10298.15
654.94
25604.78
1590.32
1927.60
2126.79
1341.19
3370.86
1670.03
1610.50
1976.15
484.77
6334.31
FWHM
[°2Th.]
0.0394
0.2362
0.6298
0.2362
0.1771
0.1378
0.6298
0.2362
0.1574
0.1082
0.1082
0.1771
0.2263
0.1574
0.1968
0.0886
0.0720
0.0787
0.1771
0.0984
0.1680
0.1378
0.0886
0.1181
0.2066
d-spacing [A]
O1757
8.70550
8.07833
5.41975
4.67661
4.26296
4.04836
3.85192
3.63510
3.48782
3.34832
3.26554
3.15322
3.03699
2.82416
2.69760
2.55428
2.55167
2.49532
2.43984
2.38109
2.37390
2.33925
2.28222
2.22791
Rel. Int. [%]
064
0.16
0.30
0.13
2.41
0.93
0.52
0.60
0.73
4.12
4.54
9.07
40.22
2.56
100.00
6.21
7.53
8.31
5.24
13.16
6.52
6.29
7.72
1.89
24.74
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
00-022-1235
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
01-086-2340;
01-085-0930
00-004-0587;
01-085-0930
F-183
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 184 of 478
DS. [°2Th.]
42.9106
43.3508
44.7959
45.4155
46.9861
47.3652
50.1310
52.5158
53.8351
54.9371
55.6850
56.4437
57.4859
57.6648
58.5688
59.3647
61.2844
62.3040
65.2679
66.2187
Height [cts]
2046.33
2777.44
3386.45
15822.34
678.58
565.44
2156.88
1131.31
716.61
285.78
619.24
4794.50
2541.21
1471.31
1128.72
2267.61
595.85
1154.72
3525.04
4146.39
FWHM
[°2Th.]
0.0984
0.1279
0.2362
0.1968
0.1181
0.1968
0.0886
0.1082
0.1181
0.2362
0.2362
0.1181
0.1440
0.0960
0.3360
0.2160
0.1920
0.1920
0.1680
0.0960
d-spacing [A]
2.10768
2.08729
2.02326
1.99709
1.93393
1.91933
1.81973
1.74257
1.70295
1.67136
1.65068
1.63028
1.60185
1.60127
1.57479
1.55556
1.51135
1.48905
1.42841
1.41019
Rel. Int. [%]
7.99
10.85
13.23
61.79
2.65
2.21
8.42
4.42
2.80
1.12
2.42
18.73
9.92
5.75
4.41
8.86
2.33
4.51
13.77
16.19
Matched by
00-043-1022
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327
01-077-2064;
01-080-2171;
01-086-2270
00-004-0864;
01-086-2270;
01-086-2340
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862
01-077-2064
01-085-0930
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340
00-004-0587
01-074-1132;
01-075-1620
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
00-004-0587;
01-077-2064;
01-075-1620
F-184
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 185 of 478
Pos. [°2Th.]
66.5178
68.1776
71.4170
73.0332
73.6077
75.2518
75.4977
76.8688
77.2708
78.2542
78.6060
80.6712
82.6334
83.9763
84.2243
86.4287
87.5641
88.9726
90.3570
91.1930
Height [cts]
3018.82
1445.79
604.40
546.22
1240.28
4716.62
2488.47
735.69
668.20
729.98
546.37
222.99
420.55
2829.54
1619.23
132.28
281.31
170.65
202.48
294.13
FWHM
[°2Th.]
0.0960
0.1320
0.2400
0.1440
0.3840
0.1320
0.1200
0.1200
0.3360
0.1200
0.2400
0.1920
0.1920
0.2040
0.0960
0.3840
0.3840
0.1920
0.1920
0.1320
d-spacing [A]
1.40806
1.37436
1.31977
1.29450
1.28581
1.26174
1.26137
1.23918
1.23374
1.22068
1.21609
1.19009
1.16673
1.15146
1.15155
1.12497
1.11328
1.09927
1.08599
1.07820
Rel. Int. [%]
11.79
5.65
2.36
2.13
4.84
18.42
9.72
2.87
2.61
2.85
2.13
0.87
1.64
11.05
6.32
0.52
1.10
0.67
0.79
1.15
Matched by
01-075-1862;
00-022-1235;
01-085-0930
01-075-1620;
01-080-2173;
01-086-2270
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-086-2340;
01-085-0930
01-077-2064
01-075-1862;
01-086-2270
01-075-1862;
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
00-043-1022;
01-086-2270;
01-086-2340
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-086-2340;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862
00-022-1235
F-185
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 186 of 478
Pos. [°2Th.]
94.0951
94.4141
95.2360
98.3857
99.3261
101.1123
101.4025
107.7911
109.8167
Height [cts]
661.18
873.67
654.09
107.36
261.23
1201.07
862.12
160.43
961.47
FWHM
[°2Th.]
0.1680
0.1920
0.1200
0.2880
0.6720
0.2400
0.1680
0.1440
0.0720
d-spacing [A]
1.05244
1.04972
1.04282
1.01768
1.01056
0.99748
0.99788
0.95341
0.94142
Rel. Int. [%]
2.58
3.41
2.55
0.42
1.02
4.69
3.37
0.63
3.76
Matched by
00-043-1022;
00-004-0864
00-004-0587;
00-004-0864
00-043-1022
F-186
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 187 of 478
4.2: 2439-E-SC
4.2.1: Measurement Conditions of 2439-E-SC
Dataset Name
File name
E-SC_002.udf
Sample Identification 2439-E-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
2439-E-SC_002
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2439-
4.2.2: Main Graphics, Analyze View of 2439-E
F-187
-------
V V
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 188 of 478
V V V V
30000 -
20000 -
10000 -
2439-E-SC_002
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565
Aluminum (01 -085-1 327)
• Quartz, syn (01-083-2467)
' '' '" I'I'MI
A/
16)
1
s
1 s
n <
II J I
ill
| J H| ,
MiLJiLiilf mm A i r ^ , ii nil
50 60 70
Position [°2Theta] (Copper (Cu))
Sylvite, syn 11 %
Aluminum Oxide Nitride 10 %
Magnesium Aluminum Oxide 10 %
Aluminum Oxide 8 %
| Fluorite, ^ Anhydrite 5 %
Aluminum Oxide Nitride 6 % |
Sodium Chloride 20 %
Quartz 1 % |=i
renciase, syn 1 %
Elpasolite, syn 3 %
Aluminum Oxide Nitride 5 %
F-188
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 189 of 478
4.2.3: Pattern List of 2439-E
Ref. Code
01-075-1862
00-004-0587
01-077-2064
01-074-1132
01-075-1620
01-080-2171
01-080-2172
01-080-2173
01-085-1327
00-043-1022
00-004-0864
00-022-1235
01-086-2270
01-080-1385
01-086-2340
01-085-0930
Score
52
46
48
52
38
14
15
16
40
31
18
27
20
15
23
18
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
5
11
20
10
4
10
6
5
3
1
7
3
5
8
1
1
Matched
Lines
19
10
9
15
9
12
12
12
5
6
6
15
35
12
15
18
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-189
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 190 of 478
4.2.4: Peak List of 2439-E
Pos. [°2Th.]
11.3009
19.3118
21.1856
22.5859
23.4176
24.7397
25.8924
26.9383
27.6698
28.6289
29.6613
29.7636
31.5592
31.9782
33.5187
35.4407
36.3405
37.1794
38.0545
38.2011
38.8084
39.7562
40.7717
42.0489
43.2399
43.6370
45.1144
45.7058
45.8585
Height [cts]
197.85
980.34
176.61
228.51
218.79
162.77
887.58
1087.54
3277.24
15226.77
1067.13
1179.17
2618.79
34307.43
1816.80
1836.06
1821.14
5434.55
1843.79
1983.77
3475.57
701.17
9357.56
515.68
1288.18
2353.04
5437.69
22632.19
11620.57
FWHM
[°2Th.]
0.2755
0.1378
0.1181
0.2362
0.1968
0.2362
0.1378
0.1378
0.1378
0.1476
0.0960
0.1181
0.0787
0.1673
0.1968
0.0886
0.1574
0.0590
0.0960
0.1378
0.0984
0.2362
0.1082
0.3149
0.1968
0.1378
0.2558
0.1800
0.0960
d-spacing [A]
7.83002
4.59627
4.19381
3.93685
3.79889
3.59879
3.44112
3.30986
3.22399
3.11813
3.00941
3.00179
2.83498
2.79878
2.67359
2.53288
2.47221
2.41833
2.36275
2.35597
2.32049
2.26733
2.21317
2.14886
2.09239
2.07427
2.00971
1.98343
1.98210
Rel. Int. [%]
0.58
2.86
0.51
0.67
0.64
0.47
2.59
3.17
9.55
44.38
3.11
3.44
7.63
100.00
5.30
5.35
5.31
15.84
5.37
5.78
10.13
2.04
27.28
1.50
3.75
6.86
15.85
65.97
33.87
Matched by
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-086-2270
01-077-2064
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-086-2270
01-075-1620
00-022-1235
01-086-2270
01-086-2270
01-075-1862;
01-086-2270;
01-086-2340
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
F-190
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 191 of 478
Pos. [°2Th.]
47.2822
47.6316
48.9087
50.4424
52.8169
54.1304
55.9550
56.6904
56.8832
57.7574
58.8821
59.6329
61.6156
62.5616
65.5012
65.7179
66.4604
66.6250
68.4518
69.9929
Height [cts]
775.24
804.24
473.62
3211.73
982.45
984.36
858.92
6536.55
4000.24
1912.57
1770.73
3295.55
603.52
727.95
5426.07
4140.41
5270.22
5441.04
1291.72
316.23
FWHM
[°2Th.]
0.1920
0.2880
0.3840
0.2160
0.1440
0.2160
0.2160
0.0840
0.0960
0.0840
0.1440
0.2160
0.3840
0.2400
0.2160
0.1440
0.1200
0.1440
0.1920
0.2880
d-spacing [A]
1.92092
1.90764
1.86077
1.80773
1.73191
1.69295
1.64199
1.62242
1.62140
1.59496
1.56715
1.54920
1.50402
1.48353
1.42389
1.42324
1.40564
1.40257
1.36952
1.34309
Rel. Int. [%]
2.26
2.34
1.38
9.36
2.86
2.87
2.50
19.05
11.66
5.57
5.16
9.61
1.76
2.12
15.82
12.07
15.36
15.86
3.77
0.92
Matched by
01-086-2270;
01-086-2340
01-074-1132;
00-022-1235
01-085-0930
01-086-2270
00-004-0864
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-086-2340
01-086-2270
00-022-1235;
01-086-2270
01-075-1862
01-086-2270
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-074-1132;
00-004-0864;
00-022-1235;
01-085-0930
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385;
01-086-2340
71.6618
746.77
0.2400
1.31586
2.18
F-191
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 192 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
73.2794
699.67
0.1920
1.29076
2.04
01-085-0930
73.9159
75.5131
75.7405
77.1153
77.5716
78.5302
80.9449
82.8676
84.2112
84.4539
86.0198
87.8340
90.6213
2023.95
6945.03
3740.07
615.77
836.49
1203.67
186.52
656.36
4297.52
2344.54
151.62
436.31
303.24
0.1920
0.1320
0.0960
0.1200
0.1920
0.1680
0.2880
0.2400
0.0480
0.1440
0.3840
0.2400
0.1440
1.28121
1.25803
1.25793
1.23584
1.22970
1.21708
1.18675
1.16403
1.14884
1.14616
1.12926
1.11056
1.08351
5.90
20.24
10.90
1.79
2.44
3.51
0.54
1.91
12.53
6.83
0.44
1.27
0.88
00-004-0587;
01-074-1132;
00-022-1235
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-074-1132;
01-086-2270;
01-085-0930
01-074-1132;
00-043-1022;
01-086-2270;
01-086-2340
01-075-1620;
01-086-2340;
01-085-0930
01-074-1132;
01-086-2270
01-075-1862;
01-080-2171;
01-080-2172;
01-086-2270;
01-080-1385
01-075-1862;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1862;
01-074-1132;
01-075-1620;
01-086-2270;
01-086-2340
00-004-0587;
01-080-2172;
01-080-2173;
01-080-1385
00-022-1235
F-192
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 193 of 478
Pos. [°2Th.] Height [cts] FWHM d-spacing [A] Rel. Int. [%] Matched by
91.3735 299.85 0.2400 1.07654 0.87
94.3004 847.70 0.1440 1.05069 2.47 00-004-0587;
00-004-0864
94.6656 _ 1308.46 _ 0.2880 _ 1.04759 _ 3.81 _ 00-004-0587
95.4417 587.83 0.1440 1.04112 1.71
99.5062 372.11 0.2880 1.00921 1.08
101.3281 1492.73 0.1680 0.99594 4.35 00-004-0587
101.6612 1125.89 0.2400 0.99357 3.28 00-004-0587;
00-022-1235
107.9463 417.63 0.2400 0.95247 1.22
108.7062 470.33 0.2880 0.94792 1.37 00-004-0587
F-193
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 194 of 478
FACILITY F
5.1: 2502-F-SC
5.1.1: Measurement Conditions of 2502-F
Dataset Name
File name
f-sc, no cover_002.udf
Sample Identification 2502-F-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2502-F-SC, no cover_002
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2502-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-ASCII (.UDF)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
5.1.2: Main Graphics, Analyze View of 2502-F
F-194
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 195 of 478
V V V V
2502-f-sc, no cover_002
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
_ Aluminum (01-085-1327)
Periclase, syn (00-043-1022)
50 60 70
Position [°2Theta] (Copper (Cu))
Aluminum Oxide Nitride 8.9 %
Magnesium Aluminum Oxide 8.9 %
Aluminum Oxide 7.9 %
| Fluorite, syn 5.9 % |
Aluminum Oxide Nitride 5.9 %
Anhydrite 5.9 %
Aluminum Oxide 9.9 %|
Sodium Chloride 19.S % |
! Aluminum 5 %
Periclase | syn 1 %
Eipasolite. svn 5 %l
Aluminum Oxide Nitride 5 %|
F-195
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 196 of 478
5.1.3: Pattern List of 2502-F
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
Score
60
47
44
46
35
18
20
21
44
33
12
26
19
20
5
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
10
5
20
9
5
9
6
5
5
1
6
5
6
8
1
Matched
Lines
21
10
9
13
9
13
12
12
5
7
4
14
37
13
17
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
1
0
0
0
0
F-196
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 197 of 478
5.1.4: Peak List of 2502-F
Pos. [°2Th.]
18.9355
22.9354
25.5104
26.5767
27.2717
27.3281
28.3134
31.6155
33.1284
35.0772
35.1285
35.9703
36.7986
36.8811
37.6879
38.4071
38.4887
40.4308
41.6723
42.8563
43.2549
43.3146
44.7177
45.3368
45.4581
49.7408
Height [cts]
1535.25
120.75
2851.08
162.38
5159.69
4722.99
10004.57
56625.01
3174.59
5009.13
4464.54
2358.76
6468.07
6475.91
3925.06
8299.79
7142.92
6438.96
210.67
2003.92
6993.65
6772.56
10702.21
38247.57
26512.33
1364.51
FWHM
[°2Th.]
0.1771
0.4723
0.1181
0.1181
0.0720
0.0492
0.1673
0.1870
0.0787
0.1080
0.0720
0.2160
0.1080
0.0840
0.1200
0.0960
0.0600
0.1080
0.3840
0.2160
0.0600
0.0600
0.2880
0.1560
0.1080
0.1920
d-spacing [A]
4.68676
3.87766
3.49178
3.35406
3.26743
3.26353
3.15216
2.83006
2.70419
2.55618
2.55890
2.49473
2.44045
2.43519
2.38489
2.34187
2.34290
2.22919
2.16561
2.10848
2.08996
2.09241
2.02494
1.99871
1.99862
1.83157
ReLIntM
2.71
0.21
5.04
0.29
9.11
8.34
17.67
100.00
5.61
8.85
7.88
4.17
11.42
11.44
6.93
14.66
12.61
11.37
0.37
3.54
12.35
11.96
18.90
67.55
46.82
2.41
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-074-1132;
00-043-1022
01-075-1862;
01-080-2172;
01-080-2173;
01-080-1385
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0930
01-075-1862
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-075-1620
F-197
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 198 of 478
Pos. [°2Th.]
50.1179
51.4443
52.4605
53.7507
55.6203
56.3674
56.5129
57.4375
57.5874
58.5499
59.2490
62.2166
65.0152
65.1495
66.0708
66.2878
66.4158
Height [cts]
2619.87
1130.33
3098.20
1256.15
511.15
10106.26
5927.28
5105.47
2736.30
1214.15
3607.78
432.78
3955.67
5531.12
6629.24
6081.31
4969.95
FWHM
[°2Th.]
0.0840
0.8640
0.1920
0.1440
0.2400
0.1440
0.0960
0.1560
0.0960
0.2400
0.2640
0.4320
0.1680
0.1440
0.0840
0.0960
0.1440
d-spacing [A]
1.81867
1.77485
1.74284
1.70401
1.65108
1.63095
1.63114
1.60309
1.60324
1.57525
1.55832
1.49093
1.43335
1.43072
1.41299
1.40889
1.40648
Rel. Int. [%]
4.63
2.00
5.47
2.22
0.90
17.85
10.47
9.02
4.83
2.14
6.37
0.76
6.99
9.77
11.71
10.74
8.78
Matched by
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
00-022-1235;
01-086-2270
00-043-1022;
01-086-2270
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-1385
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
F-198
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 199 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
01-080-2173;
01-080-1385
68.0817
68.2816
69.6490
71.3457
72.5028
72.9214
73.6102
75.1289
75.3604
76.7686
77.2219
78.1288
78.3978
80.5924
82.3223
83.8206
84.1026
86.2473
87.5224
2778.78
1799.93
175.95
852.85
392.15
622.60
1111.15
8559.88
5136.95
1026.37
854.53
2005.78
1378.01
306.32
673.90
5403.51
2912.46
224.65
176.39
0.0600
0.1200
0.2880
0.4320
0.1920
0.1200
0.2160
0.1560
0.0600
0.0960
0.3840
0.1920
0.1440
0.1920
0.1440
0.1560
0.1440
0.1920
0.2880
1.37606
1.37252
1.34888
1.32091
1.30266
1.29621
1.28577
1.26350
1.26333
1.24055
1.23440
1.22232
1.22183
1.19105
1.17035
1.15320
1.15291
1.12687
1.11371
4.91
3.18
0.31
1.51
0.69
1.10
1.96
15.12
9.07
1.81
1.51
3.54
2.43
0.54
1.19
9.54
5.14
0.40
0.31
01-075-1862;
00-022-1235;
01-085-0930
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-075-1620
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-075-1620
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327;
00-022-1235
01-075-1862
01-085-1327;
00-022-1235
01-077-2064;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
F-199
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 200 of 478
Pos. [°2Th.]
88.8694
90.2402
90.5555
91.0248
93.9934
94.3802
95.1179
95.4192
98.2164
99.2413
100.9998
101.3473
103.2726
104.7221
107.5886
109.9198
Height [cts]
270.30
434.74
320.04
531.21
766.82
1108.72
1142.63
675.46
203.25
444.14
2177.31
1379.23
59.51
48.89
549.22
2588.25
FWHM
[°2Th.]
0.1440
0.1200
0.1440
0.1680
0.1440
0.1920
0.1680
0.1440
0.2880
0.4800
0.0960
0.1680
0.5760
0.7680
0.1680
0.1440
d-spacing [A]
1.10028
1.08709
1.08412
1.07975
1.05331
1.05001
1.04381
1.04389
1.01899
1.01119
0.99828
0.99827
0.98242
0.97275
0.95464
0.94082
Rel. Int. [%]
0.48
0.77
0.57
0.94
1.35
1.96
2.02
1.19
0.36
0.78
3.85
2.44
0.11
0.09
0.97
4.57
Matched by
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-043-1022;
00-004-0864
00-004-0587;
00-004-0864
00-043-1022
F-200
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 201 of 478
5.2: 2504-F-SC
5.2.1: Measurement Conditions of 2504-F
Dataset Name
File name
f-sc, no cover.udf
Sample Identification 2504-F-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2504-F-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2504-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-ASCII (.UDF)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
5.2.2: Main Graphics, Analyze View of 2504-F
F-201
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 202 of 478
2504-f-sc, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
_ Aluminum (01-085-1327)
Periclase, syn (00-043-1022)
20 30 40 50 60 70 80 90
Position [°2Theta] (Copper (Cu))
100 110
| Aluminum Qxide Nitride 13 % |
Aluminum Qxide 11 % |
Magnesium Aluminum Oxide 10%
Aluminum Oxide Nitride 8 %
Aluminum Oxide Nitride 6 %
sodium Chloride 20 %|
Calcite 1 %
! Aluminum Nitride 4 %
| Anhyl
[~| Periclase, syn 3 %
j^ylvite. svn 5
P
Aluminum 4 %
F-202
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 203 of 478
5.2.3: Pattern List of 2504-F
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
Score
53
53
59
53
40
17
17
18
42
35
26
21
17
6
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
6
5
20
10
4
13
8
6
4
3
4
5
11
1
Matched
Lines
21
10
9
14
9
13
13
13
5
6
14
36
13
15
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-203
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 204 of 478
5.2.4: Peak List of 2504-F
Pos. [°2Th.]
11.0087
18.9633
22.2230
23.0497
24.4342
25.5282
26.5840
27.2932
28.2989
29.3337
31.2467
31.6597
33.1649
35.1161
36.0169
36.7808
37.7316
38.4293
40.4803
40.5497
42.8434
43.3082
Height [cts]
84.80
1759.03
166.08
178.98
60.90
1881.51
193.11
4984.32
14010.89
238.44
3611.82
57871.07
2354.74
3657.23
1949.76
7581.28
3031.16
7475.23
8887.73
7755.84
4154.68
6202.02
FWHM
[°2Th.]
0.3149
0.1378
0.4723
0.3149
0.2362
0.0492
0.1574
0.0984
0.1673
0.1574
0.0984
0.1673
0.0984
0.0886
0.1771
0.1082
0.0689
0.0984
0.1560
0.0480
0.2400
0.1200
d-spacing [A]
8.03722
4.67995
4.00031
3.85868
3.64309
3.48939
3.35316
3.26762
3.15374
3.04480
2.86261
2.82621
2.70130
2.55555
2.49367
2.44362
2.38420
2.34250
2.22658
2.22845
2.10908
2.08752
ReLIntM
0.15
3.04
0.29
0.31
0.11
3.25
0.33
8.61
24.21
0.41
6.24
100.00
4.07
6.32
3.37
13.10
5.24
12.92
15.36
13.40
7.18
10.72
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-077-2064
00-004-0587
01-086-2340
01-074-1132;
00-022-1235;
01-086-2270;
01-086-2340
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
00-043-1022
01-075-1862;
01-086-2270;
01-086-2340
F-204
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 205 of 478
Pos. [°2Th.]
44.7095
45.3781
45.5036
50.0975
51.5632
52.4806
53.7697
55.7150
56.3734
56.5608
57.4045
57.5881
58.5670
59.2914
61.2070
62.2420
65.1643
66.1085
66.3017
68.1184
68.2985
71.3502
Height [cts]
11884.63
39493.24
24125.01
3044.90
1221.75
2618.20
1311.76
603.32
10064.22
5275.79
3327.34
2078.26
1380.17
4193.09
303.37
1494.74
7281.14
6079.93
5750.86
2129.03
1286.18
577.73
FWHM
[°2Th.]
0.1440
0.1560
0.0600
0.3120
0.7680
0.0840
0.0840
0.2400
0.1560
0.1080
0.1200
0.1200
0.2160
0.0840
0.3360
0.2880
0.3360
0.0480
0.1440
0.0600
0.1200
0.3360
d-spacing [A]
2.02529
1.99699
1.99672
1.81936
1.77104
1.74222
1.70345
1.64850
1.63079
1.62987
1.60393
1.60322
1.57483
1.55731
1.51308
1.49038
1.43043
1.41227
1.40862
1.37541
1.37222
1.32084
Rel. Int. [%]
20.54
68.24
41.69
5.26
2.11
4.52
2.27
1.04
17.39
9.12
5.75
3.59
2.38
7.25
0.52
2.58
12.58
10.51
9.94
3.68
2.22
1.00
Matched by
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
01-075-1862
01-077-2064
01-074-1132;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270;
01-086-2340
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-1385
01-075-1862;
00-022-1235
01-075-1862;
00-022-1235
01-075-1620;
01-080-2172;
F-205
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 206 of 478
Pos. [°2Th.]
72.4565
72.9630
73.5878
75.1858
75.4205
76.7676
77.2620
78.2043
80.5759
82.3443
82.5496
83.8615
84.1407
86.3399
87.5435
88.8867
90.2808
90.5661
91.0760
93.9937
94.3936
95.1181
95.4464
98.2478
99.2320
101.0090
101.3251
Height [cts]
203.02
585.30
1320.51
9276.18
4561.90
767.11
985.16
1886.81
203.29
626.92
823.11
5902.52
2930.52
158.23
244.90
172.01
480.75
365.77
511.92
1120.94
1316.89
917.22
501.05
191.79
601.64
2038.36
1462.45
FWHM
[°2Th.]
0.2880
0.1200
0.1680
0.1560
0.0480
0.1200
0.2400
0.1680
0.1920
0.1920
0.2400
0.1320
0.0720
0.3840
0.2400
0.1440
0.1200
0.1440
0.3840
0.2400
0.2400
0.1920
0.1440
0.2880
0.1920
0.2160
0.1440
d-spacing [A]
1.30338
1.29557
1.28611
1.26269
1.26247
1.24057
1.23386
1.22133
1.19125
1.17009
1.16770
1.15274
1.15248
1.12590
1.11349
1.10011
1.08671
1.08403
1.07928
1.05330
1.04989
1.04380
1.04367
1.01874
1.01126
0.99822
0.99843
Rel. Int. [%]
0.35
1.01
2.28
16.03
7.88
1.33
1.70
3.26
0.35
1.08
1.42
10.20
5.06
0.27
0.42
0.30
0.83
0.63
0.88
1.94
2.28
1.58
0.87
0.33
1.04
3.52
2.53
Matched by
01-080-2173;
01-086-2270
01-075-1620
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-086-2340
01-077-2064
01-075-1862;
01-086-2340
01-075-1862;
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-075-1862;
01-086-2340
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-086-2340
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-043-1022
00-004-0587
F-206
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 207 of 478
Pos. [°2Th.]
103.2523
107.5948
108.0210
Height [cts]
45.47
482.64
246.65
FWHM
[°2Th.]
0.5760
0.1440
0.1920
d-spacing [A]
0.98255
0.95460
0.95438
Rel. Int. [%]
0.08
0.83
0.43
Matched by
5.3: 2506-F-SC
5.3.1: Measurement Conditions of 2506-F
Dataset Name
File name
f-sc, no cover.udf
Sample Identification 2506-F-SC, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2506-F-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2506-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-ASCII (.UDF)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
5.3.2: Main Graphics, Analyze View of 2506-F
F-207
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 208 of 478
V V
2506-f-sc, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565
_ Aluminum (01-085-1327)
Periclase, syn (00-043-1022)
50 60 70
Position [°2Theta] (Copper (Cu))
Aluminum Oxide Nitride 15 %
Aluminum Oxide 13 %
Sylvite, syn 9 %
Aluminum Oxide Nitride 8 %
Sodium Chloride 30 %
Aluminum Nitride 1 % |
Aluminum Oxide 2 % |
periclase,syn2% |
Aluminum 4 % |n Oxide 6 % |
Aluminum Oxide Nitride 6 % I
F-208
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 209 of 478
5.3.3: Pattern List of 2506-F
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-022-
1235
01-080-
1385
Score
33
57
61
34
16
15
17
17
49
40
28
17
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Elpasolite,
syn
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
K2 Na Al
F6
A12.667 O4
2
9
30
6
1
15
8
6
4
2
4
13
Matched
Lines
14
10
9
13
6
12
11
11
5
6
14
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
F-209
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 210 of 478
5.3.4: Peak List of 2506-F
Pos. [°2Th.]
14.1442
19.0217
22.9889
24.4982
25.6027
27.3846
28.3651
31.6977
32.9903
35.1755
36.9808
38.4878
40.5512
40.6035
42.9210
43.3892
44.7702
45.4214
45.5552
50.1940
51.7865
52.5136
53.8456
55.0741
Height [cts]
500.22
543.22
66.62
81.34
188.47
7238.35
22791.98
74557.24
285.00
375.80
3047.98
6644.22
14912.04
13626.94
3586.69
2386.69
9360.45
51264.29
31232.14
4680.78
1177.28
808.87
1858.05
77.50
FWHM
[°2Th.]
0.0492
0.1968
0.9446
0.2362
0.1574
0.0886
0.1771
0.1574
0.3149
0.1378
0.2362
0.1771
0.1440
0.0960
0.2400
0.1440
0.0960
0.1800
0.0840
0.0720
0.3840
0.2400
0.0840
0.2880
d-spacing [A]
6.26175
4.66572
3.86876
3.63371
3.47940
3.25691
3.14653
2.82291
2.71520
2.55137
2.43086
2.33908
2.22285
2.22563
2.10545
2.08381
2.02269
1.99519
1.99458
1.81609
1.76393
1.74120
1.70123
1.66615
Rel. Int. [%]
0.67
0.73
0.09
0.11
0.25
9.71
30.57
100.00
0.38
0.50
4.09
8.91
20.00
18.28
4.81
3.20
12.55
68.76
41.89
6.28
1.58
1.08
2.49
0.10
Matched by
01-074-1132;
00-022-1235
01-075-1862
01-077-2064
00-004-0587
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-074-1132;
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587
00-043-1022
01-075-1862
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
01-075-1862
01-077-2064
F-210
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 211 of 478
Pos. [°2Th.]
56.4383
56.6088
57.4512
58.6108
59.4041
62.2881
65.0737
65.3001
66.1467
66.3398
68.1870
68.5406
73.0032
73.6719
73.9149
75.2080
75.4290
77.3035
78.1993
82.4005
Height [cts]
14234.93
7065.04
289.16
1801.92
1135.33
1264.45
3499.82
4092.17
6529.17
6981.57
319.64
118.39
751.95
2271.24
1664.24
12578.65
7181.86
358.48
1619.84
536.91
FWHM
[°2Th.]
0.1560
0.1080
0.3360
0.0960
0.4320
0.1200
0.2640
0.1440
0.0840
0.0600
0.1680
0.7680
0.1440
0.0840
0.1200
0.1560
0.1200
0.3840
0.2160
0.2400
d-spacing [A]
1.62907
1.62861
1.60273
1.57376
1.55462
1.48939
1.43220
1.43133
1.41155
1.41141
1.37420
1.36797
1.29496
1.28485
1.28122
1.26237
1.26235
1.23330
1.22140
1.16944
Rel. Int. [%]
19.09
9.48
0.39
2.42
1.52
1.70
4.69
5.49
8.76
9.36
0.43
0.16
1.01
3.05
2.23
16.87
9.63
0.48
2.17
0.72
Matched by
01-077-2064;
01-080-2171;
01-080-1385
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-077-2064;
01-075-1620
01-075-1862;
00-022-1235
01-074-1132
01-077-2064
00-004-0587;
00-022-1235
01-075-1862;
00-004-0587;
01-074-1132;
00-022-1235
01-077-2064
01-075-1862;
01-074-1132
01-074-1132;
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327;
00-022-1235
F-211
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 212 of 478
Pos. [°2Th.]
83.8950
84.1525
87.5990
87.9083
90.3207
90.6135
94.4353
94.7861
99.0772
101.0395
101.3699
101.7534
107.6610
108.0382
108.4854
Height [cts]
8044.99
4384.14
474.16
337.54
624.26
344.99
1155.34
814.48
304.56
2208.82
1742.00
519.96
684.04
231.46
223.21
FWHM
[°2Th.]
0.1680
0.1200
0.1200
0.1440
0.1440
0.1440
0.1920
0.1440
0.7680
0.1560
0.1680
0.1440
0.0960
0.1680
0.2400
d-spacing [A]
1.15237
1.15235
1.11293
1.10981
1.08633
1.08627
1.04954
1.04918
1.01243
0.99800
0.99564
0.99539
0.95420
0.95428
0.95159
Rel. Int. [%]
10.79
5.88
0.64
0.45
0.84
0.46
1.55
1.09
0.41
2.96
2.34
0.70
0.92
0.31
0.30
Matched by
01-077-2064
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
00-004-0587;
01-080-2172;
01-080-2173;
01-080-1385
00-022-1235
00-004-0587
00-004-0587
F-212
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 213 of 478
5.4: 2508-F-SC
5.4.1: Measurement Conditions of 2508-F
Dataset Name
File name
F-SC.udf
Sample Identification 2508-F-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
5.4.2: Main Graphics, Analyze View of 2508-F
2508-F-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2508-
F-213
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 214 of 478
V V
50 60 70
Position [°2Theta] (Copper (Cu))
V V V V
40000 -
30000 -
20000 -
10000 -
2508-F-SC
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565
Aluminum (01 -085-1 327)
• Periclase, syn (00-043-1 022)
L
96)
,
u ,
I
ivi
1111
i
1 III I
I
1
1 t I
LJ_iiAuLjjliMiiUiUiAWii_J: i_Aj .rii
11
Aluminum Oxide Nitride 17%
Aluminum Oxide 15 %
Aluminum Oxide Nitride 11 %|
Aluminum Oxide Nitride '3 % \
| Magnesium Aluminum Oxide 7 % |
| Sodium Chloride 19 %\
\ Periclase, syn 1 % |
I ! ,-, ,^_ _.._ .-. .-.,
J Fluorite, syn 2 % |=<
| .".luiiiii lui 11 imiiiuc J '"^:i |
Aluminum Oxide 4 %
Sylv Anhydrite 4%
F-214
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 215 of 478
5.4.3: Pattern List of 2508-F
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
34
41
56
51
31
13
12
14
33
29
26
18
17
11
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
4
5
19
7
3
17
11
8
2
1
2
2
4
15
Matched
Lines
17
10
9
14
9
12
12
12
5
7
6
14
34
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-215
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 216 of 478
5.4.4: Peak List of 2508-F
Pos. [°2Th.]
18.9985
23.0884
24.4847
25.5509
27.3100
28.3345
30.6482
31.2579
31.6685
33.2106
35.1155
35.1850
36.0279
36.8197
37.7556
38.4920
40.4909
41.7115
42.9130
43.3323
44.8254
45.4157
45.5249
46.9812
47.3226
50.1909
50.3146
52.5343
53.8245
Height [cts]
1202.02
33.59
113.71
1471.24
3991.90
13366.79
733.17
2585.51
47285.34
1502.27
2654.03
2786.04
1248.52
5453.08
2270.19
4289.70
7852.48
234.38
1459.60
3447.56
6033.44
32345.72
23375.21
489.76
431.10
2791.25
2210.94
1452.90
1122.15
FWHM
[°2Th.]
0.1279
0.2362
0.1574
0.0590
0.1476
0.1574
0.1574
0.0984
0.1574
0.1968
0.0840
0.0689
0.1378
0.0886
0.0787
0.1673
0.1476
0.2362
0.1181
0.0886
0.0689
0.1560
0.1200
0.1920
0.1920
0.1200
0.0960
0.1200
0.0720
d-spacing [A]
4.67136
3.85230
3.63569
3.48635
3.26564
3.14986
2.91714
2.86162
2.82545
2.69769
2.55347
2.55070
2.49294
2.44113
2.38274
2.33883
2.22787
2.16545
2.10757
2.08814
2.02200
1.99542
1.99584
1.93252
1.91937
1.81620
1.81652
1.74056
1.70185
Rel. Int. [%]
2.54
0.07
0.24
3.11
8.44
28.27
1.55
5.47
100.00
3.18
5.61
5.89
2.64
11.53
4.80
9.07
16.61
0.50
3.09
7.29
12.76
68.41
49.43
1.04
0.91
5.90
4.68
3.07
2.37
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064;
01-080-2171
01-075-1620
01-075-1862
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
01-075-1862
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-086-2270
00-004-0864
01-086-2270
00-004-0587;
01-080-2173;
00-022-1235
01-075-1862
01-077-2064
F-216
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 217 of 478
Pos. [°2Th.]
55.6627
56.4314
56.5715
57.5076
57.6638
58.6427
59.3288
61.3008
62.2715
62.4791
65.2432
65.4017
66.1936
66.3707
68.2043
68.3891
71.4445
72.5389
73.0499
73.7148
73.9509
75.2366
75.4892
76.8825
77.2933
78.2753
78.4997
79.5233
80.6531
82.6651
83.9578
84.2225
Height [cts]
701.66
9962.85
6619.78
3281.29
1902.93
1541.03
3144.83
401.03
582.96
553.18
5898.64
5029.96
6032.36
6208.49
1958.61
1221.52
434.09
203.58
640.74
1856.39
1206.83
10158.39
5401.76
775.80
893.07
1370.38
984.07
84.59
189.87
657.52
6799.55
3657.36
FWHM
[°2Th.]
0.1200
0.1440
0.1200
0.0960
0.0960
0.1440
0.0840
0.1200
0.1440
0.1440
0.0720
0.1440
0.1200
0.0960
0.1680
0.1080
0.2880
0.2880
0.1200
0.1080
0.1440
0.1560
0.1320
0.1440
0.2400
0.1920
0.1440
0.2880
0.1440
0.4800
0.1680
0.1080
d-spacing [A]
1.64992
1.62926
1.62959
1.60130
1.60130
1.57298
1.55641
1.51099
1.48974
1.48529
1.42889
1.42581
1.41066
1.41082
1.37389
1.37403
1.31933
1.30210
1.29424
1.28421
1.28069
1.26196
1.26149
1.23900
1.23343
1.22040
1.22050
1.20435
1.19031
1.16636
1.15166
1.15157
Rel. Int. [%]
1.48
21.07
14.00
6.94
4.02
3.26
6.65
0.85
1.23
1.17
12.47
10.64
12.76
13.13
4.14
2.58
0.92
0.43
1.36
3.93
2.55
21.48
11.42
1.64
1.89
2.90
2.08
0.18
0.40
1.39
14.38
7.73
Matched by
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-086-2270
01-077-2064
01-075-1862;
00-022-1235
01-075-1620;
01-086-2270
01-075-1620
01-077-2064
00-004-0587;
00-022-1235
01-077-2064
01-075-1862
01-075-1862;
01-074-1132
01-074-1132;
01-085-1327
01-075-1862
01-074-1132;
01-086-2270
01-077-2064
F-217
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 218 of 478
Pos. [°2Th.]
85.7945
86.4223
87.6751
89.0177
89.2933
90.3667
90.6586
91.2014
94.1543
94.5411
94.8677
95.2434
95.5234
99.3588
101.1370
101.4579
103.4291
107.7237
108.1339
108.6137
109.8151
Height [cts]
119.60
159.92
401.47
158.41
113.60
474.07
354.95
441.67
931.81
1393.03
957.83
878.38
486.35
454.71
2302.10
1691.47
51.49
855.30
644.89
811.28
1666.63
FWHM
[°2Th.]
0.3840
0.3840
0.1440
0.1920
0.1440
0.1080
0.1440
0.2400
0.2160
0.1440
0.1440
0.1440
0.1680
0.2400
0.1800
0.1200
0.5760
0.1680
0.1440
0.1920
0.0480
d-spacing [A]
1.13165
1.12503
1.11216
1.09883
1.09887
1.08590
1.08316
1.07812
1.05193
1.04865
1.04849
1.04276
1.04303
1.01031
0.99730
0.99748
0.98136
0.95382
0.95370
0.94847
0.94143
Rel. Int. [%]
0.25
0.34
0.85
0.34
0.24
1.00
0.75
0.93
1.97
2.95
2.03
1.86
1.03
0.96
4.87
3.58
0.11
1.81
1.36
1.72
3.52
Matched by
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-022-1235
00-043-1022;
00-004-0864
00-004-0587
00-004-0587
00-043-1022
F-218
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 219 of 478
5.5: 2510-F-SC
5.5.1: Measurement Conditions of 2510-F
Dataset Name
File name
F-SC.udf
Sample Identification 2510-F-SC NO COVER
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2510-F-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2510-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
10.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
5.5.2: Main Graphics, Analyze View of 2510-F
F-219
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 220 of 478
V V
2510-F-SC
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565
_ Aluminum (01-085-1327)
Periclase, syn (00-043-1022)
50 60 70 80
Position [°2Theta] (Copper (Cu))
| Magnesium Aluminum Oxide 11.9 %
Aluminum Oxide Nitride 10.9 %
Aluminum Oxide 8.9 %
Sylvite, syn 7.9 %
Aluminum Oxide Nitride 6.9 %
Anhydrite 5.9 %
Sodium Chloride 21.3 %|
Elpasolite, syn 3 % |
Periclase, syn 4 % ]
Aim Aluminum 3 % [\
I Alurrl Aluminum Oxide 5 % |&~
F-220
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 221 of 478
5.5.3: Pattern List of 2510-F
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-022-
1235
01-086-
2270
01-080-
1385
Score
49
51
49
49
32
17
19
20
38
37
24
14
19
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
5
8
22
12
5
11
7
6
3
4
3
6
9
Matched
Lines
19
10
9
15
10
13
13
12
5
8
16
33
13
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
F-221
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 222 of 478
5.5.4: Peak List of 2510-F
Pos. [°2Th.]
10.9694
18.0663
19.0343
24.5358
25.5947
27.3776
28.4092
29.4271
31.7275
33.2477
34.4150
35.1561
35.2103
36.0501
36.9149
37.8289
38.5369
40.5666
40.6652
42.9538
43.3945
44.8601
45.4545
49.8421
Height [cts]
19.39
84.48
1147.14
55.47
771.99
3264.60
12475.85
330.25
38538.18
1670.97
300.20
1459.54
1671.17
1397.87
6066.86
1936.00
3042.66
6639.73
6621.93
3372.68
2289.28
5367.20
23181.09
569.57
FWHM
[°2Th.]
0.9446
0.2362
0.0689
0.1574
0.0787
0.1279
0.1673
0.1574
0.2066
0.1771
0.2362
0.0960
0.0590
0.1771
0.1181
0.1968
0.1279
0.0600
0.0886
0.0886
0.0984
0.2558
0.1673
0.1574
d-spacing [A]
8.06592
4.91025
4.66266
3.62823
3.48047
3.25774
3.14174
3.03534
2.82032
2.69476
2.60598
2.55062
2.54892
2.49145
2.43505
2.37829
2.33621
2.22205
2.21872
2.10566
2.08529
2.02051
1.99546
1.82960
Rel. Int. [%]
0.05
0.22
2.98
0.14
2.00
8.47
32.37
0.86
100.00
4.34
0.78
3.79
4.34
3.63
15.74
5.02
7.90
17.23
17.18
8.75
5.94
13.93
60.15
1.48
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
00-004-0587;
01-086-2270
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-080-2171;
01-086-2270;
01-080-1385
01-075-1620;
01-080-2171;
F-222
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 223 of 478
Pos. [°2Th.]
Height [cts]
FWHM
[°2Th.]
d-spacing [A]
Rel. Int. [%]
Matched by
01-080-2172;
01-080-1385
50.1992
50.3456
52.5733
53.8768
55.0029
55.7313
56.4868
56.6463
57.5504
57.6994
58.6630
59.4424
61.3196
62.3391
65.2624
65.4649
66.2194
66.5772
68.2387
69.7496
71.4258
1668.89
2047.65
902.67
836.01
230.13
634.90
6888.85
3588.73
2147.35
1334.76
1331.13
3533.29
380.69
1923.62
5802.69
5221.00
4981.36
3886.87
1270.48
230.90
675.42
0.1080
0.1574
0.0984
0.1771
0.2362
0.2362
0.1800
0.0960
0.1320
0.0720
0.1440
0.2400
0.1440
0.2640
0.0960
0.1440
0.1200
0.1680
0.1680
0.2880
0.2880
1.81591
1.81248
1.74081
1.70173
1.66952
1.64942
1.62779
1.62762
1.60021
1.60040
1.57248
1.55371
1.51057
1.48829
1.42852
1.42459
1.41017
1.40346
1.37328
1.34718
1.31963
4.33
5.31
2.34
2.17
0.60
1.65
17.88
9.31
5.57
3.46
3.45
9.17
0.99
4.99
15.06
13.55
12.93
10.09
3.30
0.60
1.75
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235
00-004-0587;
00-022-1235
01-075-1862
01-077-2064
01-074-1132;
01-086-2270
01-077-2064;
01-080-2171
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
01-086-2270
00-004-0587;
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620;
01-080-2171
01-075-1620;
01-080-2173;
01-086-2270
F-223
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 224 of 478
Pos. [°2Th.]
73.0641
73.7235
73.9586
75.2961
75.5193
76.9070
77.3890
78.2496
78.6713
80.7201
82.6947
83.9939
84.2559
85.8663
86.4529
87.7388
89.0481
90.4274
91.0669
94.1100
94.5417
95.3135
95.5953
99.3990
101.1326
101.5207
104.8529
105.9477
107.7967
109.8246
Height [cts]
550.21
1285.16
1388.73
7031.92
3490.74
614.28
873.21
1194.23
945.72
200.32
683.98
4239.21
2130.40
150.39
162.54
222.69
135.33
299.70
307.97
983.20
1207.47
888.74
435.56
522.51
1411.02
965.83
93.00
170.79
657.51
2158.22
FWHM
[°2Th.]
0.1920
0.1680
0.2400
0.1320
0.1320
0.1440
0.3840
0.1920
0.2400
0.1440
0.1920
0.1440
0.1200
0.2880
0.3840
0.6720
0.1920
0.1920
0.3840
0.2160
0.1920
0.0960
0.1440
0.2400
0.1920
0.1440
0.5760
0.5760
0.1440
0.0720
d-spacing [A]
1.29403
1.28408
1.28057
1.26111
1.26106
1.23866
1.23215
1.22074
1.21525
1.18949
1.16602
1.15126
1.15120
1.13089
1.12471
1.11152
1.09853
1.08533
1.07936
1.05231
1.04864
1.04218
1.04244
1.01001
0.99733
0.99704
0.97190
0.96485
0.95337
0.94137
Rel. Int. [%]
1.43
3.33
3.60
18.25
9.06
1.59
2.27
3.10
2.45
0.52
1.77
11.00
5.53
0.39
0.42
0.58
0.35
0.78
0.80
2.55
3.13
2.31
1.13
1.36
3.66
2.51
0.24
0.44
1.71
5.60
Matched by
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
01-074-1132
01-077-2064
01-075-1862;
01-086-2270
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-080-2171;
00-043-1022;
01-086-2270
01-075-1862
01-074-1132;
01-086-2270
01-077-2064;
01-086-2270
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-022-1235
00-043-1022
00-004-0587
00-043-1022
00-043-1022
F-224
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 225 of 478
F-225
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 226 of 478
FACILITY H
6.1: 2046-H-SC
6.1.1: Measurement Conditions of 2046-H
Dataset Name
File name
Sample Identification
Comment
2046-H-SC, no cover
D:\SAP\2046-H-SC, no cover.sd
2046-H-SC, no cover
Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 9/27/2010 4:03:00 PM
Raw Data Origin PHILIPS-binary (scan) (.SD)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 20.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 0.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPert MPD
Diffractometer Number 1
Goniometer Radius [mm] 200.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning Yes
6.1.2: Main Graphics, Analyze View of 2046-H
F-226
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 227 of 478
V V
2046-H-SC, no cover
• Aluminum Oxide (01-075-1865;
• Potassium Chloride (01-075-0;
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
, , Lj
imm
20 30 40 50 60 70 80
Position [°2Theta] (Copper (Cu))
100 110
Aluminum Oxide Nitride 10 %"| I Aluminum Nitride 10 % |
Aluminum Oxide 10 %
Aluminum Oxide 9 %
Magnesium Aluminum Qxide 9 %
sodium Chloride 16 %\
Sylvite, syn 9 % |
Aluminum Oxide Nitride 5 % |
Alumirl Fluurite, syn 5 % JT|
6.1.3: Pattern List of 2046-H
F-227
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Ref. Code
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 228 of 478
Score Compound Chemical SemiQuant Matched Strong
Name Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
54
49
51
48
55
19
20
20
26
17
17
19
22
15
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
10
9
16
9
10
10
6
5
2
5
3
5
9
1
22
10
9
14
11
12
11
11
5
5
13
38
12
18
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-228
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 229 of 478
6.1.4: Peak List of 2046-H
Pos. [°2Th.]
16.4748
19.1387
20.9852
23.2412
25.6315
26.7539
27.4351
28.4510
31.7722
33.2970
33.3567
35.2212
36.0993
36.9913
38.0153
38.6174
40.5850
40.6777
41.8989
43.4169
44.9242
45.4780
45.5989
47.0689
49.8215
50.2326
Height [cts]
81.83
1521.76
195.92
455.83
1961.53
711.68
3491.37
19480.03
36520.83
6838.22
6072.16
4607.44
4736.92
7206.42
5766.71
1778.33
12019.13
11576.22
1828.97
7283.36
8525.01
25957.25
20037.27
2271.43
3096.63
4807.98
FWHM
[°2Th.]
0.4723
0.0689
0.1968
0.3149
0.0590
0.0787
0.0787
0.1968
0.1673
0.1440
0.0360
0.1080
0.1200
0.3360
0.1080
0.1680
0.0960
0.1080
0.3840
0.0840
0.1680
0.1440
0.0960
0.2400
0.1920
0.0960
d-spacing [A]
5.38081
4.63746
4.23338
3.82732
3.47556
3.33225
3.25103
3.13722
2.81646
2.68866
2.69065
2.54606
2.48611
2.42818
2.36510
2.32959
2.22108
2.21623
2.15442
2.08254
2.01611
1.99284
1.99277
1.92912
1.82880
1.81479
Rel. Int. [%]
0.22
4.17
0.54
1.25
5.37
1.95
9.56
53.34
100.00
18.72
16.63
12.62
12.97
19.73
15.79
4.87
32.91
31.70
5.01
19.94
23.34
71.08
54.87
6.22
8.48
13.17
Matched by
01-074-1132;
01-086-2270
01-085-0930
01-075-1862
01-085-0930
01-077-2064
00-004-0587;
00-004-0864;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132
01-075-1620
01-074-1132;
01-085-1327;
01-086-2270
00-004-0587
00-004-0587;
01-086-2270
01-075-1862;
01-086-2270
01-074-1132
01-077-2064;
01-080-2171;
01-080-2172;
01-086-2270;
01-080-1385
00-004-0864
01-075-1620;
01-080-2171;
01-080-2172;
01-080-1385
00-004-0587;
01-080-2173;
F-229
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 230 of 478
Pos. [°2Th.]
Height [cts]
FWHM
[°2Th.]
d-spacing [A]
Rel. Int. [%]
Matched by
00-022-1235;
01-085-0930
52.5861
53.8941
55.7338
56.5072
56.6772
57.5470
57.7088
58.6765
59.3827
59.5540
61.3612
65.3366
66.2258
66.4389
66.5966
68.2452
68.4360
69.7391
71.4206
72.6220
73.7320
73.9490
75.2671
75.4989
2798.93
1034.15
631.48
6988.29
3534.84
4579.54
2474.38
1588.22
5232.90
4982.68
699.29
4338.21
6101.62
6448.83
4682.26
2331.23
1221.39
424.94
1875.84
830.58
1973.92
1498.88
6100.75
3476.91
0.1920
0.1440
0.2880
0.1440
0.0960
0.1440
0.1440
0.1920
0.2400
0.1440
0.1200
0.2640
0.1200
0.0840
0.0960
0.1440
0.1200
0.2400
0.2400
0.2640
0.1680
0.1440
0.1320
0.1320
1.73897
1.69981
1.64798
1.62725
1.62680
1.60029
1.60016
1.57215
1.55513
1.55492
1.50964
1.42707
1.41005
1.40954
1.40310
1.37317
1.37321
1.34736
1.31971
1.30081
1.28395
1.28390
1.26153
1.26135
7.66
2.83
1.73
19.14
9.68
12.54
6.78
4.35
14.33
13.64
1.91
11.88
16.71
17.66
12.82
6.38
3.34
1.16
5.14
2.27
5.40
4.10
16.70
9.52
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064;
01-080-2171;
01-080-1385
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862
01-074-1132;
01-086-2270
00-004-0587;
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-075-1620;
01-080-2171
01-075-1620;
01-080-2173;
01-086-2270
01-075-1620
00-004-0587;
00-022-1235
01-077-2064
F-230
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 231 of 478
Pos. [°2Th.]
76.8793
77.5282
78.2986
80.6599
81.0708
82.7867
83.9516
84.2228
86.4027
87.6745
87.9273
88.9757
90.3437
90.6556
91.1441
94.5166
94.7986
95.1860
98.2940
99.5697
101.0890
101.4174
104.7427
107.7151
108.0901
108.5642
Height [cts]
994.21
735.60
512.45
273.97
288.31
319.64
3865.61
2090.23
212.95
410.04
310.02
251.97
254.90
233.08
481.97
1624.78
1606.84
1272.35
289.58
309.55
1835.19
1416.46
117.20
265.93
89.56
193.48
FWHM
[°2Th.]
0.1440
0.4800
0.1440
0.1920
0.3840
0.5760
0.1680
0.1080
0.3840
0.1680
0.1920
0.1920
0.1200
0.1440
0.1680
0.2400
0.1920
0.1200
0.1920
0.7680
0.1680
0.1920
0.4800
0.1200
0.1440
0.1920
d-spacing [A]
1.23904
1.23028
1.22009
1.19022
1.18523
1.16496
1.15173
1.15157
1.12524
1.11216
1.10962
1.09924
1.08611
1.08319
1.07865
1.04885
1.04648
1.04583
1.01839
1.00874
0.99764
0.99777
0.97262
0.95387
0.95396
0.94876
Rel. Int. [%]
2.72
2.01
1.40
0.75
0.79
0.88
10.58
5.72
0.58
1.12
0.85
0.69
0.70
0.64
1.32
4.45
4.40
3.48
0.79
0.85
5.03
3.88
0.32
0.73
0.25
0.53
Matched by
01-075-1862;
01-086-2270
01-074-1132;
01-086-2270;
01-085-0930
01-074-1132;
01-085-1327
01-075-1862
01-075-1620;
01-085-0930
01-074-1132;
01-086-2270
01-077-2064;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
01-080-2173
01-075-1862
00-022-1235
00-022-1235
00-004-0587
00-004-0587
F-231
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 232 of 478
6.2: 2544-H-SC
6.2.1: Measurement Conditions of 2544-H
Dataset Name
File name
H-SC.udf
Sample Identification 2544-H-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
2544-H-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2544-
F-232
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 23 3 of 478
6.2.2: Main Graphics, Analyze View of 2544-H
2544-H-SC
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
96)
i li
50 60 70 80
Position [°2Theta] (Copper (Cu))
Aluminum Oxide Nitride 11.2 %
sodium Chloride 1S.4 %|
Quartz 1 %
'.-.fctlUILt! I 'A)
Aluminum Oxide Nitride 7.1 %|
Magnesium Aluminum Oxide 7.1 % |
i, ,>T-.,r-., ...T-. ,• v..-,.-j.-. Nitride 5.1
Aluminum 1 % |
inyunitj D.I :•'•:•
Fluorite, syn 6.1 % |
6.2.3: Pattern List of 2544-H
F-233
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 234 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
01-085-
0930
51
52
52
49
52
15
15
18
39
24
21
18
13
13
5
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
8
10
18
7
7
11
7
5
1
6
2
5
9
1
1
20
10
9
14
10
13
12
12
5
6
15
36
12
19
18
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
6.2.4: Peak List of 2544-H
F-234
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 23 5 of 478
Pos. [°2Th.]
16.2741
18.9841
23.0711
24.4870
25.5456
26.6018
27.2985
28.3179
29.4181
31.6538
33.2057
35.0986
36.0093
36.8244
37.7235
37.8860
38.4867
40.5062
40.5861
41.8025
43.2996
44.7567
45.3893
45.5283
Height [cts]
35.25
935.36
59.34
86.25
1534.15
433.06
2849.23
16571.75
362.53
30659.65
3736.59
3099.12
2767.23
4481.50
2837.20
3385.89
1828.36
11060.23
9346.78
676.17
3407.58
3297.82
20587.23
12271.99
FWHM
[°2Th.]
0.3149
0.1771
0.3149
0.2755
0.1574
0.1181
0.0984
0.1574
0.2362
0.1771
0.1968
0.1574
0.1771
0.0590
0.1440
0.1771
0.0689
0.1680
0.0840
0.4320
0.1680
0.2640
0.1440
0.1080
d-spacing [A]
5.44673
4.67488
3.85516
3.63534
3.48706
3.35096
3.26700
3.15167
3.03625
2.82672
2.69808
2.55678
2.49418
2.44082
2.38272
2.37484
2.33914
2.22522
2.22654
2.15916
2.08791
2.02326
1.99652
1.99570
Rel. Int. [%]
0.11
3.05
0.19
0.28
5.00
1.41
9.29
54.05
1.18
100.00
12.19
10.11
9.03
14.62
9.25
11.04
5.96
36.07
30.49
2.21
11.11
10.76
67.15
40.03
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132
01-075-1862;
01-075-1620;
01-080-2173
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587;
01-085-0930
01-075-1862
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
F-235
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 236 of 478
Pos. [°2Th.]
47.0005
49.8302
50.1688
50.2736
52.5164
53.8128
55.7461
56.4247
56.5861
57.4605
57.6248
58.6044
59.3253
59.4221
61.2761
65.2479
65.3710
66.1732
Height [cts]
604.22
1312.32
3509.51
2972.16
1513.30
734.55
592.34
6520.11
3613.99
3516.87
2028.35
1642.63
3796.09
3826.77
541.72
3768.47
4086.52
5373.75
FWHM
[°2Th.]
0.3360
0.1920
0.1200
0.1200
0.1200
0.1440
0.2880
0.1320
0.0600
0.1560
0.0720
0.1320
0.1440
0.1200
0.1680
0.1920
0.1680
0.1200
d-spacing [A]
1.93177
1.82849
1.81694
1.81340
1.74112
1.70219
1.64765
1.62943
1.62921
1.60250
1.60229
1.57392
1.55650
1.55419
1.51154
1.42880
1.42641
1.41105
Rel. Int. [%]
1.97
4.28
11.45
9.69
4.94
2.40
1.93
21.27
11.79
11.47
6.62
5.36
12.38
12.48
1.77
12.29
13.33
17.53
Matched by
00-004-0864;
01-086-2270;
01-086-2340
01-075-1620;
01-080-2171;
01-080-2172;
01-080-1385
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
00-004-0587;
00-022-1235;
01-085-0930
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-074-1132;
01-075-1620
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
01-074-1132;
01-086-2270
00-004-0587;
01-077-2064;
01-075-1620
66.3584
6398.17
0.0840
1.41106
20.87
F-236
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 237 of 478
Pos. [°2Th.]
68.1678
68.3664
69.7966
71.3780
72.5977
73.0395
73.7144
73.9082
75.2488
75.4685
76.8357
77.2803
78.2348
80.6465
81.0525
82.6744
83.9320
84.2028
86.5318
Height [cts]
2067.32
1260.98
295.00
1334.45
676.50
686.95
2358.20
1740.39
6843.19
3599.17
844.44
716.10
569.57
258.13
204.95
369.59
4428.34
2405.51
185.84
FWHM
[°2Th.]
0.1920
0.1200
0.4320
0.0960
0.2400
0.1440
0.1320
0.1200
0.1320
0.1320
0.1440
0.4800
0.2880
0.1920
0.2880
0.4800
0.1200
0.1320
0.4800
d-spacing [A]
1.37454
1.37443
1.34639
1.32040
1.30119
1.29440
1.28421
1.28451
1.26179
1.26179
1.23964
1.23361
1.22093
1.19039
1.18545
1.16625
1.15195
1.15179
1.12389
Rel. Int. [%]
6.74
4.11
0.96
4.35
2.21
2.24
7.69
5.68
22.32
11.74
2.75
2.34
1.86
0.84
0.67
1.21
14.44
7.85
0.61
Matched by
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-075-1620;
01-080-2171;
01-080-2172;
01-080-1385;
01-086-2340
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-075-1620;
01-086-2340
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-086-2340
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-075-1862;
01-086-2340
01-075-1620;
01-086-2340;
01-085-0930
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-086-2340;
01-085-0930
01-075-1862
F-237
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 23 8 of 478
Pos. [°2Th.]
87.6495
87.9418
88.9377
90.3547
90.6426
91.1428
94.5310
94.8289
95.2183
98.3242
99.3718
101.1071
101.4597
104.7300
107.7531
108.1347
108.5981
109.7971
Height [cts]
544.31
376.91
213.82
319.34
283.88
459.16
1657.65
1447.37
1086.36
207.94
264.06
1828.22
1534.91
72.02
615.89
549.35
882.95
1252.81
FWHM
[°2Th.]
0.1440
0.1440
0.1920
0.1680
0.1440
0.1920
0.1080
0.1440
0.1200
0.2880
0.7680
0.1680
0.1680
0.3840
0.1200
0.1440
0.2160
0.0480
d-spacing [A]
1.11242
1.11223
1.09961
1.08601
1.08331
1.07866
1.04873
1.04622
1.04556
1.01816
1.01022
0.99751
0.99747
0.97270
0.95364
0.95133
0.95091
0.94153
Rel. Int. [%]
1.78
1.23
0.70
1.04
0.93
1.50
5.41
4.72
3.54
0.68
0.86
5.96
5.01
0.23
2.01
1.79
2.88
4.09
Matched by
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-004-0587
F-238
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 23 9 of 478
6.3: 2555-H-SC
6.3.1: Measurement Conditions of 2555-H
Dataset Name
File name
H-SC.udf
Sample Identification 2555-H-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
6.3.2: Main Graphics, Analyze View of 2555-H
2555-H-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2555-
F-239
-------
V V
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 240 of 478
VV
V W V
2555-H-SC
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
K
frflnftf
50 60 70 80
Position [°2Theta] (Copper (Cu))
Sylvite,syn 9.9 % | | Sodium Chloride 11 .9 % |
^^^ | Aluminum Oxide 13. 9 %"|
Magnesium Aluminum Oxide 8.9 %
Nrtride
|
Aluminum Oxide 5.9 %|
Elpasolite, syn 3 % fc % |
Aluminum Oxide Nitride 5.9 % |
6.3.3: Pattern List of 2555-H
F-240
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 241 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
46
36
33
36
36
16
20
21
26
21
25
26
20
14
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
14
10
12
9
10
6
5
5
2
9
3
8
6
2
21
10
9
15
12
13
12
11
5
6
16
40
13
22
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-241
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 242 of 478
6.3.4: Peak List of 2555-H
Pos. [°2Th.]
16.2129
19.0277
21.6765
23.0390
24.4605
25.5167
26.5799
27.3061
28.2976
29.3564
31.6512
33.1715
35.0783
35.1413
35.9937
36.8083
37.8844
38.4428
39.2597
40.4851
40.5657
41.8271
43.2942
44.8099
45.3820
45.5031
Height [cts]
61.99
941.61
58.60
89.40
101.25
2296.59
357.49
2833.00
14619.11
409.12
30458.97
5792.04
4144.79
4428.18
3779.48
4052.91
4870.29
1447.80
429.00
9721.87
8662.00
762.11
5002.49
3333.31
20556.10
13356.11
FWHM
[°2Th.]
0.1968
0.2165
0.2362
0.2362
0.2362
0.0689
0.1181
0.1673
0.1673
0.1574
0.1181
0.0689
0.0720
0.0492
0.0590
0.2755
0.3149
0.1574
0.2362
0.1560
0.0840
0.3360
0.1080
0.2400
0.1560
0.0720
d-spacing [A]
5.46714
4.66426
4.09992
3.86044
3.63923
3.49094
3.35366
3.26611
3.15388
3.04249
2.82694
2.70078
2.55610
2.55378
2.49523
2.44185
2.37493
2.34171
2.29485
2.22633
2.22761
2.15795
2.08816
2.02098
1.99683
1.99675
Rel. Int. [%]
0.20
3.09
0.19
0.29
0.33
7.54
1.17
9.30
48.00
1.34
100.00
19.02
13.61
14.54
12.41
13.31
15.99
4.75
1.41
31.92
28.44
2.50
16.42
10.94
67.49
43.85
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-077-2064;
01-080-2171;
01-080-1385
01-075-1620
01-075-1862
01-075-1862
01-075-1620;
01-086-2340
01-074-1132
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-086-2340
00-004-0587
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327
01-077-2064;
01-086-2270
F-242
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 243 of 478
Pos. [°2Th.]
46.9814
49.7808
50.1461
50.2936
52.4810
53.8035
55.7190
56.4267
56.5760
57.4317
57.6130
58.6134
59.3154
60.6214
65.2332
66.1651
66.3563
Height [cts]
768.82
1813.66
3119.33
2297.19
2160.72
719.21
625.00
6327.52
3485.62
4835.67
2908.39
1558.38
4618.51
632.54
3268.60
6082.56
6642.55
FWHM
[°2Th.]
0.2880
0.2160
0.0840
0.1200
0.1080
0.1200
0.2400
0.1320
0.0840
0.1680
0.1200
0.1200
0.2400
0.2880
0.1200
0.1200
0.1920
d-spacing [A]
1.93251
1.83019
1.81772
1.81273
1.74221
1.70246
1.64838
1.62938
1.62947
1.60323
1.60259
1.57369
1.55673
1.52628
1.42909
1.41120
1.40760
Rel. Int. [%]
2.52
5.95
10.24
7.54
7.09
2.36
2.05
20.77
11.44
15.88
9.55
5.12
15.16
2.08
10.73
19.97
21.81
Matched by
00-004-0864;
01-086-2270;
01-086-2340
01-075-1620;
01-080-2171
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
00-004-0587;
00-022-1235
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385;
01-086-2340
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
F-243
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 244 of 478
Pos. [°2Th.]
68.1372
68.3663
69.6863
71.3465
72.5788
73.0270
73.6748
73.9183
75.2278
75.4534
76.8271
77.1388
77.4524
78.2197
80.6222
81.0211
82.6276
83.9472
84.1626
86.2864
87.6408
Height [cts]
2825.04
1561.01
486.70
1854.66
925.39
699.22
2072.68
1476.24
6697.10
3617.75
1232.77
900.24
702.34
576.62
353.81
323.90
285.34
4168.92
2433.86
287.61
511.53
FWHM
[°2Th.]
0.0960
0.1200
0.2400
0.1920
0.3360
0.1440
0.0720
0.1200
0.1680
0.1320
0.0840
0.1920
0.1440
0.1920
0.1680
0.2880
0.3840
0.1680
0.1200
0.1920
0.1200
d-spacing [A]
1.37508
1.37444
1.34825
1.32090
1.30148
1.29459
1.28480
1.28117
1.26209
1.26200
1.23975
1.23552
1.23436
1.22113
1.19069
1.18583
1.16680
1.15178
1.15224
1.12646
1.11251
Rel. Int. [%]
9.27
5.12
1.60
6.09
3.04
2.30
6.80
4.85
21.99
11.88
4.05
2.96
2.31
1.89
1.16
1.06
0.94
13.69
7.99
0.94
1.68
Matched by
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620;
01-086-2340
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-075-1620;
01-086-2340
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-086-2340
00-004-0587;
01-074-1132;
00-022-1235
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-075-1862;
01-086-2340
01-075-1620;
01-086-2340
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-086-2340
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
F-244
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 245 of 478
Pos. [°2Th.]
88.9924
90.3295
90.6507
91.1371
94.5337
94.8409
95.1980
95.5193
98.3182
99.3751
101.1008
101.4735
104.7802
107.7294
108.0997
108.6081
109.0126
109.7994
Height [cts]
375.10
279.33
276.42
550.77
1664.85
1712.98
1530.79
757.63
309.23
227.41
2175.52
1528.53
210.73
707.64
626.63
932.57
844.37
1284.43
FWHM
[°2Th.]
0.1920
0.1440
0.1440
0.1440
0.1440
0.1680
0.2640
0.1440
0.3360
0.3840
0.0720
0.1920
0.5760
0.1200
0.1440
0.1200
0.1920
0.0360
d-spacing [A]
1.09907
1.08625
1.08323
1.07872
1.04871
1.04612
1.04314
1.04306
1.01820
1.01019
0.99756
0.99737
0.97237
0.95378
0.95154
0.94850
0.94846
0.94152
Rel. Int. [%]
1.23
0.92
0.91
1.81
5.47
5.62
5.03
2.49
1.02
0.75
7.14
5.02
0.69
2.32
2.06
3.06
2.77
4.22
Matched by
01-075-1862
00-022-1235
00-022-1235
00-004-0587
00-004-0587
F-245
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 246 of 478
6.4: 2559-H-SC
6.4.1: Measurement Conditions of 2559-H
Dataset Name
File name
H-SC.udf
Sample Identification 2559-H-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
6.4.2: Main Graphics, Analyze View of 2559-H
2559-H-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2559-
F-246
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 247 of 478
V VV V V
2559-H-SC
I Aluminum Oxide (01-075-1865
I Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
96)
Position [°2"meta] (Copper (Cu))
Magnesium Aluminum Oxide 9.9 %
Aluminum Oxide Nitride 8.9 %
Sylvite, syn 10.9 % |
Sodium Chloride 15.5 % |
I Elpasolite. svn 3
Aluminum 2 %
Anhydrite 5.9 %
Aluminum Oxide Nitride 5.9 %|
F-247
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 248 of 478
6.4.3: Pattern List of 2559-H
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
52
53
47
53
52
15
21
22
34
24
24
23
18
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
9
11
16
10
9
9
6
5
2
8
3
6
7
Matched
Lines
21
10
9
15
12
12
12
11
5
7
15
40
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
F-248
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 249 of 478
6.4.4: Peak List of 2559-H
Pos. [°2Th.]
16.2868
19.0058
23.0794
24.5074
25.5530
26.6502
27.3489
28.3798
29.5809
31.2914
31.6929
31.7474
33.2198
35.1564
36.0485
36.9127
37.7892
37.9298
38.5343
40.5670
41.8325
43.3520
44.8969
45.4331
Height [cts]
33.91
1126.17
65.88
84.57
1245.87
210.70
2407.18
14358.28
287.56
2330.61
25646.05
21958.13
3955.02
2945.16
2972.55
5525.10
3070.86
3262.90
1740.88
9641.07
908.64
3133.37
4257.67
17639.97
FWHM
[°2Th.]
0.2362
0.0787
0.2362
0.2362
0.0787
0.1181
0.0984
0.1476
0.2362
0.1181
0.1200
0.0360
0.1320
0.0960
0.2640
0.1080
0.1680
0.1440
0.0960
0.1920
0.2880
0.1440
0.2880
0.1320
d-spacing [A]
5.44250
4.66958
3.85378
3.63237
3.48605
3.34498
3.26109
3.14493
3.01991
2.85863
2.82098
2.82326
2.69473
2.55060
2.48950
2.43317
2.37872
2.37023
2.33443
2.22202
2.15768
2.08551
2.01727
1.99470
ReLIntM
0.13
4.39
0.26
0.33
4.86
0.82
9.39
55.99
1.12
9.09
100.00
85.62
15.42
11.48
11.59
21.54
11.97
12.72
6.79
37.59
3.54
12.22
16.60
68.78
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132
01-075-1862;
01-075-1620
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-080-2171;
01-086-2270
45.5788
9306.39
0.1080
1.99360
36.29
F-249
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 250 of 478
Pos. [°2Th.]
47.0024
47.3326
49.8164
50.1951
52.5588
53.8567
55.7192
56.4562
56.6193
57.5101
57.6588
58.6603
59.3644
60.6178
61.3124
65.2901
65.4584
66.2007
66.4188
68.2273
68.4081
Height [cts]
605.28
582.18
1327.97
3094.02
1375.85
637.98
624.97
5398.76
3087.71
3226.01
1985.77
1582.56
4135.33
741.92
535.00
4394.81
4753.23
5080.68
5788.29
1804.82
1115.79
FWHM
[°2Th.]
0.1920
0.1920
0.2400
0.2160
0.0840
0.1680
0.2880
0.1200
0.0960
0.1440
0.0960
0.1080
0.2880
0.3360
0.1920
0.1200
0.1680
0.0960
0.1200
0.0720
0.0720
d-spacing [A]
1.93170
1.91899
1.82897
1.81606
1.73981
1.70091
1.64838
1.62860
1.62833
1.60123
1.60143
1.57255
1.55557
1.52637
1.51073
1.42798
1.42471
1.41053
1.40642
1.37348
1.37370
Rel. Int. [%]
2.36
2.27
5.18
12.06
5.36
2.49
2.44
21.05
12.04
12.58
7.74
6.17
16.12
2.89
2.09
17.14
18.53
19.81
22.57
7.04
4.35
Matched by
00-004-0864;
01-086-2270
01-086-2270
01-075-1620;
01-080-2171;
01-080-1385
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-086-2270
00-004-0587;
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235
F-250
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 251 of 478
Pos. [°2Th.]
69.7277
71.4000
72.5746
73.7344
75.2769
75.4928
76.8908
77.4671
78.2743
80.6936
82.7096
83.9588
84.2094
86.4091
87.6448
88.9982
90.4029
90.6879
91.1810
94.5511
95.2649
95.5638
98.3264
99.4302
101.1213
101.4956
104.7758
107.7752
108.6391
109.0581
109.7991
Height [cts]
338.80
1356.23
761.56
2130.76
5811.09
3212.94
909.25
783.36
601.92
267.57
416.66
3760.38
2034.45
216.13
461.06
215.51
250.72
248.54
454.42
1751.69
1104.85
541.33
232.82
339.23
1690.63
1372.11
148.96
711.57
986.76
852.74
1204.45
FWHM
[°2Th.]
0.1920
0.1920
0.4320
0.1920
0.1440
0.1080
0.0840
0.1920
0.2880
0.1920
0.2880
0.1200
0.1320
0.3840
0.1920
0.1440
0.1440
0.1440
0.1920
0.1680
0.1200
0.1440
0.2880
0.5760
0.1920
0.2160
0.6720
0.1680
0.1920
0.1920
0.0360
d-spacing [A]
1.34755
1.32004
1.30154
1.28391
1.26139
1.26144
1.23888
1.23110
1.22041
1.18981
1.16585
1.15165
1.15172
1.12517
1.11247
1.09902
1.08556
1.08289
1.07831
1.04856
1.04258
1.04270
1.01814
1.00978
0.99741
0.99474
0.97240
0.95350
0.94831
0.94819
0.94152
Rel. Int. [%]
1.32
5.29
2.97
8.31
22.66
12.53
3.55
3.05
2.35
1.04
1.62
14.66
7.93
0.84
1.80
0.84
0.98
0.97
1.77
6.83
4.31
2.11
0.91
1.32
6.59
5.35
0.58
2.77
3.85
3.33
4.70
Matched by
01-074-1132;
01-075-1620;
01-080-2171
01-075-1620;
01-080-2173;
01-086-2270
01-075-1620
00-004-0587;
00-022-1235
01-077-2064
01-075-1862;
01-086-2270
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-075-1862
01-074-1132;
01-086-2270
01-077-2064
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-022-1235
00-004-0587
00-004-0587
00-004-0587
F-251
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 252 of 478
6.5: 2568-H-SC
6.5.1: Measurement Conditions of 2568-H
Dataset Name
File name
H-SC, no cover.udf
Sample Identification 2568-H-SC, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2568-H-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2568-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
6.5.2: Main Graphics, Analyze View of 2568-H
F-252
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 253 of 478
2568-H-SC, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
50 60 70
Position [°2Theta] (Copper (Cu))
Sylvite,syn10?T| I Aluminum Oxide 12 % |
Aluminum Oxide Nitride 9 %
Aluminum Oxide 8 %
Magnesium Aluminum Oxide 8 %
Fluorite, syn 6 %
Aluminum Nitride 6 %
Sodium Chloride 15 %
rm
Periclase, syn 1 %
, ay 11 j -A.
Quartz low 4 % |
Anhydrite 5 % |
Alumirj Aluminum Oxide Nitride 5 % |
F-253
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 254 of 478
6.5.3: Pattern List of 2568-H
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0335
Score
57
55
56
52
50
15
19
18
31
8
21
21
21
18
13
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz low
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
12
10
15
8
6
9
6
5
2
1
6
3
5
8
4
Matched
Lines
22
10
9
14
11
12
12
11
5
5
6
13
38
12
18
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
1
0
0
0
0
0
F-254
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 255 of 478
6.5.4: Peak List of 2568-H
Pos. [°2Th.]
16.4673
18.9356
23.0051
25.4596
26.4988
27.2284
28.2244
31.5634
33.0828
35.0036
35.9153
36.7562
37.6375
37.7551
38.3521
40.3957
40.4563
41.6724
43.1978
44.6970
45.2820
45.4192
46.8242
49.6631
Height [cts]
44.39
1221.41
376.57
3203.47
194.26
3538.93
23968.65
35429.42
4365.47
6210.84
3252.96
6203.02
4620.16
4509.00
1901.62
15139.92
14423.37
1590.41
8970.76
8853.07
25914.17
16931.78
2508.25
2784.18
FWHM
[°2Th.]
0.9446
0.0886
0.4723
0.1082
0.1181
0.0689
0.1771
0.1673
0.1771
0.1082
0.1968
0.0886
0.1080
0.1574
0.0787
0.1320
0.0840
0.6720
0.1560
0.2640
0.1440
0.0840
0.2400
0.1440
d-spacing [A]
5.38325
4.68674
3.86607
3.49864
3.36375
3.27524
3.16189
2.83461
2.70782
2.56350
2.50050
2.44519
2.38796
2.38277
2.34704
2.23105
2.23339
2.16560
2.09260
2.02583
2.00101
2.00024
1.93863
1.83425
ReLIntM
0.13
3.45
1.06
9.04
0.55
9.99
67.65
100.00
12.32
17.53
9.18
17.51
13.04
12.73
5.37
42.73
40.71
4.49
25.32
24.99
73.14
47.79
7.08
7.86
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270
01-075-1862;
01-086-2270
01-085-0335
01-077-2064
00-004-0587;
00-004-0864
01-077-2064
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022;
01-085-0335
01-075-1862;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
01-075-1620;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0335
01-075-1862
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
01-075-1620
F-255
-------
Pos. [°2Th.] Height [cts]
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 256 of 478
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
50.0288
52.4517
53.7021
55.5382
56.3024
56.4781
57.3382
57.5095
58.5007
59.1943
61.1660
65.1468
65.2642
66.0460
66.2314
68.0013
68.2341
69.6129
5635.59
3720.19
1085.50
600.03
6537.91
3374.41
6189.44
3304.03
1854.44
4063.08
820.69
4257.08
4470.73
5251.10
7029.01
3029.19
1766.40
252.20
0.0960
0.0960
0.1200
0.3840
0.1560
0.1080
0.1440
0.0960
0.1680
0.2880
0.1680
0.2160
0.1680
0.0960
0.0840
0.0960
0.0960
0.3840
1.82170
1.74311
1.70544
1.65332
1.63268
1.63206
1.60563
1.60523
1.57646
1.55963
1.51399
1.43077
1.42848
1.41346
1.41345
1.37750
1.37677
1.34949
15.91
10.50
3.06
1.69
18.45
9.52
17.47
9.33
5.23
11.47
2.32
12.02
12.62
14.82
19.84
8.55
4.99
0.71
00-004-0587;
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0335
01-075-1862;
01-086-2270
01-077-2064
01-074-1132;
00-022-1235;
01-086-2270;
01-085-0335
01-077-2064
01-075-1862;
01-085-0335
00-004-0587
01-074-1132;
01-075-1620;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
01-085-0335
01-074-1132;
01-075-1620
F-256
-------
Pos. [°2Th.] Height [cts]
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 257 of 478
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
71.2617
72.4711
73.5321
73.7357
75.1005
75.3105
76.7007
76.9778
78.1130
80.5525
82.5717
83.7895
84.0487
86.2496
87.4887
88.8070
90.1990
90.4952
90.9673
94.3655
94.6718
95.0169
1134.65
553.95
2217.13
1905.86
5651.03
3326.66
1282.31
1046.26
488.41
354.18
321.53
3555.69
2090.44
254.95
484.63
367.88
273.78
267.49
517.53
1579.54
1401.45
1357.42
0.2400
0.3360
0.1080
0.1440
0.1200
0.0840
0.1440
0.1920
0.2400
0.1440
0.5760
0.1440
0.1200
0.4800
0.1920
0.1920
0.1200
0.1440
0.2880
0.2400
0.1440
0.1200
1.32226
1.30315
1.28694
1.28389
1.26391
1.26404
1.24148
1.23770
1.22253
1.19154
1.16744
1.15355
1.15351
1.12684
1.11405
1.10089
1.08748
1.08469
1.08029
1.05013
1.05015
1.04465
3.20
1.56
6.26
5.38
15.95
9.39
3.62
2.95
1.38
1.00
0.91
10.04
5.90
0.72
1.37
1.04
0.77
0.75
1.46
4.46
3.96
3.83
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620
00-004-0587;
00-022-1235;
01-085-0335
00-004-0587;
00-022-1235
01-077-2064
01-075-1862
01-075-1862;
01-086-2270
01-085-1327;
00-022-1235
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-085-0335
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0335
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-004-0587;
00-004-0864
F-257
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 258 of 478
Pos. [°2Th.]
95.3872
98.1651
99.2892
100.9263
101.2999
103.2325
104.6721
107.5767
108.4034
109.8079
109.8921
Height [cts]
608.19
223.76
308.68
1778.52
1414.12
67.41
67.80
393.98
571.96
1997.74
1554.86
FWHM
[°2Th.]
0.1440
0.3360
0.4800
0.1920
0.2160
0.5760
0.7680
0.1200
0.2400
0.1080
0.0600
d-spacing [A]
1.04416
1.01938
1.01083
0.99881
0.99614
0.98269
0.97308
0.95471
0.94972
0.94147
0.94098
Rel. Int. [%]
1.72
0.63
0.87
5.02
3.99
0.19
0.19
1.11
1.61
5.64
4.39
Matched by
00-004-0587
00-004-0587
00-043-1022
00-043-1022
F-258
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 259 of 478
FACILITY J
7.1: 2512-J-SC
7.1.1: Measurement Conditions of 2512-J
Dataset Name
File name
J-SC, no cover_002.udf
Sample Identification 2512-J-SC
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2512-J-SC, no cover_002
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2512-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-ASCII (.UDF)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
F-259
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 260 of 478
7.1.2: Main Graphics, Analyze View of 2512-J
VV
2512-J-SC, no cover_002
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-056!
Aluminum (01-085-1327)
I Quartz, syn (01-083-2467)
I Periclase, syn (00-043-1022)
50 60 70 80
Position [°2Theta] (Copper (Cu))
Aluminum Oxide Nitride 11.8 %
Sylvite,syn9.8%
Aluminum Oxide Nitride 8.8 %
Aluminum Oxide 11.8 %
| Aluminum Oxide 6.9 % |
| Aluminum Oxide Nitride 6.9 % |
Magnesium Aluminum Oxide 5.9 % |
| Sodium Chloride 14.7 %
"Quartz 2.9 % |
Periclase, syn 1 % |]
Aluminum Nitride 2.9 %]
Anhl Aluminum 3.9 % |
F-260
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 261 of 478
7.1.3: Pattern List of 2512-J
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
Score
52
50
55
37
36
14
15
16
47
23
15
19
15
16
31
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
7
10
15
6
3
12
9
7
4
1
5
3
5
12
3
Matched
Lines
19
10
9
12
9
13
11
11
5
7
6
13
37
13
22
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-261
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 262 of 478
7.1.4: Peak List of 2512-J
Pos. [°2Th.]
18.9425
20.8213
22.2139
24.3813
25.5309
26.5923
27.3301
28.3034
29.3339
31.6478
33.1353
34.6286
35.0924
36.0066
36.8275
37.7277
38.4594
39.4240
40.4741
42.8928
43.3001
44.7024
45.3670
47.2702
48.8972
50.1007
Height [cts]
733.50
811.17
1338.68
477.10
2210.65
4548.01
3970.43
24120.18
819.89
37021.99
2269.23
1627.65
4218.03
1788.66
3809.62
3374.33
8915.70
1376.23
15997.41
3401.98
7273.68
11195.21
27708.14
3303.69
1920.46
6703.75
FWHM
[°2Th.]
0.1378
0.1181
0.0787
0.2362
0.0787
0.1181
0.1181
0.1476
0.2362
0.1476
0.0984
0.1574
0.0689
0.1771
0.1574
0.1378
0.1279
0.1574
0.1378
0.1574
0.0886
0.1378
0.1378
0.1181
0.2362
0.0689
d-spacing [A]
4.68506
4.26635
4.00194
3.65087
3.48903
3.35213
3.26329
3.15325
3.04478
2.82724
2.70364
2.59040
2.55722
2.49436
2.44062
2.38444
2.34074
2.28566
2.22875
2.10852
2.08962
2.02727
1.99911
1.92297
1.86272
1.82076
ReLIntM
1.98
2.19
3.62
1.29
5.97
12.28
10.72
65.15
2.21
100.00
6.13
4.40
11.39
4.83
10.29
9.11
24.08
3.72
43.21
9.19
19.65
30.24
74.84
8.92
5.19
18.11
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862
01-074-1132;
01-085-1327;
00-022-1235
01-080-2173;
01-085-0930
00-004-0587
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-086-2270
00-022-1235
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
51.6643
2276.05
0.5510
1.76927
6.15
F-262
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 263 of 478
Pos. [°2Th.]
52.4761
53.7826
54.7964
56.3891
56.5476
57.4017
57.5798
58.5600
59.2876
59.9195
61.2472
62.2415
65.0860
66.1172
66.2918
66.4728
67.6591
68.0802
68.2982
71.3757
72.3942
72.9608
73.5923
73.8147
75.1408
75.1936
75.3792
76.2842
76.7761
Height [cts]
3329.06
1417.74
518.85
6818.51
4197.83
3703.19
2438.05
2084.93
1887.44
1393.98
911.96
416.56
3455.60
4830.12
6550.74
4979.74
414.18
2082.19
1422.63
325.47
238.96
400.13
2289.08
1534.18
5224.82
5563.04
3425.78
333.33
704.68
FWHM
[°2Th.]
0.1378
0.1181
0.2362
0.1560
0.0960
0.0480
0.0960
0.0960
0.2160
0.1200
0.1200
0.1920
0.2640
0.0720
0.1440
0.1200
0.1440
0.1200
0.0960
0.3360
0.3840
0.1440
0.1680
0.1440
0.0600
0.0480
0.0840
0.1440
0.1200
d-spacing [A]
1.74380
1.70448
1.67532
1.63038
1.63022
1.60400
1.59946
1.57500
1.55740
1.54248
1.51218
1.49039
1.43196
1.41211
1.40881
1.40890
1.38363
1.37609
1.37564
1.32043
1.30434
1.29561
1.28604
1.28590
1.26333
1.26258
1.26306
1.24722
1.24045
Rel. Int. [%]
8.99
3.83
1.40
18.42
11.34
10.00
6.59
5.63
5.10
3.77
2.46
1.13
9.33
13.05
17.69
13.45
1.12
5.62
3.84
0.88
0.65
1.08
6.18
4.14
14.11
15.03
9.25
0.90
1.90
Matched by
01-075-1862
01-077-2064
01-085-0930
01-077-2064
01-075-1862;
01-085-0930
01-075-1862
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-085-0930
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171
01-085-0930
01-075-1862;
00-022-1235;
01-085-0930
01-075-1620;
01-080-2173;
01-086-2270
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-077-2064
01-075-1620
01-075-1862
F-263
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 264 of 478
Pos. [°2Th.]
77.2033
78.1629
78.4547
79.8518
80.5893
82.4251
83.8912
84.0820
86.3208
87.5155
87.9410
88.8665
90.2618
91.0466
94.3651
95.1416
99.0923
101.0075
101.3011
106.5669
107.6149
108.4030
109.9386
Height [cts]
512.86
1758.52
1339.85
86.09
203.23
553.78
3340.41
2122.09
122.73
463.14
379.80
228.24
256.10
351.22
1167.46
782.36
275.79
1368.78
1290.49
109.66
343.72
581.79
1570.04
FWHM
[°2Th.]
0.3840
0.2400
0.1680
0.2880
0.1440
0.1920
0.1680
0.0840
0.3840
0.2400
0.1920
0.1440
0.1440
0.1920
0.2160
0.1680
0.5760
0.0960
0.1680
0.5760
0.1920
0.1680
0.0840
d-spacing [A]
1.23465
1.22187
1.22108
1.20022
1.19109
1.16915
1.15241
1.15314
1.12610
1.11378
1.11224
1.10030
1.08689
1.07955
1.05014
1.04361
1.01231
0.99823
0.99860
0.96095
0.95448
0.94972
0.94071
Rel. Int. [%]
1.39
4.75
3.62
0.23
0.55
1.50
9.02
5.73
0.33
1.25
1.03
0.62
0.69
0.95
3.15
2.11
0.74
3.70
3.49
0.30
0.93
1.57
4.24
Matched by
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327
01-080-2171;
01-086-2270;
01-080-1385;
01-085-0930
01-075-1862
01-085-1327
01-077-2064;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-004-0587;
00-004-0864
00-004-0587
00-043-1022
F-264
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 265 of 478
7.2: 2515-J-SC
7.2:1: Measurement Conditions of 2515-J
Dataset Name
File name
J-SC.udf
Sample Identification 2515-J-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
2515-J-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2515-
7.2.2: Main Graphics, Analyze View of 2515-J
F-265
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 266 of 478
2515-J-SC
• Aluminum Oxide (01-075-1865;
• Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
50 60 70
Position [°2Theta] (Copper (Cu))
Sylvite, syn 11.9
Aluminum Oxide Nitride 9.9 % |
Aluminum Oxide 8.9 %|
Aluminum Oxide 8.9 %
Magnesium Aluminum Oxide 7.9 % |
Aluminum Qxide Nitride 5.9 %
Sodium Chloride 20.8 %]
F-266
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 267 of 478
7.2.3: Pattern List of 2515-J
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
01-085-
0930
Score
55
43
48
44
35
11
14
17
40
7
24
20
14
18
23
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
9
12
21
8
4
10
6
5
4
1
4
5
9
1
2
Matched
Lines
20
10
9
12
8
11
11
12
5
6
14
33
11
17
20
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-267
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 268 of 478
7.2.4: Peak List of 2515-J
Pos. [°2Th.]
11.2362
19.0814
20.9154
22.3293
24.4889
25.6375
26.6921
27.4594
28.4280
28.4912
29.4775
31.7656
33.2680
34.7448
35.2639
35.7137
36.1128
36.9769
37.8437
38.5469
39.5676
40.5550
42.0552
43.4416
44.9197
Height [cts]
152.77
472.96
366.23
537.92
203.42
993.07
1883.33
2468.88
12463.55
9561.35
702.72
24900.67
1214.76
768.27
2108.40
938.09
1182.65
3030.78
1916.15
3420.15
815.15
8595.17
626.22
2902.02
4240.69
FWHM
[°2Th.]
0.7872
0.2362
0.1378
0.0886
0.3149
0.0787
0.0787
0.1279
0.1560
0.0480
0.1680
0.2280
0.1680
0.1920
0.1320
0.1920
0.2400
0.1080
0.1680
0.1560
0.1920
0.1920
0.3840
0.1320
0.2640
d-spacing [A]
7.87493
4.65126
4.24737
3.98151
3.63507
3.47476
3.33982
3.24822
3.13710
3.13808
3.02776
2.81469
2.69094
2.57986
2.54307
2.51207
2.48521
2.42909
2.37543
2.33370
2.27582
2.22265
2.14677
2.08142
2.01630
Rel. Int. [%]
0.61
1.90
1.47
2.16
0.82
3.99
7.56
9.91
50.05
38.40
2.82
100.00
4.88
3.09
8.47
3.77
4.75
12.17
7.70
13.74
3.27
34.52
2.51
11.65
17.03
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
01-086-2270
01-086-2340
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-075-1620;
01-086-2270;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
01-086-2340;
01-085-0930
00-004-0587
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
F-268
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 269 of 478
Pos. [°2Th.]
45.5022
45.6223
47.4019
50.1908
52.6021
53.9244
54.9751
56.5191
56.6884
57.5447
58.6596
59.4596
60.0654
61.3697
62.4473
65.2945
66.2636
Height [cts]
17807.90
12998.78
1299.42
3083.67
1206.79
908.69
354.25
5691.75
3628.94
2254.77
1588.71
1910.69
1219.87
829.34
554.52
3315.82
4880.26
FWHM
[°2Th.]
0.1560
0.0840
0.1680
0.0840
0.1920
0.1200
0.2880
0.1440
0.0960
0.0960
0.1920
0.2160
0.2400
0.3360
0.2880
0.1920
0.1080
d-spacing [A]
1.99183
1.99181
1.91634
1.81620
1.73848
1.69893
1.66892
1.62693
1.62651
1.60035
1.57257
1.55330
1.53908
1.50946
1.48597
1.42789
1.40934
Rel. Int. [%]
71.52
52.20
5.22
12.38
4.85
3.65
1.42
22.86
14.57
9.06
6.38
7.67
4.90
3.33
2.23
13.32
19.60
Matched by
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-086-2270
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-085-0930
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385;
01-086-2340
01-075-1862;
01-086-2340
00-004-0587
01-075-1862;
01-074-1132;
01-075-1620
01-085-0930
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
01-075-1862;
00-004-0587;
01-077-2064;
01-075-1620;
01-080-2171;
01-080-1385
F-269
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 270 of 478
Pos. [°2Th.]
66.4360
68.2613
69.2154
71.5169
73.1179
73.7198
73.9256
75.3495
75.5686
76.4353
76.9280
77.5337
78.3612
80.8035
82.5605
84.0238
84.2884
86.4853
87.6209
Height [cts]
5642.53
1780.96
385.51
477.42
614.70
2075.25
1468.36
6167.73
3532.98
486.28
654.93
587.00
1278.55
228.82
417.49
4061.48
2339.44
118.61
398.02
FWHM
[°2Th.]
0.0720
0.0840
0.2880
0.6720
0.1440
0.1680
0.1440
0.1560
0.1200
0.1440
0.1440
0.4800
0.1440
0.2880
0.4320
0.1320
0.1080
0.3840
0.1920
d-spacing [A]
1.40960
1.37288
1.35627
1.31817
1.29321
1.28413
1.28425
1.26035
1.26036
1.24513
1.23838
1.23021
1.21928
1.18847
1.16758
1.15093
1.15084
1.12438
1.11271
Rel. Int. [%]
22.66
7.15
1.55
1.92
2.47
8.33
5.90
24.77
14.19
1.95
2.63
2.36
5.13
0.92
1.68
16.31
9.40
0.48
1.60
Matched by
01-075-1862;
00-022-1235;
01-085-0930
00-022-1235;
01-086-2340
01-075-1620;
01-086-2270
01-077-2064
00-004-0587;
00-022-1235;
01-086-2340
01-077-2064;
01-080-2171
01-075-1620;
01-086-2340
01-075-1862;
01-086-2270
01-074-1132;
01-086-2270;
01-085-0930
01-074-1132;
01-085-1327;
00-043-1022;
01-086-2270;
01-086-2340
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
01-086-2270
01-075-1862;
01-077-2064;
01-086-2270;
01-086-2340;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
F-270
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 271 of 478
Pos. [°2Th.]
88.0863
89.0270
90.4466
91.2174
94.5138
95.2953
99.4425
101.1670
101.5251
106.8023
107.8112
108.5503
109.8275
Height [cts]
319.14
139.71
345.01
249.14
1163.37
641.66
250.40
1475.46
1221.61
264.85
692.97
854.81
1150.60
FWHM
[°2Th.]
0.1920
0.2400
0.1440
0.2400
0.1680
0.1440
0.5760
0.1440
0.1920
0.5760
0.2160
0.2400
0.0360
d-spacing [A]
1.10803
1.09874
1.08515
1.07798
1.04888
1.04233
1.00969
0.99709
0.99701
0.95948
0.95328
0.94884
0.94135
Rel. Int. [%]
1.28
0.56
1.39
1.00
4.67
2.58
1.01
5.93
4.91
1.06
2.78
3.43
4.62
Matched by
01-086-2270
01-075-1862
00-022-1235
00-004-0587
00-004-0587
00-004-0587
00-043-1022
F-271
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 272 of 478
7.3: 2517-J-SC
7.3.1: Measurement Conditions of 2517-J
Dataset Name
File name
J-SC, no cover.udf
Sample Identification 2517-J-SC, NO COVER
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2517-J-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2517-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
7.3.2: Main Graphics, Analyze View of 2517-J
F-272
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 273 of 478
V VIV
2517-J-SC, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
• Periclase, syn (00-043-1022)
tall
20 30 40 50 60 70 80 90
Position [°2Theta] (Copper (Cu))
100 110
Sodium Chloride 13.1 %
Aluminum Oxide Nitride 12.1 %
Aluminum Oxide Nitride 9.1 % |
| Sylvite, syn 7.1
Aluminum Oxide 15.2 %|
Aluminum Oxide Nitride 16.2 %
Periclase
.IH-J. CM.JI-. "1 &/- I
se, syn 1 % |
Aluminum
Quartz
mm 1 % |^n
a •*• k %\
L\\ ihriini irri t I
77^ Anhydrite 4 % |^T , , „ \
Maign^^iLHn'i ^.i^iiiiM^TT^Uxide 5.1 % |
F-273
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 274 of 478
7.3.3: Pattern List of 2517-J
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
Score
39
47
54
39
44
16
17
18
23
27
12
15
12
17
27
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
5
7
13
5
4
16
12
9
1
1
3
2
4
15
2
Matched
Lines
19
10
9
13
11
13
12
12
5
6
4
13
38
12
21
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-274
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 275 of 478
7.3.4: Peak List of 2517-J
Pos. [°2Th.]
18.9184
20.7936
22.7664
25.5271
26.5663
27.2928
28.2597
29.3011
31.6249
32.3243
33.1117
33.7248
34.0521
35.0865
35.5643
35.9866
36.8281
37.7099
37.8408
38.4941
39.3737
40.4120
41.8673
42.8452
43.2394
44.7328
Height [cts]
799.87
575.99
826.15
1828.19
2980.30
3963.47
21338.74
737.34
38403.13
975.42
2840.36
1275.91
1087.06
3731.25
1571.47
2510.86
4674.30
3379.84
3558.44
2335.85
1173.46
13312.09
1815.96
3234.29
6225.85
8580.70
FWHM
[°2Th.]
0.1181
0.1574
0.4723
0.0787
0.1082
0.0984
0.1574
0.1378
0.1870
0.1181
0.0590
0.2362
0.1574
0.0787
0.1181
0.1378
0.2165
0.1200
0.1574
0.1968
0.1574
0.1870
0.2362
0.1574
0.0590
0.1181
d-spacing [A]
4.69096
4.27196
3.90605
3.48954
3.35536
3.26766
3.15803
3.04811
2.82924
2.76960
2.70552
2.65772
2.63293
2.55763
2.52436
2.49570
2.44059
2.38355
2.37757
2.33871
2.28847
2.23203
2.15776
2.11075
2.09241
2.02596
ReLIntM
2.08
1.50
2.15
4.76
7.76
10.32
55.57
1.92
100.00
2.54
7.40
3.32
2.83
9.72
4.09
6.54
12.17
8.80
9.27
6.08
3.06
34.66
4.73
8.42
16.21
22.34
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-080-2173
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
00-004-0587;
01-085-0930
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
F-275
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 276 of 478
Pos. [°2Th.]
45.3419
47.2083
49.7122
50.0580
51.3941
52.4489
53.7564
56.3639
56.5468
57.4036
58.5260
59.2823
59.8733
61.2501
62.2015
65.1483
66.0946
66.2745
68.0825
69.6647
70.5276
Height [cts]
27654.29
2933.97
2603.08
5724.11
2049.87
2962.26
1363.96
6909.97
3501.15
2878.14
1828.41
2880.40
1467.03
537.44
536.68
3270.57
5309.74
6533.08
2286.81
213.23
384.81
FWHM
[°2Th.]
0.0886
0.0984
0.1181
0.0886
0.4723
0.1378
0.1181
0.1680
0.0960
0.1200
0.1920
0.2160
0.2400
0.2880
0.3360
0.2160
0.1200
0.2160
0.1680
0.2880
0.4800
d-spacing [A]
2.00016
1.92534
1.83408
1.82221
1.77794
1.74464
1.70525
1.63105
1.63024
1.60395
1.57584
1.55752
1.54356
1.51212
1.49125
1.43074
1.41253
1.40913
1.37605
1.34862
1.33422
Rel. Int. [%]
72.01
7.64
6.78
14.91
5.34
7.71
3.55
17.99
9.12
7.49
4.76
7.50
3.82
1.40
1.40
8.52
13.83
17.01
5.95
0.56
1.00
Matched by
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-085-0930
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-075-1620
01-075-1862
F-276
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 277 of 478
Pos. [°2Th.]
71.2977
72.4845
73.6062
73.8180
75.1600
75.3769
76.2942
76.7544
77.1914
78.1696
80.7655
82.4755
83.8120
83.8903
84.0974
86.2753
87.5589
87.8621
88.8417
90.2449
90.6372
Height [cts]
809.88
373.23
2137.21
1522.59
5830.71
3207.02
440.15
628.36
551.53
547.72
139.20
283.31
3258.39
3244.46
1938.17
93.41
392.11
350.31
119.61
219.83
288.02
FWHM
[°2Th.]
0.1680
0.1440
0.0960
0.1680
0.1320
0.1200
0.1440
0.1440
0.4800
0.3360
0.9600
0.2880
0.0840
0.0600
0.1440
0.5760
0.1680
0.2880
0.5760
0.1440
0.1920
d-spacing [A]
1.32168
1.30294
1.28583
1.28267
1.26306
1.26309
1.24708
1.24075
1.23481
1.22178
1.18893
1.16856
1.15330
1.15242
1.15011
1.12657
1.11333
1.11027
1.10055
1.08705
1.08336
Rel. Int. [%]
2.11
0.97
5.57
3.96
15.18
8.35
1.15
1.64
1.44
1.43
0.36
0.74
8.48
8.45
5.05
0.24
1.02
0.91
0.31
0.57
0.75
Matched by
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620
00-004-0587;
00-022-1235;
01-085-0930
00-004-0587;
00-022-1235
01-077-2064
01-075-1620
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327;
00-022-1235
01-075-1862
01-074-1132;
01-085-1327
01-077-2064;
01-085-0930
01-077-2064;
01-085-0930
01-075-1862;
01-077-2064;
01-080-2171;
01-086-2270;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
00-004-0587;
01-080-2172;
01-080-2173
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
F-277
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 278 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
91.0246
94.3065
94.7096
95.0684
99.2305
317.52
1102.09
1011.67
914.64
227.06
0.2400
0.1920
0.1920
0.1680
0.4800
1.07976
1.05063
1.04722
1.04681
1.01127
0.83
2.87
2.63
2.38
0.59
00-004-0587;
00-004-0864
00-004-0587
100.9912
101.3026
104.3879
107.6243
108.3281
109.9130
1384.47
1233.72
40.82
326.94
442.56
1694.51
0.1920
0.2160
0.9600
0.2400
0.2400
0.0720
0.99835
0.99612
0.97495
0.95442
0.95017
0.94086
3.61
3.21
0.11
0.85
1.15
4.41
00-004-0587
00-004-0587
00-043-1022
F-278
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 279 of 478
7.4: 2519-J-SC
7.4.1: Measurement Conditions of 2519-J
Dataset Name
File name
J-SC.udf
Sample Identification 2519-J-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
7.4.2: Main Graphics, Analyze View of 2519-J
2519-J-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2519-
F-279
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 280 of 478
V V
2519-J-SC
I Aluminum Oxide (01-075-1865
I Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
| Quartz, syn (01-083-2467)
96)
i. JiiJilUI
50 60 70
Position [°2"meta] (Copper (Cu))
Fluorite, syn 11.9 % |
Aluminum Oxide Nitride 11.9 % |
Aluminum Oxide 10.9%
Sylvite, syn 10.9 %
Aluminum Oxide Nitride 7.9 %
Aluminum Oxide Nitride 5.9 %
Sodium Chloride 14.9~%"|
Aluminum 1 %
i Quartz 2 % l~
rfcalcitel % |n2%"h
Magnesium Aluminum Oxide 5 % |
Alumhl Anhydrite 4 % |]
7.4.3: Pattern List of 2519-J
F-280
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 281 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
01-085-
0930
46
51
56
46
36
13
14
16
38
7
13
18
18
14
17
30
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
6
11
15
5
4
12
8
6
1
1
12
2
4
11
1
2
19
10
9
12
9
11
11
12
5
6
4
13
35
11
18
20
0
0
0
0
0
0
0
0
0
0
1
0
0
0
0
0
F-281
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 282 of 478
7.4.4: Peak List of 2519-J
Pos. [°2Th.]
10.0589
10.3355
11.0537
14.0181
18.9755
20.7948
23.1205
24.4491
25.5029
26.5860
27.2905
28.2729
29.3783
31.6538
33.1804
33.7617
35.0862
35.5961
36.0358
36.8206
37.7333
38.4496
39.4381
40.4406
41.8457
42.4193
Height [cts]
74.52
131.55
145.67
138.97
540.80
392.52
183.58
164.99
1274.00
1658.84
2547.92
16122.50
835.55
25840.60
1842.89
665.47
2478.00
890.16
1543.28
3046.15
2221.08
2267.76
713.30
10893.05
507.82
588.06
FWHM
[°2Th.]
0.0295
0.6298
0.4723
0.0787
0.1574
0.0787
0.3936
0.2362
0.0787
0.1181
0.1181
0.1968
0.1771
0.1771
0.0689
0.2362
0.0886
0.1181
0.1574
0.2165
0.1771
0.0886
0.1574
0.1378
0.2362
0.1181
d-spacing [A]
8.79389
8.55912
8.00458
6.31781
4.67697
4.27173
3.84703
3.64090
3.49280
3.35291
3.26794
3.15657
3.04027
2.82672
2.70007
2.65491
2.55766
2.52218
2.49241
2.44107
2.38410
2.34131
2.28488
2.23052
2.15882
2.13094
Rel. Int. [%]
0.29
0.51
0.56
0.54
2.09
1.52
0.71
0.64
4.93
6.42
9.86
62.39
3.23
100.00
7.13
2.58
9.59
3.44
5.97
11.79
8.60
8.78
2.76
42.15
1.97
2.28
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-086-2340
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
01-080-2172;
01-080-2173;
01-086-2340;
01-085-0930
00-004-0587;
01-085-0930
01-085-0930
F-282
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 283 of 478
Pos. [°2Th.]
43.2989
44.7914
45.3740
45.5202
47.2660
48.5280
50.1059
50.2401
52.4744
53.8050
56.3999
56.5717
57.4337
57.6194
58.5791
59.3218
61.2377
62.3222
65.2034
65.3264
66.1630
Height [cts]
3201.20
3554.39
17926.42
11370.81
1246.66
462.21
3932.55
3221.71
1415.53
861.25
5682.39
3491.35
2838.22
1809.91
1954.50
2207.87
726.51
476.57
2957.03
3196.61
5434.16
FWHM
[°2Th.]
0.1476
0.2362
0.1560
0.1200
0.1320
0.2880
0.1200
0.0960
0.1320
0.1320
0.1200
0.1200
0.0960
0.0960
0.1680
0.1920
0.2880
0.3840
0.2160
0.1680
0.0960
d-spacing [A]
2.08968
2.02345
1.99716
1.99603
1.92153
1.87447
1.81908
1.81904
1.74241
1.70242
1.63009
1.62958
1.60318
1.60243
1.57453
1.55658
1.51239
1.48866
1.42967
1.42727
1.41124
Rel. Int. [%]
12.39
13.76
69.37
44.00
4.82
1.79
15.22
12.47
5.48
3.33
21.99
13.51
10.98
7.00
7.56
8.54
2.81
1.84
11.44
12.37
21.03
Matched by
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-086-2270;
01-086-2340
01-086-2270;
01-086-2340
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862
01-077-2064
01-077-2064
01-075-1862;
01-086-2340;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
01-086-2270
01-074-1132;
01-086-2270
01-077-2064;
01-075-1620
F-283
-------
Pos. [°2Th.] Height [cts]
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 284 of 478
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
66.3308
66.4859
68.1512
68.3450
71.3431
72.5487
73.0472
73.6339
73.8609
75.2254
75.4408
76.8376
78.2565
80.6446
82.4473
83.9140
84.1926
86.3569
87.5595
6568.07
5042.50
1933.61
1314.26
740.76
405.80
616.47
2517.82
1728.37
5915.75
3469.29
741.59
875.16
265.91
320.77
3814.05
2192.54
200.27
527.34
0.1200
0.0960
0.1680
0.1200
0.1680
0.2880
0.1200
0.1560
0.1440
0.1440
0.0960
0.1680
0.3360
0.1440
0.2880
0.1320
0.1440
0.1920
0.1680
1.40808
1.40866
1.37483
1.37481
1.32095
1.30195
1.29429
1.28542
1.28521
1.26212
1.26218
1.23961
1.22065
1.19041
1.16889
1.15215
1.15191
1.12572
1.11333
25.42
19.51
7.48
5.09
2.87
1.57
2.39
9.74
6.69
22.89
13.43
2.87
3.39
1.03
1.24
14.76
8.48
0.78
2.04
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270
01-075-1620;
01-086-2340
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-086-2340;
01-085-0930
01-077-2064
01-075-1862
01-074-1132;
01-085-1327
01-075-1862;
01-086-2340
01-074-1132;
01-085-1327
01-077-2064;
01-086-2340;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
F-284
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 285 of 478
Pos. [°2Th.] Height [cts]
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
88.0079
88.9746
90.3288
399.67
181.31
256.14
0.2400
0.1920
0.1680
1.10881
1.09925
1.08625
1.55
0.70
0.99
01-080-1385;
01-085-0930
01-075-1862
00-022-1235
91.1338
94.4244
94.7518
95.1873
99.3439
101.0843
101.4370
106.6915
107.7243
108.5223
109.7716
323.33
1360.72
1155.00
918.07
208.49
1554.98
1388.63
301.22
706.79
1026.38
1199.51
0.1920
0.1920
0.1920
0.1680
0.3840
0.1080
0.1680
0.1440
0.2640
0.2400
0.1320
1.07875
1.04963
1.04687
1.04582
1.01042
0.99768
0.99763
0.96017
0.95381
0.94901
0.94168
1.25
5.27
4.47
3.55
0.81
6.02
5.37
1.17
2.74
3.97
4.64
00-004-0587;
00-004-0864
00-004-0587
00-004-0587
00-043-1022
F-285
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 286 of 478
FACILITY L
8.1: 2482-L-SC
8.1.1: Measurement Conditions of 2482-L
Dataset Name
File name
SC, no cover.sd
Sample Identification 2482-L-Sc, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 9/20/2010 10:56:00 AM
2482-L-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2482-L-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
F-286
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 287 of 478
8.1.2: Main Graphics, Analyze View of 2482-L
2482-L-SC, no cover
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-0
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-056;
Aluminum (01 -085-1 327)
I Periclase, syn (00-043-1 022)
96)
! ! ii r ], i
50 60 70
Position [°2Theta] (Copper (Cu))
Magnesium Aluminum Oxide 17:3 % \
Aluminum Oxide Nitride 12.9 %
Aluminum Oxide 10.9 %
Aluminum Oxide Nitride 7.9 %
| Aluminum Oxide Nitride 5.9 % |
Sodium Chloride 19.3 %|
j| Fluorite, syn 2 %
.-.i,;.-.!.-.^..-.—.-...-. .1 Q^
Aluminum 3 % 13
Sylvite, syn 4 % |
F-287
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 288 of 478
8.1.3: Pattern List of 2482-L
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-080-
1385
Score
34
52
61
61
45
17
15
15
31
42
30
26
16
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
A12.667 O4
3
4
20
18
5
13
8
6
3
4
2
4
11
Matched
Lines
15
10
9
15
11
11
12
12
5
8
6
16
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
F-288
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 289 of 478
8.1.4: Peak List of 2482-L
Pos. [°2Th.]
15.6736
18.9830
23.1067
25.5651
27.3381
28.3316
31.2570
31.6772
33.1793
35.1020
36.0588
36.8138
37.8800
38.4495
40.4744
40.5663
42.8845
43.3042
44.7704
44.8247
45.3908
45.5041
46.9674
47.3013
49.7867
50.1628
Height [cts]
155.17
4080.36
637.18
433.66
5445.36
14807.44
8015.88
59892.18
3023.05
1126.58
2233.93
17746.47
2783.95
3893.46
8586.98
8843.97
7138.10
4201.50
18157.76
18264.11
39429.00
26127.38
2629.51
2885.08
2514.96
4238.78
FWHM
[°2Th.]
0.2362
0.1082
0.1574
0.1574
0.1279
0.1378
0.0787
0.1870
0.0984
0.1574
0.1771
0.1574
0.1968
0.0787
0.1440
0.0840
0.0960
0.0960
0.1440
0.0360
0.1800
0.0720
0.1920
0.1920
0.1920
0.1920
d-spacing [A]
5.65403
4.67514
3.84929
3.48443
3.26235
3.15017
2.86169
2.82468
2.70016
2.55654
2.49087
2.44150
2.37520
2.34132
2.22689
2.22758
2.10716
2.08770
2.02268
2.02537
1.99646
1.99670
1.93305
1.92018
1.82999
1.81715
ReLIntM
0.26
6.81
1.06
0.72
9.09
24.72
13.38
100.00
5.05
1.88
3.73
29.63
4.65
6.50
14.34
14.77
11.92
7.02
30.32
30.49
65.83
43.62
4.39
4.82
4.20
7.08
Matched by
01-074-1132;
00-022-1235
01-075-1862
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587
00-043-1022
01-075-1862
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064
00-004-0864
01-075-1620;
01-080-2171
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
51.7282
2168.48
0.4800
1.76578
3.62
F-289
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 290 of 478
Pos. [°2Th.]
52.4871
53.7696
55.5881
56.3880
56.5619
57.4468
58.5654
59.2919
59.4898
62.2363
65.1970
65.3791
66.1023
66.3335
68.1430
68.5901
69.7148
71.3356
72.5980
72.9769
73.6244
75.1836
75.3930
77.2562
78.1756
78.5565
80.9314
Height [cts]
1909.65
1657.34
1780.70
9573.32
5150.39
1026.94
1459.87
8260.74
5856.39
2214.11
13452.39
8913.20
5125.14
4553.34
661.29
491.88
156.04
701.26
460.46
613.53
1267.78
8017.12
4370.18
1553.01
1113.56
912.08
74.50
FWHM
[°2Th.]
0.2400
0.1440
0.2400
0.1440
0.0960
0.1920
0.1920
0.1080
0.0720
0.2640
0.1800
0.1440
0.0960
0.1440
0.1680
0.2880
0.2880
0.1920
0.3360
0.1440
0.1680
0.1320
0.1320
0.1920
0.1920
0.1920
0.6720
d-spacing [A]
1.74202
1.70345
1.65196
1.63040
1.62984
1.60285
1.57487
1.55730
1.55644
1.49050
1.42979
1.42979
1.41239
1.40802
1.37498
1.36710
1.34777
1.32108
1.30118
1.29858
1.28556
1.26272
1.26286
1.23393
1.22171
1.21673
1.18691
Rel. Int. [%]
3.19
2.77
2.97
15.98
8.60
1.71
2.44
13.79
9.78
3.70
22.46
14.88
8.56
7.60
1.10
0.82
0.26
1.17
0.77
1.02
2.12
13.39
7.30
2.59
1.86
1.52
0.12
Matched by
01-075-1862
01-077-2064
01-074-1132;
00-004-0864
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
00-043-1022
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1862;
00-022-1235
01-074-1132;
00-004-0864
01-074-1132;
01-075-1620;
01-080-2171
01-075-1620;
01-080-2172;
01-080-2173
01-075-1620
00-004-0587;
00-022-1235
01-077-2064
01-075-1862;
01-074-1132
01-085-1327;
00-022-1235
01-074-1132;
00-043-1022
01-075-1620
F-290
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 291 of 478
Pos. [°2Th.]
82.5515
83.8645
84.1308
85.6938
87.5711
90.2642
90.8797
93.9884
94.3951
99.2439
101.0082
101.3682
104.7107
105.7555
107.6329
109.8329
Height [cts]
1158.94
4744.69
2453.10
294.34
244.70
368.27
592.62
1906.23
1527.01
920.27
1440.77
976.67
60.50
86.68
597.58
2743.73
FWHM
[°2Th.]
0.1440
0.1920
0.1440
0.1440
0.1920
0.1920
0.2400
0.2880
0.2400
0.2880
0.0840
0.1920
0.5760
0.5760
0.2400
0.0960
d-spacing [A]
1.16768
1.15271
1.15259
1.13272
1.11321
1.08686
1.08110
1.05335
1.05249
1.01117
0.99822
0.99812
0.97283
0.96607
0.95437
0.94132
Rel. Int. [%]
1.94
7.92
4.10
0.49
0.41
0.61
0.99
3.18
2.55
1.54
2.41
1.63
0.10
0.14
1.00
4.58
Matched by
01-074-1132;
01-085-1327
01-077-2064
01-074-1132;
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385
00-022-1235
00-043-1022;
00-004-0864
00-043-1022;
00-004-0864
00-043-1022
F-291
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 292 of 478
8.2: 2484-L-SC
8.2.1: Measurement Conditions of 2484-L
Dataset Name
File name
SC_006.sd
Sample Identification 2484-L-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 8/5/2010 6:54:00 AM
2484-L-SC_006
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2484-L-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
10.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
F-292
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 293 of 478
8.2.2: Main Graphics, Analyze View of 2484-L
2484-L-SC_006
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
I Periclase, syn (00-043-1022)
96)
m
A
10 20 30 40 50 60 70 80 90 100 110
Position [°2Theta] (Copper (Cu))
Sodium Chloride 16.2 %
Aluminum Oxide Nitride 7.1 %
Anhydrite 6.1 %
Elpasolite, syn 6.1 %
Aluminum Oxide
Aluminum Nitride 6.1 %
Magnesium Aluminum Oxide 23.2 % |
Aluminum Oxide Nitride 3 %
I Aluminum 4 %
Periclase, syn 4 % |
Aluminum Oxide Nitride 4 % ]
F-293
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 294 of 478
8.2.3:Pattern List of 2484-L
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
50
39
41
50
34
13
14
15
31
34
24
32
22
14
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
6
5
16
23
6
7
4
3
4
4
4
6
6
5
Matched
Lines
20
10
9
14
10
12
12
12
5
8
6
17
37
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-294
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 295 of 478
8.2.4: Peak List of 2484-L
Pos. [°2Th.]
16.3933
19.0042
23.0943
24.4679
25.5611
26.6202
27.3502
28.3146
28.3741
31.2412
31.6693
33.2008
35.1381
35.6153
36.0187
36.8682
37.7662
37.9115
38.5093
40.5357
42.8889
43.3570
44.7964
44.8679
45.4104
45.5258
46.9632
Height [cts]
29.20
2935.13
127.55
89.84
1011.78
160.21
3393.97
7823.07
7618.29
5345.08
36360.15
2479.83
2169.41
840.57
1940.96
14981.02
2289.08
2324.36
3007.98
5402.53
4401.33
2805.64
10963.51
10621.90
24150.21
16258.59
626.10
FWHM
[°2Th.]
0.2362
0.1279
0.1574
0.1181
0.1181
0.1181
0.0492
0.1080
0.0600
0.0840
0.1680
0.2160
0.1080
0.1440
0.2160
0.1920
0.1440
0.1440
0.1680
0.1440
0.0840
0.0960
0.1080
0.0720
0.1440
0.0840
0.2400
d-spacing [A]
5.40737
4.66998
3.85133
3.63814
3.48498
3.34868
3.26094
3.14942
3.15076
2.86074
2.82304
2.69623
2.55188
2.51878
2.49149
2.43601
2.38012
2.37133
2.33589
2.22367
2.10695
2.08528
2.02156
2.02352
1.99565
1.99580
1.93322
ReLIntM
0.08
8.07
0.35
0.25
2.78
0.44
9.33
21.52
20.95
14.70
100.00
6.82
5.97
2.31
5.34
41.20
6.30
6.39
8.27
14.86
12.10
7.72
30.15
29.21
66.42
44.72
1.72
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064;
01-080-2171;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
F-295
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 296 of 478
Pos. [°2Th.]
47.3246
49.7393
50.1521
52.5316
53.8366
55.6551
56.4219
56.5827
57.4762
58.5972
59.3031
59.3900
59.4959
61.3019
62.2782
65.2207
65.2698
65.4156
66.1631
66.3699
68.1804
68.3987
69.6973
71.3995
73.0366
73.6996
Height [cts]
658.25
913.28
1726.87
1163.79
1023.58
1752.47
7592.67
4783.21
2278.94
1362.66
7575.05
8261.37
6726.73
441.51
2608.95
13469.00
13738.25
10243.71
4882.33
4517.80
1671.57
1215.92
393.73
1024.75
673.44
1289.19
FWHM
[°2Th.]
0.2880
0.2400
0.2400
0.1680
0.1680
0.2880
0.1680
0.0960
0.1560
0.1440
0.0600
0.0840
0.1200
0.2880
0.0720
0.1320
0.0720
0.1440
0.0840
0.0960
0.1440
0.0720
0.2880
0.1440
0.1680
0.1680
d-spacing [A]
1.91929
1.83163
1.81751
1.74065
1.70149
1.65013
1.62951
1.62930
1.60210
1.57409
1.55703
1.55496
1.55244
1.51096
1.48960
1.42933
1.42837
1.42554
1.41124
1.41084
1.37431
1.37386
1.34807
1.32005
1.29445
1.28443
Rel. Int. [%]
1.81
2.51
4.75
3.20
2.82
4.82
20.88
13.16
6.27
3.75
20.83
22.72
18.50
1.21
7.18
37.04
37.78
28.17
13.43
12.43
4.60
3.34
1.08
2.82
1.85
3.55
Matched by
01-086-2270
01-075-1620
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-074-1132;
01-075-1620
01-074-1132;
01-075-1620
01-075-1862
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-085-1327;
01-086-2270
01-074-1132;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620
01-075-1620;
01-080-2173;
01-086-2270
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
F-296
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 297 of 478
Pos. [°2Th.]
75.2686
75.4553
76.8932
77.3110
77.5781
78.2247
78.5960
80.7128
82.6144
83.9217
84.2258
85.8286
87.6733
88.9651
90.3854
94.0936
94.4708
95.2475
99.3427
101.1167
101.4434
104.7029
105.8657
107.7641
109.7735
Height [cts]
7731.11
4601.85
803.24
1896.42
1403.17
1164.60
1147.49
248.08
1392.74
4922.23
2690.92
427.08
252.41
155.84
411.68
2441.48
1964.46
692.14
1097.45
1737.02
1230.89
145.49
241.62
945.02
1914.33
FWHM
[°2Th.]
0.1320
0.1080
0.1440
0.1440
0.1440
0.1920
0.2880
0.4800
0.2160
0.1080
0.1080
0.2640
0.2400
0.1440
0.1440
0.2160
0.2400
0.1920
0.3360
0.1920
0.1680
0.5760
0.5760
0.1680
0.0360
d-spacing [A]
1.26150
1.26197
1.23885
1.23320
1.23267
1.22106
1.21622
1.18958
1.16695
1.15207
1.15154
1.13129
1.11218
1.09934
1.08572
1.05245
1.04924
1.04273
1.01043
0.99745
0.99759
0.97288
0.96537
0.95357
0.94167
Rel. Int. [%]
21.26
12.66
2.21
5.22
3.86
3.20
3.16
0.68
3.83
13.54
7.40
1.17
0.69
0.43
1.13
6.71
5.40
1.90
3.02
4.78
3.39
0.40
0.66
2.60
5.26
Matched by
01-077-2064
01-075-1862;
01-086-2270
01-075-1862;
01-074-1132
01-074-1132;
01-085-1327
01-074-1132;
00-043-1022;
01-086-2270
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064
01-074-1132;
01-075-1620;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-022-1235
00-043-1022;
00-004-0864
00-004-0587;
00-004-0864
00-043-1022;
00-004-0864
00-043-1022
F-297
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 298 of 478
8.3: 2486-L-SC
8.3.1: Measurement Conditions of 2486-L
Dataset Name
File name
SC, no cover.sd
Sample Identification 2486-L-SC, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 9/21/2010 4:12:00 AM
2486-L-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2486-L-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
8.3.2: Main Graphics, Analyze View of 2486-L
F-298
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 299 of 478
2486-L-SC, no cover
| Aluminum Oxide (01-075-1865
(Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-0565
Aluminum (01-085-1327)
I Periclase, syn (00-043-1022)
96)
50 60 70
Position [°2"meta] (Copper (Cu))
Sylvite, syn 10.1 %
Aluminum Nitride 9.1 %|
Aluminum Qxide S.1 %
| Fluorite, syn 7V1%
Aluminum Qxide Nitride 7.1 % |
Magnesium Aluminum Oxide 10.1 % |
Sodium Chloride 19.2%
Calcite 1
Periclase, syn 1 % ]e 4 % |
Elpasolite, syn 3 % \ ~ ., ^ |
Anhydrite 6.1 %
Aluminum Oxide 7.1 %
F-299
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 300 of 478
8.3.3: Pattern List of 2486-L
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
Score
54
42
41
44
39
18
20
19
30
27
19
32
26
20
12
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
8
10
19
10
9
7
5
4
2
1
7
3
6
7
1
Matched
Lines
23
10
9
14
11
12
12
11
5
7
5
15
39
12
18
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-300
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 301 of 478
8.3.4: Peak List of 2486-L
Pos. [°2Th.]
11.0974
16.2435
18.8818
18.9432
21.0380
23.0137
23.8019
24.4061
25.4559
25.5136
26.5549
27.2561
28.2676
29.3195
31.1727
31.6095
33.0803
33.7313
35.0599
35.8917
36.7987
37.7720
37.8583
38.4179
40.4080
41.7138
42.8199
Height [cts]
38.92
70.19
2217.30
2565.64
228.34
314.11
323.60
369.53
2776.25
2862.00
837.77
6023.62
25602.28
1215.10
5081.80
62878.02
8939.73
2221.09
5387.06
6203.36
10779.92
7980.34
6874.35
2869.15
12753.38
993.51
2168.34
FWHM
[°2Th.]
0.9446
0.4723
0.0720
0.0689
0.3149
0.1968
0.1968
0.1181
0.0720
0.0590
0.0984
0.1181
0.1574
0.1574
0.1181
0.1574
0.0886
0.1378
0.0984
0.0394
0.1279
0.0600
0.0590
0.1968
0.1574
0.1574
0.1181
d-spacing [A]
7.97314
5.45693
4.69608
4.68487
4.22288
3.86463
3.73842
3.64721
3.49624
3.49136
3.35677
3.27198
3.15715
3.04624
2.86924
2.83058
2.70801
2.65723
2.55952
2.50209
2.44247
2.37977
2.37651
2.34317
2.23225
2.16534
2.11193
ReLIntM
0.06
0.11
3.53
4.08
0.36
0.50
0.51
0.59
4.42
4.55
1.33
9.58
40.72
1.93
8.08
100.00
14.22
3.53
8.57
9.87
17.14
12.69
10.93
4.56
20.28
1.58
3.45
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-074-1132;
00-022-1235;
01-086-2340
01-077-2064
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587
01-075-1862
00-043-1022
F-301
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 302 of 478
Pos. [°2Th.]
43.2748
44.6770
45.3343
45.4402
46.8868
49.6939
50.0758
52.4290
53.7665
54.9060
55.6027
56.3308
56.5090
57.3692
57.5593
58.5303
59.2282
60.3472
61.1844
62.2101
65.1512
65.3173
Height [cts]
5510.31
6287.95
33921.75
22831.59
933.23
2555.77
3736.10
2066.65
1375.89
449.79
1072.63
8643.86
5058.80
3979.31
2530.01
2156.66
6163.91
1485.84
867.86
913.96
6000.02
5805.26
FWHM
[°2Th.]
0.1476
0.0787
0.1800
0.0960
0.2880
0.1200
0.0720
0.0960
0.0840
0.2880
0.2880
0.1200
0.0840
0.1560
0.0960
0.1440
0.2640
0.2400
0.1920
0.3360
0.1920
0.1440
d-spacing [A]
2.09078
2.02837
1.99882
1.99936
1.93619
1.83319
1.82010
1.74381
1.70355
1.67086
1.65156
1.63193
1.63125
1.60483
1.60396
1.57573
1.55882
1.53256
1.51358
1.49107
1.43069
1.43100
Rel. Int. [%]
8.76
10.00
53.95
36.31
1.48
4.06
5.94
3.29
2.19
0.72
1.71
13.75
8.05
6.33
4.02
3.43
9.80
2.36
1.38
1.45
9.54
9.23
Matched by
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
01-075-1862;
01-086-2270
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340
00-004-0587
01-074-1132;
01-075-1620;
00-022-1235;
01-086-2270
01-080-2171;
01-080-2172;
01-080-1385
01-075-1862;
01-086-2270;
01-086-2340
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
F-302
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 303 of 478
Pos. [°2Th.]
66.0890
66.2624
68.1164
68.2714
69.5627
70.4707
71.2121
71.3126
72.4843
73.5983
73.8056
75.1396
75.3574
76.7270
77.2730
78.1327
80.9317
82.5348
83.8500
84.1032
85.8574
Height [cts]
6803.63
6527.04
2233.90
1523.40
642.41
686.48
1845.49
1884.33
922.59
1891.49
1608.36
7570.65
4283.81
872.54
921.51
687.00
356.77
515.05
4674.62
2433.55
193.86
FWHM
[°2Th.]
0.0840
0.0960
0.0720
0.0960
0.1920
0.3840
0.0960
0.0720
0.1920
0.1080
0.1440
0.1320
0.0720
0.1440
0.3840
0.1920
0.2880
0.2400
0.1080
0.1200
0.4320
d-spacing [A]
1.41264
1.41287
1.37545
1.37270
1.35034
1.33515
1.32306
1.32144
1.30294
1.28595
1.28285
1.26335
1.26337
1.24112
1.23371
1.22227
1.18691
1.16787
1.15287
1.15290
1.13098
Rel. Int. [%]
10.82
10.38
3.55
2.42
1.02
1.09
2.94
3.00
1.47
3.01
2.56
12.04
6.81
1.39
1.47
1.09
0.57
0.82
7.43
3.87
0.31
Matched by
01-077-2064;
01-075-1620
01-075-1862;
00-022-1235
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620
01-075-1862
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620
00-004-0587;
00-022-1235;
01-086-2340
00-004-0587;
00-022-1235;
01-086-2340
01-077-2064
01-075-1862;
01-086-2340
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327;
00-022-1235
01-075-1620
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-086-2340
01-074-1132;
01-075-1620;
F-303
-------
Pos. [°2Th.] Height [cts]
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 304 of 478
FWHM d-spacing [A] Rel. Int. [%] Matched by
[°2Th.]
86.2816
195.87
0.3840
1.12651
0.31
01-086-2270;
01-086-2340
01-075-1862
87.5269
88.8470
90.2516
90.5052
91.1040
93.9747
94.4142
94.6861
95.0850
98.1469
99.2347
100.9637
101.3170
104.5693
107.6114
108.4108
109.8302
109.9223
331.26
206.57
362.61
275.86
424.53
860.17
1499.98
1425.28
1047.41
201.52
362.05
1882.91
1355.04
110.46
477.33
424.10
2563.80
2103.32
0.2400
0.1920
0.0960
0.1440
0.2640
0.2400
0.2160
0.1440
0.1920
0.3840
0.6720
0.0960
0.1680
0.4800
0.1200
0.1920
0.0600
0.0840
1.11366
1.10050
1.08698
1.08460
1.07902
1.05347
1.04972
1.05002
1.04408
1.01952
1.01124
0.99854
0.99849
0.97376
0.95450
0.94967
0.94134
0.94081
0.53
0.33
0.58
0.44
0.68
1.37
2.39
2.27
1.67
0.32
0.58
2.99
2.16
0.18
0.76
0.67
4.08
3.35
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-043-1022
00-004-0587;
00-004-0864
00-004-0587
00-043-1022
00-043-1022
F-304
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 305 of 478
8.4: 2488-L-SC
8.4.1: Measurement Conditions of 2488-L
Dataset Name
File name
SC, no cover.sd
Sample Identification 2488-L-SC, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 9/21/2010 9:26:00 PM
2488-L-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2488-L-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
8.4.2: Main Graphics, Analyze View of 2488-L
F-305
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 306 of 478
2488-L-SC, no cover
Aluminum Oxide (01-075-1865
Potassium Chloride (01-075-02
Sodium Chloride (01-072-1668;
Spinel (01-086-2258)
Aluminum Nitride (01-076-056!
Aluminum (01-085-1327)
96)
10 20 30 40 50 60 70 80
Position [°2"meta] (Copper (Cu))
90 100 110
Aluminum Oxide Nitride 14.1 %|
Aluminum Oxide 13.1 %
Aluminum Oxide Nitride 10.1 % ]
Magnesium Aluminum Oxide 9.1 %
| Aluminum Oxide Nitride 7.1 % |
Sodium Chloride 19.2%
AlumT^1*6-syn 5/l ^l
F-306
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 307 of 478
8.4.3: Pattern List of 2488-L
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
40
44
57
53
50
16
17
18
32
33
20
20
17
17
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
3
5
19
9
6
14
10
7
1
2
3
2
5
13
Matched
Lines
18
10
9
16
11
13
13
12
5
6
5
14
38
13
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-307
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 308 of 478
8.4.4: Peak List of 2488-L
Pos. [°2Th.]
9.9836
10.1092
18.9958
23.0858
25.5650
26.6043
27.3506
28.3280
29.3837
31.6768
33.1465
33.7963
35.1003
35.9975
36.7969
36.8542
37.8759
38.4732
40.5299
41.7476
42.8747
43.3154
44.7716
45.3896
45.4503
Height |cts]
368~80
363.58
2611.99
115.11
1805.22
625.39
6587.71
20731.34
706.88
69470.19
5498.52
1176.64
3462.70
4301.70
11361.08
12682.59
4885.30
2554.39
11292.30
699.59
4075.19
3774.52
8715.42
36414.25
30910.50
FWHM
[°2Th.]
0.0295
0.2362
0.1771
0.2362
0.0492
0.1378
0.0787
0.1968
0.1574
0.1968
0.0787
0.2362
0.0492
0.1968
0.0960
0.0590
0.2755
0.1771
0.1476
0.3149
0.1771
0.0787
0.1378
0.1560
0.0480
d-spacing [A]
O6002
8.75022
4.67201
3.85273
3.48445
3.35065
3.26089
3.15056
3.03973
2.82472
2.70276
2.65226
2.55666
2.49497
2.44056
2.43892
2.37545
2.33993
2.22581
2.16367
2.10936
2.08892
2.02430
1.99651
1.99894
Rel7lnt7[%]
O53
0.52
3.76
0.17
2.60
0.90
9.48
29.84
1.02
100.00
7.91
1.69
4.98
6.19
16.35
18.26
7.03
3.68
16.25
1.01
5.87
5.43
12.55
52.42
44.49
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
01-075-1862
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
F-308
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 309 of 478
Pos. [°2Th.]
46.9450
49.7428
50.1205
52.4943
53.7825
54.9262
55.6555
56.3745
56.5651
57.4318
58.6125
59.2815
61.2395
62.2524
65.1719
65.3614
66.1205
66.3260
68.1175
69.6324
71.2904
72.5322
73.6103
Height [cts]
891.36
1589.17
2911.19
1327.64
1294.62
500.91
1278.42
9156.96
4937.78
2796.43
1805.32
5536.44
597.07
1807.38
7344.82
6387.29
5914.47
5370.27
1573.61
420.23
1263.66
774.78
1457.80
FWHM
[°2Th.]
0.2400
0.1680
0.0960
0.2160
0.0840
0.2880
0.2400
0.1560
0.0960
0.1680
0.1680
0.1920
0.1920
0.1920
0.0960
0.1680
0.0840
0.0960
0.1680
0.2880
0.1200
0.2880
0.2160
d-spacing [A]
1.93393
1.83150
1.81858
1.74180
1.70308
1.67029
1.65012
1.63076
1.62976
1.60323
1.57372
1.55754
1.51235
1.49016
1.43028
1.42659
1.41204
1.41167
1.37543
1.34916
1.32180
1.30220
1.28577
Rel. Int. [%]
1.28
2.29
4.19
1.91
1.86
0.72
1.84
13.18
7.11
4.03
2.60
7.97
0.86
2.60
10.57
9.19
8.51
7.73
2.27
0.60
1.82
1.12
2.10
Matched by
00-004-0864;
01-086-2270
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327
01-074-1132;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620
00-004-0587;
00-022-1235
73.8729
1366.56
0.1440
1.28503
1.97
F-309
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 310 of 478
Pos. [°2Th.]
75.1704
75.4116
76.7748
77.2771
78.1806
78.5484
80.9134
82.5592
83.8836
84.1275
85.7196
87.5887
88.9180
90.2602
91.0329
94.0144
94.4416
95.1194
98.1511
99.2404
100.9959
101.3700
104.6935
107.6151
108.5395
Height [cts]
7629.55
4067.26
617.23
984.14
713.16
632.00
210.23
685.68
4642.22
2499.40
181.62
296.89
132.56
315.87
392.10
1110.96
1337.13
812.34
142.95
483.55
1618.40
1072.07
60.87
268.40
46.84
FWHM
[°2Th.]
0.1560
0.1200
0.1440
0.2880
0.1920
0.2400
0.6720
0.2400
0.1320
0.1080
0.3840
0.2160
0.1920
0.1920
0.3840
0.2160
0.2880
0.1440
0.3840
0.2400
0.1680
0.1680
0.7680
0.1440
0.2880
d-spacing [A]
1.26291
1.26260
1.24047
1.23365
1.22164
1.21684
1.18713
1.16759
1.15249
1.15263
1.13245
1.11303
1.09980
1.08690
1.07968
1.05313
1.04949
1.04379
1.01949
1.01120
0.99831
0.99811
0.97294
0.95448
0.94891
Rel. Int. [%]
10.98
5.85
0.89
1.42
1.03
0.91
0.30
0.99
6.68
3.60
0.26
0.43
0.19
0.45
0.56
1.60
1.92
1.17
0.21
0.70
2.33
1.54
0.09
0.39
0.07
Matched by
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327
01-074-1132;
00-043-1022;
01-086-2270
01-075-1620
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064
01-074-1132;
01-075-1620;
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385
01-075-1862;
01-086-2270
00-022-1235
00-043-1022;
00-004-0864
00-004-0587;
00-004-0864
00-004-0587
F-310
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 311 of 478
8.5: 2490-L-SC
8.5.1: Measurement Conditions of 2490-L
Dataset Name
File name
no cover.sd
Sample Identification 2490-L-sc, no cover
Comment Exported by X'Pert SW
Generated by todd in project Ft. Devens.
2490-L-sc, no cover
C:\DocumentsandSettings\xhuang\Desktop\SAP-xrd\9-24-10\2490-L-sc,
Measurement Date / Time
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
9/5/2010 8:05:00 PM
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
8.5.2: Main Graphics, Analyze View of 2490-L
F-311
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 312 of 478
V V V V
2490-L-sc, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
• Periclase, syn (00-043-1022)
50 60 70 80
Position [°2Theta] (Copper (Cu))
Aluminum Qxide 7.9 %]
Magnesium Aluminum Oxide 7.9 % \ s'
I Aluminum Oxide 7.9 % I ^^.
Sylvite,syn 6.9 %
I Anhydrite 6.9 %
Aluminum Qxide Nitride 5.9 % |
| Fluorite, syn 5 %
Aluminum Oxide Nitride 8.9 %
sodium Chloride 17.8 %|
! Aluminum ^ % |
\ Calcite 1 % [.n 2 % I
luminum Oxide Nitride 5 % |
Quaij
Aluminum Nitride 5 %
F-312
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 313 of 478
8.5.3: Pattern List of 2490-L
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-086-
2340
01-085-
0930
Score
56
50
45
39
35
17
19
20
39
26
16
27
21
17
20
36
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Calcite
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Ca ( C O3 )
Si O2
8
7
18
8
5
9
6
5
3
2
5
4
7
8
1
5
Matched
Lines
21
10
9
12
10
12
13
13
5
7
5
16
35
13
17
24
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-313
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 314 of 478
8.5.4: Peak List of 2490-L
Pos. [°2Th.]
13.9434
16.3217
18.9503
20.7789
21.9484
22.9884
24.4591
25.4737
26.5291
27.2518
27.2912
28.2530
29.3434
30.8345
31.5939
31.6526
33.1128
33.7065
35.0331
35.9131
36.7538
37.6834
38.3717
38.4486
39.3759
40.4343
41.7013
Height [cts]
72.51
204.79
1634.08
1570.76
358.61
447.68
682.07
2820.43
8441.70
5870.92
5480.58
15819.85
2420.24
2588.91
57775.62
48911.32
4839.31
1303.03
5144.83
3743.25
7538.44
4656.64
6108.86
5791.40
1514.11
8875.04
856.98
[°2Th.]
0.3149
0.1378
0.1574
0.0394
0.1574
0.2362
0.1378
0.0886
0.1476
0.0960
0.0689
0.1279
0.2362
0.1181
0.1560
0.0960
0.2400
0.2880
0.1440
0.1920
0.1680
0.1080
0.1200
0.0720
0.1680
0.0720
0.2880
d-spacing [A]
6.35148
5.43095
4.68314
4.27495
4.04974
3.86883
3.63944
3.49673
3.35998
3.26978
3.26785
3.15875
3.04381
2.89993
2.82960
2.83151
2.70319
2.65692
2.55929
2.49857
2.44332
2.38516
2.34395
2.34525
2.28645
2.22901
2.16417
ReLIntM
0.13
0.35
2.83
2.72
0.62
0.77
1.18
4.88
14.61
10.16
9.49
27.38
4.19
4.48
100.00
84.66
8.38
2.26
8.90
6.48
13.05
8.06
10.57
10.02
2.62
15.36
1.48
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
00-022-1235
01-086-2270;
01-086-2340
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
01-077-2064
00-004-0587;
00-004-0864
01-086-2340
01-077-2064
01-075-1620
01-075-1862
01-075-1620;
01-086-2340
01-074-1132;
00-043-1022
01-075-1862;
01-080-2172;
01-080-2173;
01-080-1385
01-074-1132;
01-085-1327;
00-022-1235
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-086-2340;
01-085-0930
00-004-0587;
01-085-0930
01-075-1862
F-314
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 315 of 478
Pos. [°2Th.]
42.3730
42.7898
43.2697
44.6701
45.3316
47.2041
48.4757
49.7326
50.0286
50.1639
52.4356
53.7319
54.7447
55.5834
56.3382
57.3637
57.5393
58.5857
59.2462
59.8436
Height [cts]
1343.82
3335.86
5380.39
7222.10
29137.50
1051.08
693.00
1609.69
3643.58
3407.65
2110.76
1248.28
661.55
1076.34
7481.57
4055.92
2673.22
1700.09
3692.65
1812.01
FWHM
[°2Th.]
0.1920
0.2160
0.1320
0.2400
0.2040
0.2880
0.2880
0.2400
0.0840
0.0960
0.0960
0.1920
0.1440
0.1920
0.1080
0.1560
0.1080
0.2880
0.2160
0.1440
d-spacing [A]
2.13140
2.11160
2.08928
2.02698
1.99893
1.92391
1.87637
1.83185
1.82171
1.81711
1.74361
1.70456
1.67540
1.65209
1.63173
1.60497
1.60447
1.57437
1.55839
1.54425
Rel. Int. [%]
2.33
5.77
9.31
12.50
50.43
1.82
1.20
2.79
6.31
5.90
3.65
2.16
1.15
1.86
12.95
7.02
4.63
2.94
6.39
3.14
Matched by
01-085-0930
00-043-1022
01-075-1862;
01-086-2270;
01-086-2340
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270;
01-086-2340
01-086-2340
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-085-0930
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862;
01-086-2340;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-085-0930
F-315
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 316 of 478
Pos. [°2Th.]
60.5408
61.1862
62.1769
65.0974
66.0759
66.3728
67.6041
68.0419
68.2619
69.5553
71.2727
72.4147
73.5976
75.1463
Height [cts]
891.27
805.13
1396.48
4917.93
5090.58
4590.83
809.10
2497.18
1806.20
429.66
998.69
581.20
1339.57
5856.04
FWHM
[°2Th.]
0.2880
0.1680
0.1680
0.0960
0.1680
0.2400
0.1440
0.0960
0.1200
0.3840
0.3840
0.2880
0.1920
0.0960
d-spacing [A]
1.52812
1.51354
1.49178
1.43174
1.41289
1.40729
1.38462
1.37677
1.37287
1.35047
1.32209
1.30402
1.28596
1.26325
Rel. Int. [%]
1.54
1.39
2.42
8.51
8.81
7.95
1.40
4.32
3.13
0.74
1.73
1.01
2.32
10.14
Matched by
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385;
01-086-2340
01-075-1862;
01-086-2270;
01-086-2340
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2340
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-085-0930
01-075-1862;
01-085-0930
01-075-1862;
00-022-1235;
01-085-0930
01-074-1132;
01-075-1620;
00-022-1235
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620
00-004-0587;
00-022-1235;
01-086-2340;
01-085-0930
01-077-2064
F-316
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 317 of 478
Pos. [°2Th.]
75.3723
76.7245
77.1631
78.1213
79.7424
80.5440
81.3327
82.3686
83.8093
84.1029
86.3134
87.6025
88.8485
90.2461
91.0015
93.8955
94.4412
95.0828
95.4108
99.0685
100.9613
101.2834
104.6490
107.5405
109.9041
Height [cts]
3345.79
839.25
815.86
1226.80
276.10
318.87
321.37
564.82
3538.21
1934.09
166.50
213.83
198.55
198.66
415.85
586.15
954.62
847.05
410.11
261.86
1303.77
953.31
41.09
308.58
1640.49
FWHM
[°2Th.]
0.1440
0.1680
0.4800
0.0960
0.1920
0.1920
0.1920
0.4800
0.1920
0.1920
0.3840
0.6720
0.1920
0.5760
0.1680
0.2880
0.3840
0.2160
0.1440
0.5760
0.2640
0.2400
0.7680
0.4800
0.0600
d-spacing [A]
1.26003
1.24115
1.23519
1.22242
1.20160
1.19164
1.18207
1.16981
1.15333
1.15290
1.12617
1.11289
1.10048
1.08704
1.07997
1.05415
1.04949
1.04410
1.04396
1.01249
0.99856
0.99873
0.97323
0.95493
0.94091
Rel. Int. [%]
5.79
1.45
1.41
2.12
0.48
0.55
0.56
0.98
6.12
3.35
0.29
0.37
0.34
0.34
0.72
1.01
1.65
1.47
0.71
0.45
2.26
1.65
0.07
0.53
2.84
Matched by
01-077-2064;
01-080-2171
01-075-1862;
01-086-2340
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327;
00-022-1235
01-080-2171;
01-086-2270;
01-085-0930
01-075-1862;
01-086-2340
01-086-2340;
01-085-0930
01-085-1327;
00-022-1235
01-077-2064;
01-086-2340;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-043-1022
00-004-0587;
00-004-0864
00-043-1022
F-317
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 318 of 478
FACILITY M
9.1: 2601-M-SC
9.1.1: Measurement Conditions of 2601-M
Dataset Name
File name
M-SC, no cover.udf
Sample Identification 2601-M-SC, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2601-M-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2601-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
F-318
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 319 of 478
9.1.2: Main Graphics, Analyze View of 2601-M
2601-M-SC, no cover
| Aluminum Oxide (01-075-1865
| Potassium Chloride (01-075-0^96)
Sodium Chloride (01-072-1668
Spinel (01-086-2258)
I Aluminum Nitride (01-076-056!
Aluminum (01-085-1327)
50 60 70
Position [°2Theta] (Copper (Cu))
Quartz low 16 % |
Sylvite, syn 14 %
Aluminum Oxide 10 %|
Aluminum Oxide Nitride 9 % |
["Aluminum 6 %~|
Sodium Chloride 20 % |
Aluminum Oxide 1 %
Aluminum iwiae
Aluminum Oxide Nitride 5 % |
Maj Elpasolite, syn 4 % |de 5 % |
Aluminum Oxide Nitride 6 % I
9.1.3: Pattern List of 2601-M
F-319
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 320 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-022-
1235
01-080-
1385
01-085-
0335
13
59
57
37
40
17
17
17
53
43
25
18
27
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Elpasolite,
syn
Aluminum
Oxide
Quartz low
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
K2 Na Al
F6
A12.667 O4
Si O2
1
14
20
5
2
9
6
5
6
2
4
10
16
13
10
9
11
8
13
12
11
5
7
15
12
18
0
0
0
0
0
0
0
0
0
0
0
0
0
F-320
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 321 of 478
9.1.4: Peak List of 2601-M
Pos. [°2Th.]
10.7952
18.9091
20.7829
21.9201
22.7481
24.4017
25.5133
26.5207
27.2758
28.2594
29.7320
31.6092
33.0930
35.9800
36.7924
37.7448
38.3758
38.4685
40.4187
40.4728
41.7279
42.8273
44.6131
45.3198
45.4466
47.3086
50.0631
Height [cts]
80.99
691.40
415.33
259.53
269.83
346.93
392.43
1777.72
6310.01
41263.36
779.94
63827.51
2367.24
2054.53
3876.62
2254.15
17098.49
14052.68
23329.81
21384.02
739.73
4173.59
8824.10
33122.64
20558.48
508.13
6294.47
FWHM
[°2Th.]
0.9446
0.1181
0.1181
0.4723
0.3149
0.1574
0.1574
0.1082
0.1771
0.1870
0.1181
0.2165
0.1378
0.1574
0.1574
0.1574
0.1560
0.0960
0.1440
0.0840
0.3840
0.1920
0.1320
0.1680
0.0600
0.2880
0.0600
d-spacing [A]
8.19563
4.69325
4.27415
4.05491
3.90916
3.64786
3.49140
3.36101
3.26966
3.15806
3.00490
2.83061
2.70700
2.49614
2.44287
2.38340
2.34371
2.34408
2.22984
2.23251
2.16285
2.10984
2.02944
1.99943
1.99910
1.91991
1.82053
ReLIntM
0.13
1.08
0.65
0.41
0.42
0.54
0.61
2.79
9.89
64.65
1.22
100.00
3.71
3.22
6.07
3.53
26.79
22.02
36.55
33.50
1.16
6.54
13.82
51.89
32.21
0.80
9.86
Matched by
01-074-1132;
00-022-1235
01-085-0335
00-022-1235
01-075-1862
01-085-0335
01-077-2064
00-004-0587
01-077-2064;
01-080-2171
01-075-1620
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0335
01-075-1862
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0335
F-321
-------
Pos. [°2Th.] Height [cts]
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 322 of 478
FWHM
[°2Th.]
d-spacing [A] Rel. Int. [%] Matched by
50.1750
52.4665
53.7233
54.8308
56.3108
56.4589
57.3551
58.5222
59.2552
62.1827
65.0280
65.1757
66.0611
66.2463
68.1213
71.2607
72.8957
73.5631
73.7680
5041.16
113.20
998.41
294.64
8250.92
5877.35
303.99
2670.71
1490.20
1505.85
4612.61
4066.73
5074.08
7380.27
183.32
350.59
442.95
2939.97
2100.24
0.0960
0.2880
0.1680
0.3360
0.1560
0.0960
0.1920
0.1320
0.1440
0.1200
0.1080
0.1680
0.1200
0.1320
0.2880
0.1920
0.1440
0.0720
0.1200
1.81674
1.74265
1.70481
1.67297
1.63246
1.63257
1.60519
1.57593
1.55817
1.49166
1.43310
1.43021
1.41317
1.40967
1.37536
1.32228
1.29660
1.28648
1.28341
7.90
0.18
1.56
0.46
12.93
9.21
0.48
4.18
2.33
2.36
7.23
6.37
7.95
11.56
0.29
0.55
0.69
4.61
3.29
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0335
01-075-1862
01-077-2064
01-085-0335
01-077-2064
01-075-1862;
01-085-0335
00-004-0587
01-074-1132;
01-075-1620;
00-022-1235
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-075-1620;
01-080-2171
01-075-1862;
00-022-1235;
01-085-0335
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-077-2064
00-004-0587;
00-022-1235;
01-085-0335
00-004-0587;
00-022-1235
F-322
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 323 of 478
Pos. [°2Th.]
75.1293
75.3467
78.1484
78.3788
82.3598
82.5884
83.8364
84.0893
87.4951
87.7896
90.2314
94.3412
94.6883
98.9889
101.0011
101.3365
101.6759
107.6004
108.3654
108.7931
109.8130
109.9386
Height [cts]
7015.62
3864.85
3172.29
2081.36
884.16
639.50
4132.72
2201.84
637.35
409.99
296.50
1445.67
1005.44
360.91
1207.88
1327.86
565.79
368.51
659.71
533.28
2400.84
1722.45
FWHM
[°2Th.]
0.1680
0.1200
0.1800
0.1440
0.1920
0.1440
0.1440
0.1200
0.1200
0.1440
0.1440
0.2400
0.1920
0.1920
0.1680
0.2160
0.1920
0.1680
0.2160
0.1920
0.0840
0.0600
d-spacing [A]
1.26350
1.26352
1.22206
1.22208
1.16991
1.17015
1.15302
1.15306
1.11398
1.11100
1.08717
1.05034
1.05001
1.01309
0.99827
0.99588
0.99594
0.95457
0.94995
0.94975
0.94144
0.94071
Rel. Int. [%]
10.99
6.06
4.97
3.26
1.39
1.00
6.47
3.45
1.00
0.64
0.46
2.26
1.58
0.57
1.89
2.08
0.89
0.58
1.03
0.84
3.76
2.70
Matched by
01-077-2064
01-085-1327;
00-022-1235
01-085-1327;
00-022-1235
01-077-2064;
01-085-0335
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0335
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
00-022-1235
00-004-0587
00-022-1235
00-004-0587
00-004-0587
00-043-1022
00-043-1022
F-323
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 324 of 478
9.2: 2605-M-SC
9.2.1: Measurement Conditions of 2605-M
Dataset Name
File name
M-SC, no cover.udf
Sample Identification 2605-M-SC, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2605-M-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2605-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
9.2.2: Main Graphics, Analyze View of 2605-M
F-324
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 325 of 478
V V V
2605-M-SC, no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0;
• Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
• Periclase, syn (00-043-1022)
4«<
50 60 70 80
Position [°2Theta] (Copper (Cu))
Aluminum Oxide 14%
Aluminum Oxide Nitride 10 %
Aluminum Oxide Nitride 9 %
Aluminum Oxide 6 %
Aluminum Oxide Nitride 14 %
Sodium Chloride 17 %\
j--.. L_ * i-ir i
, Periclase, syn 1 %
Aluminum 3 % I
Fluorite, syn 3 %
Sylvite, syn 5 % |
I Anhydrite 5 % I
' ^^^-^^^^^^^^^^^^J.
Maqrj Aluminum Nitride 4 % fe % I
9.2.3: Pattern List of 2605-M
F-325
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 326 of 478
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
Score
48
46
58
42
35
20
20
20
50
34
18
25
16
22
18
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
6
5
17
5
4
14
10
9
3
1
3
3
5
14
1
Matched
Lines
21
10
9
14
8
13
13
13
5
7
5
14
37
13
21
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-326
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 327 of 478
9.2.4: Peak List of 2605-M
as. [°2Th.]
"1L0434
16.2083
18.2540
18.9663
20.8276
22.0289
25.5302
26.5930
27.3005
28.3000
29.3555
30.8699
31.6428
33.1367
35.0696
35.9591
36.8139
37.7218
38.4300
39.3523
40.4376
42.8607
43.2767
Height [cts]
7L69
35.85
450.49
804.77
218.70
87.69
2054.42
968.70
4298.76
16362.88
1297.92
2660.29
44042.39
3685.76
4811.97
3458.83
5612.81
5518.87
7905.10
2361.27
9446.08
1976.19
4102.97
FWHM
[°2Th.]
0.6298
0.4723
0.1181
0.1181
0.2362
0.4723
0.1771
0.1181
0.1476
0.1771
0.1574
0.1574
0.1181
0.1574
0.0984
0.1181
0.2165
0.1378
0.1181
0.2362
0.0886
0.1968
0.0492
d-spacing [A]
8XJ1202
5.46870
4.86019
4.67922
4.26507
4.03513
3.48913
3.35204
3.26676
3.15361
3.04258
2.89669
2.82768
2.70354
2.55883
2.49755
2.44150
2.38479
2.34246
2.28966
2.23068
2.11002
2.09070
Rel. Int. [%]
OT6
0.08
1.02
1.83
0.50
0.20
4.66
2.20
9.76
37.15
2.95
6.04
100.00
8.37
10.93
7.85
12.74
12.53
17.95
5.36
21.45
4.49
9.32
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
00-022-1235
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620;
01-080-2172;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
00-004-0587;
01-085-0930
00-043-1022
01-075-1862;
01-086-2270
F-327
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 328 of 478
Pos. [°2Th.]
44.6647
45.3579
47.3863
49.7019
50.0879
52.4502
53.7818
54.9415
56.3460
56.5358
57.4147
58.5601
59.2742
61.1885
62.2261
65.0238
66.1384
66.2911
67.1271
68.1396
71.3250
72.9472
Height [cts]
5732.21
23614.84
1223.31
609.59
2436.18
1205.26
696.33
137.78
5522.21
3136.56
2839.89
1363.59
1735.90
1008.87
1096.10
3365.46
5859.34
6849.69
4700.37
2504.70
265.82
265.01
FWHM
[°2Th.]
0.1771
0.1181
0.4723
0.1181
0.0590
0.1181
0.1181
0.2362
0.1560
0.0960
0.1320
0.1200
0.3360
0.2880
0.3840
0.1200
0.0840
0.0960
0.4800
0.1440
0.3840
0.1440
d-spacing [A]
2.02890
1.99949
1.91853
1.83443
1.82120
1.74460
1.70451
1.67124
1.63152
1.63053
1.60367
1.57500
1.55772
1.51349
1.49072
1.43318
1.41171
1.41232
1.39329
1.37504
1.32125
1.29581
Rel. Int. [%]
13.02
53.62
2.78
1.38
5.53
2.74
1.58
0.31
12.54
7.12
6.45
3.10
3.94
2.29
2.49
7.64
13.30
15.55
10.67
5.69
0.60
0.60
Matched by
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-086-2270
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-085-0930
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270
00-043-1022;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-075-1620
01-086-2270
01-075-1862;
00-022-1235;
01-085-0930
01-075-1620;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-077-2064;
01-086-2270
F-328
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 329 of 478
Pos. [°2Th.]
73.6084
73.8133
75.1673
75.4010
76.7785
77.1643
78.1334
80.5968
82.3550
83.8607
84.1195
86.3348
87.5260
88.9110
90.2532
91.0674
94.4347
94.7286
95.1218
99.0492
101.0024
101.3244
101.7300
107.6132
108.4422
109.9386
Height [cts]
1272.26
869.04
4856.19
2425.76
525.79
456.38
1517.48
148.68
387.56
3141.00
1684.14
179.02
307.09
165.94
195.66
216.39
771.06
596.36
534.45
208.15
1222.30
1058.33
386.57
277.77
331.97
1260.07
FWHM
[°2Th.]
0.1200
0.0960
0.1560
0.0600
0.1680
0.2880
0.1680
0.2880
0.4320
0.1320
0.0960
0.2880
0.1680
0.2400
0.1920
0.1440
0.1680
0.1440
0.1920
0.5760
0.2160
0.1440
0.1920
0.1920
0.1920
0.0240
d-spacing [A]
1.28580
1.28592
1.26295
1.26275
1.24042
1.23517
1.22226
1.19100
1.16997
1.15275
1.15272
1.12595
1.11367
1.09987
1.08697
1.07936
1.04955
1.04967
1.04377
1.01264
0.99826
0.99844
0.99309
0.95449
0.94949
0.94071
Rel. Int. [%]
2.89
1.97
11.03
5.51
1.19
1.04
3.45
0.34
0.88
7.13
3.82
0.41
0.70
0.38
0.44
0.49
1.75
1.35
1.21
0.47
2.78
2.40
0.88
0.63
0.75
2.86
Matched by
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327;
00-022-1235
01-075-1862
01-085-1327;
00-022-1235
01-077-2064;
01-085-0930
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-004-0587;
00-004-0864
00-004-0587;
00-022-1235
00-004-0587
00-043-1022
F-329
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 330 of 478
9.3: 2609-M-SC
9.3.1: Measurement Conditions of 2609-M
Dataset Name
File name
M-SC-NO COVER_004.udf
Sample Identification
Comment
2609-M-SC-NO COVER_004
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2609-
2609-M-SC-NO COVER
Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
9.3.2: Main Graphics, Analyze View of 2609-M
F-330
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 331 of 478
2609-M-SC-NO COVER_004
• Potassium Chloride (01-075-0296)
• Sodium Chloride (01-072-1668)
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-0565)
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
• Periclase, syn (00-043-1022)
10 20 30 40 50 60 70 80 90 100 110
Position [°2Theta] (Copper (Cu))
Sylvite, syn 11.1 % |
Sodium Chloride 11.1 %
Aluminum Oxide Nitride 11.1 %
Magnesium Aluminum Oxide 13.1 % |
Aluminum 18.2%
Aluminum NJtrirjp 2 %
Quartz 1 % I. ...... ... , ,,, \
.,.., ~,...ite Nitride b.1 % |
El| Periclase, syn 2 %|
Aluminum Oxide 10.1 % | | Aluminum Oxide Nitride 8.1 % |
9.3.3: Pattern List of 2609-M
F-331
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 332 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-022-
1235
01-080-
1385
01-085-
0930
59
61
17
43
20
18
19
48
38
24
19
31
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Elpasolite,
syn
Aluminum
Oxide
Quartz
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
K2 Na Al
F6
A12.667 O4
Si O2
11
11
13
2
11
8
6
18
2
6
10
1
10
9
10
7
11
11
11
5
7
15
11
18
0
0
0
0
0
0
0
0
0
0
0
0
F-332
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 333 of 478
9.3.4: Peak List of 2609-M
Pos. [°2Th.]
11.0271
18.9736
20.8501
22.3149
24.5188
25.5722
26.6616
27.4165
28.3666
31.7237
33.2442
36.0661
36.9418
37.9159
38.5207
38.5978
40.5313
41.8019
42.9720
44.7760
45.4388
47.4168
50.2206
52.4305
53.8529
Height [cts]
106.72
137.21
117.52
164.78
63.06
35.54
589.51
1490.28
17468.05
17206.39
573.62
568.56
984.11
1015.45
31310.20
25117.45
11725.92
468.69
2345.03
15574.33
12040.88
222.49
3870.50
55.64
428.85
FWHM
[°2Th.]
0.5510
0.1574
0.1181
0.1574
0.1574
0.2362
0.0984
0.1279
0.1574
0.1771
0.1968
0.1574
0.2362
0.1968
0.1560
0.0720
0.2280
0.2400
0.1920
0.2040
0.1680
0.3840
0.1800
0.5760
0.1440
d-spacing [A]
8.02385
4.67743
4.26051
3.98406
3.63070
3.48349
3.34358
3.25320
3.14637
2.82065
2.69504
2.49038
2.43334
2.37303
2.33522
2.33653
2.22390
2.15919
2.10307
2.02244
1.99447
1.91578
1.81519
1.74376
1.70102
ReLIntM
0.34
0.44
0.38
0.53
0.20
0.11
1.88
4.76
55.79
54.95
1.83
1.82
3.14
3.24
100.00
80.22
37.45
1.50
7.49
49.74
38.46
0.71
12.36
0.18
1.37
Matched by
01-074-1132;
00-022-1235
01-085-0930
01-085-0930
01-077-2064
00-004-0587
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1620
01-074-1132;
00-043-1022
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0930
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-080-2171;
01-080-2172;
01-080-1385
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-077-2064
F-333
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 334 of 478
Pos. [°2Th.]
54.9566
56.4391
56.6254
58.6533
59.3971
62.3101
65.1589
65.3442
66.4043
68.2147
71.4365
73.7290
73.9363
75.2877
75.4827
78.2995
78.5343
82.4912
82.7939
83.9821
84.2358
87.6639
90.3969
94.5101
Height [cts]
71.53
3411.50
2092.83
1757.27
641.59
1185.95
9795.49
6634.39
4930.29
113.68
214.83
2420.82
1654.13
3662.02
2081.48
9333.36
5930.83
2623.05
1450.86
2285.27
1219.05
530.50
180.38
1141.18
FWHM
[°2Th.]
0.2880
0.1800
0.0960
0.0960
0.3840
0.3360
0.1680
0.1440
0.1560
0.3360
0.2880
0.1920
0.1440
0.1080
0.0960
0.1560
0.1680
0.2400
0.1680
0.1920
0.1200
0.2400
0.1440
0.2160
d-spacing [A]
1.66944
1.62905
1.62817
1.57272
1.55479
1.48891
1.43054
1.43047
1.40670
1.37371
1.31946
1.28399
1.28409
1.26123
1.26158
1.22008
1.22005
1.16838
1.16777
1.15139
1.15143
1.11227
1.08561
1.04891
Rel. Int. [%]
0.23
10.90
6.68
5.61
2.05
3.79
31.29
21.19
15.75
0.36
0.69
7.73
5.28
11.70
6.65
29.81
18.94
8.38
4.63
7.30
3.89
1.69
0.58
3.64
Matched by
01-085-0930
01-077-2064;
01-080-2171
00-004-0587
01-074-1132;
01-075-1620
00-043-1022
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
00-022-1235;
01-085-0930
01-075-1620;
01-080-2173
00-004-0587;
00-022-1235
01-077-2064;
01-080-2171
01-074-1132;
01-085-1327
01-074-1132;
01-085-1327
01-077-2064;
01-085-0930
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
00-022-1235
00-004-0587
F-334
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 335 of 478
Pos. [°2Th.]
94.8816
99.1251
99.4947
101.1521
101.4865
107.7619
108.5761
109.8260
Height [cts]
803.37
894.93
651.96
762.15
1028.08
359.21
787.44
1282.58
FWHM
[°2Th.]
0.1920
0.1680
0.1440
0.0960
0.1680
0.1920
0.2400
0.0600
d-spacing [A]
1.04838
1.01207
1.01181
0.99719
0.99728
0.95358
0.94869
0.94136
Rel. Int. [%]
2.57
2.86
2.08
2.43
3.28
1.15
2.51
4.10
Matched by
00-004-0587
00-004-0587
00-043-1022
F-335
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 336 of 478
9.4: 2613-M-SC
9.4.1: Measurement Conditions of 2613-M
Dataset Name
File name
M-SC, no cover.udf
Sample Identification 2613-M-SC, no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2613-M-SC, no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2613-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
9.4.2: Main Graphics, Analyze View of 2613-M
F-336
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 337 of 478
V V
30000 -
20000 -
10000-
2613-M-SC, no cover
• Aluminum Oxide (01-075-J865)
• Potassium Chloride (01-0
Sodium Chloride (01-072
• Spinel (01-086-2258)
• Aluminum Nitride (01-076
Aluminum (01 -085-1 327)
• Quartz, syn (01-083-2467
• Periclase,
syn (00-043-1 0
i
'5-0296)
1668,
056
, ?
i ,iA
i i i i i i
/-I
\
|
A.,'
'
i
,!
'i i i \
'"••'' : :_ ^ A-AA :
50 60 70
Position [°2Theta] (Copper (Cu))
Sodium Chloride W2%] I Sylvrte, syn 13.3 %|
Magnesium Aluminum Oxide 8.2 %
l'-HI I III I'-HI I I ••_••.•••.I'-H'_- I ^ILI I'-H'_- -T . 1 ?O
Aluminum Oxide Nitride 8.2 %
9.4.3: Pattern List of 2613-M
F-337
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 338 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
31
60
60
27
45
19
18
16
54
38
11
22
15
19
35
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
2
13
11
8
3
8
5
4
14
2
8
6
6
7
1
13
10
9
10
9
11
11
10
5
7
4
15
29
11
20
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-338
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 339 of 478
9.4.4: Peak List of 2613-M
Pos. [°2Th.]
10.8753
18.9541
20.7727
22.2170
24.4069
25.5042
26.5600
27.2728
28.2718
30.8285
31.6184
33.1255
35.0621
35.9197
36.8277
37.8248
38.3942
38.4825
40.4331
40.5197
41.7410
42.8030
43.2797
44.6402
45.3184
Height |cts]
77/78
333.80
396.97
419.25
403.09
739.96
2136.08
3485.10
34898.57
1658.69
33109.27
2715.09
1274.61
1982.82
2143.27
2787.10
35843.59
29718.26
21572.14
17682.13
1493.96
3984.38
3268.84
21868.60
21623.98
FWHM
[°2Th.]
0.5510
0.1968
0.1574
0.2362
0.1574
0.0787
0.1574
0.0689
0.1771
0.1574
0.1771
0.1771
0.1378
0.0886
0.1279
0.2362
0.1680
0.0720
0.2160
0.0480
0.2640
0.2400
0.1920
0.2040
0.1560
d-spacing [A]
813545
4.68221
4.27623
4.00138
3.64710
3.49262
3.35613
3.27001
3.15670
2.90048
2.82981
2.70442
2.55936
2.50020
2.44062
2.37854
2.34263
2.34326
2.22907
2.23003
2.16220
2.11098
2.08883
2.02827
1.99949
Rel7lnt7[%]
022
0.93
1.11
1.17
1.12
2.06
5.96
9.72
97.36
4.63
92.37
7.57
3.56
5.53
5.98
7.78
100.00
82.91
60.18
49.33
4.17
11.12
9.12
61.01
60.33
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0930
01-075-1862
00-043-1022
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
F-339
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 340 of 478
Pos. [°2Th.]
45.4210
47.2957
50.0962
51.7508
52.4394
53.7463
54.8338
56.3302
56.5045
57.3798
58.5292
59.2470
62.2321
64.9783
65.0323
65.1830
66.0632
66.2862
Height [cts]
17215.03
1662.81
7283.83
1639.07
1381.99
974.70
268.47
5217.73
2900.22
687.38
2506.84
1359.80
1107.71
8149.34
9266.65
6942.95
3970.63
6356.56
FWHM
[°2Th.]
0.0960
0.3840
0.1080
0.8640
0.2400
0.1080
0.2880
0.1560
0.1200
0.1200
0.2160
0.1920
0.1680
0.0840
0.0600
0.1920
0.0720
0.1200
d-spacing [A]
2.00016
1.92040
1.81941
1.76506
1.74349
1.70414
1.67288
1.63194
1.63136
1.60456
1.57576
1.55837
1.49059
1.43408
1.43301
1.43007
1.41313
1.40891
Rel. Int. [%]
48.03
4.64
20.32
4.57
3.86
2.72
0.75
14.56
8.09
1.92
6.99
3.79
3.09
22.74
25.85
19.37
11.08
17.73
Matched by
01-086-2270
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-085-0930
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
00-022-1235;
01-086-2270
00-043-1022;
01-086-2270
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327;
00-022-1235
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064;
01-075-1620;
01-085-0930
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-1385
F-340
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 341 of 478
Pos. [°2Th.]
68.0560
m__™mm
72.4562
72.9047
73.5537
75.1236
75.3626
78.1198
78.3976
81.0453
82.3432
82.6258
83.8250
84.0847
87.4761
90.2426
94.4121
94.6972
98.9376
100.9349
101.3004
107.5799
108.4313
109.9364
Height [cts]
408.60
•-•-•-——•--
238.71
356.42
2809.07
4503.63
2393.45
7426.22
4771.55
86.77
2092.80
1241.98
2689.96
1454.45
585.59
176.75
1392.59
998.42
749.04
960.38
1257.34
270.18
653.04
1261.24
FWHM
[°2Th.]
0.1920
_„__
0.2880
0.1440
0.1680
0.1200
0.1440
0.1800
0.1680
0.5760
0.2160
0.1920
0.1200
0.0960
0.1200
0.1920
0.1680
0.1440
0.1920
0.1680
0.1200
0.1920
0.2400
0.0840
d-spacing [A]
1.37652
-'-———'-
1.30338
1.29646
1.28662
1.26358
1.26330
1.22244
1.22183
1.18553
1.17010
1.16972
1.15315
1.15311
1.11417
1.08707
1.04974
1.04993
1.01348
0.99875
0.99861
0.95469
0.94955
0.94073
Rel. Int. [%]
1.14
mm_™™mmm
0.67
0.99
7.84
12.56
6.68
20.72
13.31
0.24
5.84
3.47
7.50
4.06
1.63
0.49
3.89
2.79
2.09
2.68
3.51
0.75
1.82
3.52
Matched by
01-075-1862;
00-022-1235;
01-085-0930
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-075-1620
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-085-1327;
00-022-1235
01-075-1620;
01-085-0930
01-085-1327;
00-022-1235
01-077-2064;
01-085-0930
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
00-022-1235
00-004-0587;
00-004-0864
00-022-1235
00-004-0587
00-043-1022
F-341
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 342 of 478
FACILITY N
10.1: 2492-N-SC
10.1.1: Measurement Conditions of 2492-N
Dataset Name
File name
SC,no cover.sd
Sample Identification 2492-N-SC,no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 9/24/2010 6:39:00 PM
2492-N-SC,no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2492-N-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
10.1.2: Main Graphics, Analyze View of 2492-N
F-342
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 343 of 478
V V
2492-N-SC,no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
TTTT-
H
|
50 60 70 80
Position [°2Theta] (Copper (Cu))
Sodium Chloride 16.8 %
Aluminum Oxide Nitride 12.9 %
Aluminum Oxide 11.9 %
Aluminum Oxide Nitride 8.9 %
Aluminum Oxide 22.8 %
Aluminum 1
Quartz 1 % |,|uminum Oxide 2 % |
Aluminum Nitride 3 %
Aluminum Oxide Nitride 6.9 %
10.1.3: Pattern List of 2492-N
F-343
-------
Ref. Code
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 344 of 478
Score Compound Chemical SemiQuant Matched Strong
Name Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
62
47
59
30
27
16
18
18
49
25
23
21
19
20
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
23
4
17
2
3
13
9
7
1
2
1
6
12
1
24
10
9
13
9
9
9
9
5
6
13
34
9
18
0
0
0
0
0
0
0
0
0
0
0
0
0
0
10.1.4: Peak List of 2492-N
F-344
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 345 of 478
Pos. [°2Th.]
16.3163
18.3861
18.9152
19.9003
20.4906
21.6006
23.0249
24.4109
25.4742
26.5467
27.2471
28.2539
29.5366
30.5451
31.5897
33.1383
35.0213
35.9626
36.8134
37.6590
38.3883
40.4014
41.5952
43.2197
43.3362
44.5837
45.3159
45.4338
46.1020
46.8599
Height [cts]
81.99
248.06
388.61
179.85
103.86
117.08
155.17
275.06
16493.36
718.20
6516.87
14624.11
441.35
790.50
68156.91
1671.56
25634.49
1130.97
1739.19
12190.62
3479.72
7320.23
514.61
27070.55
20988.35
2982.66
35338.67
23127.41
745.47
884.29
FWHM
[°2Th.]
0.1574
0.3149
0.1181
0.1574
0.6298
0.2362
0.1968
0.1574
0.1673
0.1378
0.1476
0.1673
0.1181
0.1181
0.1771
0.1771
0.2066
0.1968
0.1968
0.1378
0.1378
0.1771
0.1968
0.1800
0.0960
0.1200
0.1920
0.0840
0.1920
0.2400
d-spacing [A]
5.43274
4.82555
4.69174
4.46166
4.33444
4.11416
3.86277
3.64651
3.49667
3.35778
3.27304
3.15866
3.02434
2.92675
2.83231
2.70341
2.56225
2.49731
2.44153
2.38863
2.34491
2.23259
2.17124
2.09159
2.09142
2.03071
1.99959
1.99963
1.96731
1.93724
Rel. Int. [%]
0.12
0.36
0.57
0.26
0.15
0.17
0.23
0.40
24.20
1.05
9.56
21.46
0.65
1.16
100.00
2.45
37.61
1.66
2.55
17.89
5.11
10.74
0.76
39.72
30.79
4.38
51.85
33.93
1.09
1.30
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064
01-075-1620
01-075-1862
01-075-1620
01-074-1132
01-075-1862;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0930
01-075-1862
01-075-1862;
01-086-2270
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
01-075-1862
00-004-0864;
01-086-2270
F-345
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 346 of 478
Pos. [°2Th.]
50.0799
52.4276
52.5641
53.7391
56.3210
56.4710
57.3781
57.5496
58.5210
59.2229
59.6122
61.1847
62.4511
64.9599
66.0894
66.3728
66.5734
68.0659
Height [cts]
2072.29
11582.11
7777.18
1194.56
9184.80
5946.84
22783.80
12745.58
976.79
926.00
997.05
2108.09
148.77
1112.49
5050.93
10389.96
5883.09
13139.20
FWHM
[°2Th.]
0.1440
0.1920
0.0840
0.1320
0.1800
0.0960
0.1680
0.1320
0.0960
0.1680
0.1440
0.1200
0.6720
0.1200
0.1440
0.1440
0.0840
0.1560
d-spacing [A]
1.81996
1.74385
1.74397
1.70435
1.63219
1.63225
1.60460
1.60420
1.57596
1.55894
1.54969
1.51358
1.48589
1.43444
1.41263
1.40729
1.40702
1.37635
Rel. Int. [%]
3.04
16.99
11.41
1.75
13.48
8.73
33.43
18.70
1.43
1.36
1.46
3.09
0.22
1.63
7.41
15.24
8.63
19.28
Matched by
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-077-2064
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620;
00-022-1235;
01-086-2270
01-075-1862
01-075-1862;
01-086-2270
01-086-2270
01-085-1327;
00-022-1235
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
68.3043
6236.42
0.1320
1.37553
9.15
F-346
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 347 of 478
Pos. [°2Th.]
70.2688
71.2872
72.8888
73.5681
75.1355
75.3286
76.7179
77.0987
77.3242
78.1111
80.5340
80.7984
82.2755
83.8006
84.0345
86.1757
86.4035
87.5444
88.8084
89.1034
90.2136
90.5727
91.0402
91.3190
Height [cts]
305.60
230.42
490.09
1073.82
7595.16
4607.32
3559.52
2472.49
1206.61
733.52
1310.14
757.89
267.76
4662.35
3039.65
858.33
877.29
263.30
1303.32
837.97
405.03
598.91
1756.22
934.55
FWHM
[°2Th.]
0.1920
0.3840
0.1440
0.1440
0.1680
0.0960
0.1440
0.2400
0.1200
0.1440
0.1920
0.1200
0.1920
0.1440
0.1320
0.1680
0.1920
0.1920
0.0960
0.1680
0.1920
0.2160
0.1200
0.1680
d-spacing [A]
1.33849
1.32185
1.29671
1.28640
1.26341
1.26378
1.24124
1.23606
1.23608
1.22255
1.19177
1.19149
1.17090
1.15342
1.15367
1.12762
1.12523
1.11348
1.10087
1.09799
1.08734
1.08396
1.07961
1.07972
Rel. Int. [%]
0.45
0.34
0.72
1.58
11.14
6.76
5.22
3.63
1.77
1.08
1.92
1.11
0.39
6.84
4.46
1.26
1.29
0.39
1.91
1.23
0.59
0.88
2.58
1.37
Matched by
01-075-1862;
01-080-2173;
01-086-2270
01-075-1620;
01-080-2171;
01-080-2172;
01-080-2173;
01-086-2270;
01-080-1385
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235;
01-085-0930
01-077-2064
01-075-1862
01-075-1862;
01-086-2270
01-085-1327;
00-022-1235
01-075-1862
01-085-1327;
00-022-1235
01-077-2064;
01-085-0930
01-075-1862
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
01-075-1862
00-022-1235
00-022-1235
F-347
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 348 of 478
Pos. [°2Th.]
94.3868
95.0852
95.4021
98.1606
100.9480
101.2998
103.1709
103.4990
107.6014
107.9613
108.4580
109.9257
Height [cts]
671.47
3333.32
1880.05
359.21
3419.73
2067.28
417.80
218.51
291.14
108.47
95.63
701.65
FWHM
[°2Th.]
0.1440
0.1680
0.1440
0.2160
0.0960
0.1320
0.1920
0.1440
0.2640
0.1920
0.1920
0.1080
d-spacing [A]
1.04995
1.04408
1.04403
1.01942
0.99866
0.99861
0.98311
0.98332
0.95456
0.95474
0.94939
0.94079
Rel. Int. [%]
0.99
4.89
2.76
0.53
5.02
3.03
0.61
0.32
0.43
0.16
0.14
1.03
Matched by
00-004-0587;
00-004-0864
00-022-1235
00-004-0587
F-348
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 349 of 478
10.2: 2494-N-SC
10.2.1: Measurement Conditions of 2494-N
Dataset Name
File name
SC_002.sd
Sample Identification 2494-N-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Measurement Date / Time 8/2/2010 11:34:00 AM
2494-N-SC_002
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\9-24-10\2494-N-
Raw Data Origin
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
PHILIPS-binary (scan) (.SD)
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
10.00
10.00
2.0000
0.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPert MPD
1
200.00
91.00
No
Yes
10.2.2:Main Graphics, Analyze View of 2494-N
F-349
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 3 50 of 478
' W V V V V V V
2494-N-SC_002
• Aluminum Oxide (01-075-1865;
• Potassium Chloride (01-075-0;
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
Aluminum (01-085-1327)
• Aluminum Nitride (01-076-056!
TTTT1
50 60 70
Position [°2Theta] (Copper (Cu))
Aluminum Oxide Nitride 8.9 %
A ummum Oxide Nitride 6.9 %
Aluminum Qxide 32.7 %]
Aluminum 1 % |
! Aluminum Nrtrirte
ElpasQlite, svn 1 %
. ,
.pxide 3 %
Fluorite, syn 3 %
Aluminum Oxide Nitride 5.9 %
10.2.3: Pattern List of 2494-N
F-350
-------
Ref. Code
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 351 of 478
Score Compound Chemical SemiQuant Matched Strong
Name Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
67
54
53
15
32
14
14
14
45
25
22
24
15
5
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
33
5
12
3
3
9
7
6
1
3
1
8
9
1
24
10
9
11
9
10
10
10
5
6
14
34
10
15
0
0
0
1
0
0
0
0
0
0
0
0
0
0
10.2.4: Peak List of 2494-N
F-351
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 3 52 of 478
Pos. [°2Th.]
18.9723
23.1407
24.5492
25.5838
26.6718
27.3708
28.3735
31.6969
31.7861
33.2816
35.1617
36.0583
37.7833
38.4854
38.8903
40.5618
41.7195
43.3512
43.4833
44.7659
45.4443
45.6012
46.2207
46.9765
Height [cts]
25.88
44.03
92.12
8748.90
113.39
2425.94
9778.12
26401.62
20534.50
1128.99
16163.75
626.85
7106.66
1505.70
264.50
6132.01
244.78
17981.77
13238.04
2216.87
17004.93
9261.42
551.71
485.81
FWHM
[°2Th.]
0.6298
0.3149
0.1378
0.1574
0.1181
0.0886
0.1279
0.1440
0.0480
0.0960
0.1800
0.1200
0.1440
0.2160
0.2400
0.1320
0.1920
0.1680
0.0600
0.1680
0.1680
0.0960
0.1920
0.2400
d-spacing [A]
4.67774
3.84371
3.62629
3.48194
3.34231
3.25852
3.14562
2.82064
2.81991
2.68986
2.55023
2.48884
2.37909
2.33728
2.31388
2.22230
2.16327
2.08555
2.08468
2.02287
1.99424
1.99268
1.96253
1.93270
Rel. Int. [%]
0.10
0.17
0.35
33.14
0.43
9.19
37.04
100.00
77.78
4.28
61.22
2.37
26.92
5.70
1.00
23.23
0.93
68.11
50.14
8.40
64.41
35.08
2.09
1.84
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1620
01-075-1862
01-075-1620
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235;
01-086-2270
00-004-0587
01-075-1862
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-080-2171;
01-086-2270;
01-080-1385
01-075-1862
00-004-0864;
01-086-2270
F-352
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 353 of 478
Pos. [°2Th.]
473755
=_
52.5438
52.7167
53.8731
56.4827
56.6369
57.5038
57.6727
58.6679
59.3732
59.7429
61.3327
65.1340
66.2228
66.5075
66.7162
68.2126
68.4058
70.4454
71.4996
73.0558
73.7507
Height [cts]
40428
_=_=_
8418.80
5729.39
631.84
5279.75
3194.93
18670.98
12290.50
888.05
740.18
709.07
1883.23
687.92
3622.68
9731.17
5968.09
11705.47
7403.69
338.50
432.59
403.59
1319.28
FWHM
[°2Th.]
01920
==noi8F=
0.1560
0.0720
0.1440
0.0840
0.1200
0.1320
0.0600
0.2160
0.1920
0.1440
0.1320
0.1680
0.1200
0.1680
0.0720
0.1440
0.1200
0.1920
0.2160
0.1440
0.1920
d-spacing [A]
L91735
=^^
1.74027
1.73928
1.70043
1.62790
1.62383
1.60139
1.60107
1.57236
1.55536
1.54661
1.51028
1.43102
1.41011
1.40476
1.40436
1.37374
1.37374
1.33557
1.31845
1.29415
1.28367
Rel. Int. [%]
L53
=^^
31.89
21.70
2.39
20.00
12.10
70.72
46.55
3.36
2.80
2.69
7.13
2.61
13.72
36.86
22.61
44.34
28.04
1.28
1.64
1.53
5.00
Matched by
01-086^70
n^O04-0587T
01-080-2172;
01-080-2173;
00-022-1235;
01-085-0930
01-075-1862
01-077-2064
01-077-2064;
01-080-2171
01-077-2064;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862
00-004-0587
01-074-1132;
01-075-1620
01-075-1862
01-075-1862
01-074-1132;
01-085-1327
00-004-0587;
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
01-075-1862
01-075-1620;
01-086-2270
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
F-353
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 3 54 of 478
Pos. [°2Th.]
75.2366
75.2926
75.5121
76.8400
77.1324
77.2465
77.5034
78.2420
80.7027
80.9567
82.4669
83.9432
84.2266
86.3274
86.5787
87.6659
89.0015
89.3042
90.3913
90.7064
91.1941
91.5051
94.5773
95.2765
95.5712
98.3968
101.0981
101.4594
103.3218
103.6939
Height [cts]
4682.80
5116.57
2969.84
3261.92
2953.03
2683.80
1179.51
496.48
1413.24
840.02
275.58
3156.34
2243.89
837.93
861.88
316.48
1438.41
813.15
294.43
563.12
1750.05
910.28
703.63
3422.06
1949.04
461.87
3297.08
2079.88
463.80
197.67
FWHM
[°2Th.]
0.0600
0.0720
0.1200
0.1440
0.0960
0.1440
0.1200
0.1680
0.0840
0.1200
0.3840
0.1200
0.1680
0.1680
0.1440
0.1680
0.0840
0.1440
0.1440
0.1200
0.1680
0.1680
0.1680
0.1680
0.1440
0.1920
0.0720
0.1680
0.1680
0.1440
d-spacing [A]
1.26196
1.26116
1.26117
1.23958
1.23867
1.23407
1.23367
1.22084
1.18970
1.18661
1.16866
1.15183
1.14867
1.12603
1.12340
1.11225
1.09899
1.09604
1.08567
1.08271
1.07819
1.07801
1.04834
1.04249
1.04264
1.01760
0.99758
0.99747
0.98208
0.98201
Rel. Int. [%]
17.74
19.38
11.25
12.36
11.19
10.17
4.47
1.88
5.35
3.18
1.04
11.96
8.50
3.17
3.26
1.20
5.45
3.08
1.12
2.13
6.63
3.45
2.67
12.96
7.38
1.75
12.49
7.88
1.76
0.75
Matched by
01-077-2064
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-074-1132;
01-085-1327
01-075-1862
01-075-1620;
01-085-0930
01-074-1132;
01-085-1327
01-077-2064;
01-085-0930
01-075-1862;
01-080-2171;
01-080-2172;
01-086-2270;
01-080-1385
01-075-1862
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385;
01-085-0930
01-075-1862
00-022-1235
00-004-0587
F-354
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 355 of 478
Pos. [°2Th.] Height [cts] FWHM d-spacing [A] Rel. Int. [%] Matched by
107.7621
108.6384
109.8280
296.26
373.90
1241.94
0.1920
0.2400
0.0480
0.95358
0.94832
0.94135
1.12
1.42
4.70
00-004-0587
F-355
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 3 56 of 478
10.3: 2496-N-SC
10.3.1: Measurement Conditions of 2496-N
Dataset Name
File name
N-SC.udf
Sample Identification 2496-N-SC
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 110.0000
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Divergence Slit Type Automatic
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 2.0000
Measurement Temperature [°C] 25.00
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPERT
Diffractometer Number 1
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning No
10.3.2: Main Graphics, Analyze View OF 2496-N
2496-N-SC
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2496-
F-356
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 3 57 of 478
V V V V V
2496-N-SC
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
• Quartz, syn (01-083-2467)
50 60 70
Position [°2Theta] (Copper (Cu))
Sodium Chloride 13.9 %
Aluminum Oxide Nitride 12.9 %
Aluminum Oxide 11.9 %
Aluminum Oxide Nitride 15.8 %
Aluminum Oxide 16.8 %
i) Elpasolite, syn 1 %~|"|
Aluminum 1 %
Sylvite, syn 3 %
irrnJxide 3 %
Aluminum Oxide Nitride 9.9 % |
10.3.3: Pattern List OF 2496-N
F-357
-------
Ref. Code
Score Compound
Name
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 358 of 478
Chemical SemiQuant Matched Strong
Formula [%] Lines Unmatched
Lines
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
01-085-
0930
43
43
55
35
20
12
15
15
35
8
21
17
17
15
11
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Quartz
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
Si O2
12
3
14
3
3
16
13
10
1
1
1
1
5
17
1
21
10
9
13
7
10
11
11
5
6
6
13
35
10
18
0
0
0
0
0
0
0
0
0
1
0
0
0
0
0
F-358
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 359 of 478
10.3.4: Peak List of 2496-N
Pos. [°2Th.]
18.9545
20.7728
23.0584
24.4553
25.4777
26.5677
27.2798
28.2751
31.6065
33.1971
35.0561
35.9535
36.8105
37.6800
38.4279
40.4386
41.6561
43.2661
43.3594
44.7001
45.3495
45.4594
46.9340
50.1338
52.4748
Height [cts]
377.81
84.99
28.40
144.65
5649.54
443.78
3153.87
7611.40
33298.05
522.15
10459.47
492.08
1794.80
4649.32
1910.33
4599.88
227.47
12638.05
10675.91
2595.87
21846.23
17034.76
406.30
1588.05
6229.23
FWHM
[°2Th.]
0.1968
0.1574
0.2362
0.1378
0.1476
0.1378
0.0886
0.1673
0.1771
0.0984
0.1574
0.1574
0.0886
0.1378
0.1673
0.1574
0.1378
0.1440
0.0600
0.1920
0.1560
0.0960
0.2400
0.1920
0.1320
d-spacing [A]
4.68211
4.27619
3.85724
3.64000
3.49620
3.35517
3.26919
3.15633
2.83085
2.69876
2.55978
2.49793
2.44171
2.38735
2.34259
2.23063
2.16821
2.08945
2.09035
2.02569
1.99818
1.99856
1.93435
1.81813
1.74240
ReLIntM
1.13
0.26
0.09
0.43
16.97
1.33
9.47
22.86
100.00
1.57
31.41
1.48
5.39
13.96
5.74
13.81
0.68
37.95
32.06
7.80
65.61
51.16
1.22
4.77
18.71
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-085-0930
01-086-2270
01-075-1862;
01-086-2270
01-085-0930
01-077-2064
00-004-0587;
00-004-0864
01-077-2064
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-075-1862;
01-080-2172;
01-080-2173
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587;
01-085-0930
01-075-1862
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
00-004-0864;
01-086-2270
00-004-0587;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385;
01-085-0930
01-075-1862
F-359
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 360 of 478
Pos. [°2Th.]
52.6312
53.7861
56.3718
56.5450
57.4075
57.5935
58.5949
59.3301
59.6724
61.2506
62.4304
65.2055
66.1491
66.4597
66.6416
68.1371
68.3405
70.3216
71.4325
72.9792
73.6705
75.2164
75.4566
76.8311
77.1798
77.3990
78.1740
Height [cts]
3712.31
813.58
6858.29
4314.63
12885.75
8233.12
894.19
1138.95
890.63
1453.20
42.14
1994.67
4283.99
7591.04
4000.28
8155.08
4741.32
220.17
236.99
493.47
1173.76
7216.69
3822.54
2989.00
1997.73
1139.55
736.44
FWHM
[°2Th.]
0.1200
0.1680
0.1440
0.0960
0.1440
0.1320
0.1680
0.1680
0.1440
0.1440
0.5760
0.1440
0.1200
0.1200
0.1200
0.1560
0.0960
0.2880
0.3360
0.1440
0.1680
0.1320
0.1200
0.0840
0.1440
0.1200
0.2400
d-spacing [A]
1.74191
1.70297
1.63084
1.63029
1.60385
1.60309
1.57415
1.55638
1.54827
1.51211
1.48634
1.42963
1.41150
1.40566
1.40575
1.37508
1.37489
1.33762
1.31952
1.29532
1.28487
1.26225
1.26196
1.23970
1.23496
1.23507
1.22173
Rel. Int. [%]
11.15
2.44
20.60
12.96
38.70
24.73
2.69
3.42
2.67
4.36
0.13
5.99
12.87
22.80
12.01
24.49
14.24
0.66
0.71
1.48
3.53
21.67
11.48
8.98
6.00
3.42
2.21
Matched by
01-077-2064
01-077-2064
01-075-1862;
01-085-0930
00-004-0587
01-074-1132;
01-075-1620
01-075-1862
01-075-1862;
01-086-2270
00-043-1022
01-074-1132;
01-085-1327
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
01-080-1385
01-075-1862;
00-022-1235;
01-085-0930
01-075-1862;
01-086-2270
01-075-1620;
01-086-2270
01-077-2064;
01-086-2270
00-004-0587;
00-022-1235
01-077-2064
01-075-1862
01-075-1862;
01-074-1132;
01-086-2270
01-085-1327;
00-022-1235
F-360
-------
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 361 of 478
Pos. [°2Th.]
80.6277
80.8620
82.3565
83.9281
84.1731
86.2669
86.5019
87.5945
88.9248
89.2208
90.3401
90.6808
91.1224
91.4012
94.4753
95.1693
95.5075
98.3281
101.0591
101.4194
103.2657
107.6696
108.5997
109.7364
Height [cts]
956.38
623.40
301.14
4680.93
2936.27
638.85
638.17
231.62
1083.03
606.42
431.48
511.42
1352.95
748.18
745.70
2464.44
1424.04
329.45
2977.73
1883.12
334.81
619.00
699.60
1408.40
FWHM
[°2Th.]
0.1440
0.0960
0.2880
0.1560
0.1200
0.1440
0.1920
0.2400
0.1200
0.1440
0.0960
0.1680
0.0960
0.1440
0.1920
0.0960
0.0960
0.1680
0.0960
0.2160
0.1680
0.2160
0.2400
0.0480
d-spacing [A]
1.19062
1.19071
1.16995
1.15200
1.15212
1.12666
1.12420
1.11297
1.09973
1.09958
1.08615
1.08295
1.07885
1.07629
1.04920
1.04338
1.04316
1.01813
0.99786
0.99529
0.98246
0.95414
0.94855
0.94188
Rel. Int. [%]
2.87
1.87
0.90
14.06
8.82
1.92
1.92
0.70
3.25
1.82
1.30
1.54
4.06
2.25
2.24
7.40
4.28
0.99
8.94
5.66
1.01
1.86
2.10
4.23
Matched by
01-075-1862
01-085-1327;
00-022-1235
01-077-2064;
01-085-0930
01-075-1862
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385;
01-085-0930
01-075-1862;
01-086-2270
00-022-1235
00-004-0587;
00-004-0864
00-004-0587
00-004-0587
00-043-1022
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Date: June 6 2013
Revision No.: 1
Page 362 of 478
10.4: 2498-N-SC
10.4.1: Measurement Conditions of 2498-N
Dataset Name
File name
N-SC,no cover.udf
Sample Identification 2498-N-SC,no cover
Comment Exported by X'Pert SW
Generated by Ford in project SAP.
Raw Data Origin PHILIPS-ASCII (.UDF)
Scan Axis
Start Position [°2Th.]
End Position [°2Th.]
Step Size [°2Th.]
Scan Step Time [s]
Scan Type
Offset [°2Th.]
Divergence Slit Type
Irradiated Length [mm]
Specimen Length [mm]
Receiving Slit Size [mm]
Measurement Temperature [°C]
Anode Material
K-Alphal [A]
K-Alpha2 [A]
K-Beta [A]
K-A2/K-A1 Ratio
Generator Settings
Diffractometer Type
2498-N-SC,no cover
C:\Documents and Settings\xhuang\Desktop\SAP-xrd\SC-no cover\2498-
Diffractometer Number
Goniometer Radius [mm]
Dist. Focus-Diverg. Slit [mm]
Incident Beam Monochromator
Spinning
Gonio
10.0000
110.0000
0.0100
5.0000
Pre-set time
0.0000
Automatic
20.00
10.00
2.0000
25.00
Cu
1.54060
1.54443
1.39225
0.50000
40 mA, 45 kV
XPERT
1
240.00
91.00
No
No
10.4.2: Main Graphics, Analyze View of 2498-N
F-362
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 363 of 478
2498-N-SC,no cover
• Aluminum Oxide (01-075-1865
• Potassium Chloride (01-075-0:
Sodium Chloride (01-072-1668
• Spinel (01-086-2258)
• Aluminum Nitride (01-076-056:
Aluminum (01-085-1327)
I? ',
50 60 70
Position [°2Theta] (Copper (Cu))
Aluminum Oxide 12.1 %
Magnesium Aluminum Oxide 12.1 %
Aluminum Oxide Nitride 9.1 %
Aluminum Oxide 8.1 %|
["Anhydrite 7.1 %
Aluminum Oxide Nitride 6.1 %
.j. .7^.7.'!,:^:, ,;:.jie4%
Fluorite, syn 4 % \\
F-363
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 364 of 478
10.4.3: Pattern List of 2498-N
Ref. Code
01-075-
1862
00-004-
0587
01-077-
2064
01-074-
1132
01-075-
1620
01-080-
2171
01-080-
2172
01-080-
2173
01-085-
1327
00-043-
1022
00-004-
0864
00-022-
1235
01-086-
2270
01-080-
1385
Score
59
41
48
53
49
17
18
19
29
10
20
29
22
18
Compound
Name
Aluminum
Oxide
Sylvite, syn
Sodium
Chloride
Magnesium
Aluminum
Oxide
Aluminum
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Oxide
Nitride
Aluminum
Periclase,
syn
Fluorite, syn
Elpasolite,
syn
Anhydrite
Aluminum
Oxide
Chemical SemiQuant
Formula [%]
A12O3
KC1
NaCl
Mg A12 O4
A1N
A12.85
O3.45
N0.55
A12.81
O3.56
N0.44
A12.78
O3.65
N0.35
Al
MgO
CaF2
K2 Na Al
F6
Ca ( S O4 )
A12.667 O4
12
5
20
12
6
9
6
4
2
1
4
3
7
8
Matched
Lines
22
10
9
15
11
12
12
12
5
7
5
17
38
12
Strong
Unmatched
Lines
0
0
0
0
0
0
0
0
0
0
0
0
0
0
F-364
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 365 of 478
10.4.4: Peak List of 2498-N
Pos. [°2Th.]
18.9736
23.0855
24.4619
25.5046
25.5568
26.5823
27.3156
28.3223
30.5653
31.1937
31.6288
33.1889
35.1095
35.9841
36.7778
36.8301
37.7110
37.8823
38.4273
40.4129
40.4627
41.6043
43.2605
43.8080
44.7313
45.3572
Height [cts]
3575.44
186.52
265.83
5490.32
5031.29
595.19
7241.97
15843.06
1827.60
7266.05
74958.65
5973.09
10026.84
3708.59
14048.43
14967.21
6025.68
5432.35
3022.09
6828.79
8341.99
506.07
9465.14
1265.80
10465.37
39866.75
FWHM
[°2Th.]
0.0492
0.1574
0.1574
0.1080
0.0360
0.1200
0.1440
0.1800
0.1680
0.1440
0.2280
0.1440
0.1440
0.0960
0.1200
0.1080
0.0720
0.1920
0.2640
0.0480
0.0480
0.2880
0.1440
0.0720
0.1440
0.2160
d-spacing [A]
4.67744
3.85278
3.63903
3.48968
3.49132
3.35059
3.26228
3.14857
2.92244
2.86498
2.82656
2.69717
2.55390
2.49380
2.44178
2.43844
2.38348
2.37309
2.34068
2.23014
2.23304
2.16899
2.08971
2.06486
2.02435
1.99786
Rel. Int. [%]
4.77
0.25
0.35
7.32
6.71
0.79
9.66
21.14
2.44
9.69
100.00
7.97
13.38
4.95
18.74
19.97
8.04
7.25
4.03
9.11
11.13
0.68
12.63
1.69
13.96
53.18
Matched by
01-074-1132;
00-022-1235;
01-086-2270
01-075-1862;
01-086-2270
01-077-2064
00-004-0587;
00-004-0864
01-074-1132;
00-022-1235;
01-086-2270
01-077-2064
01-075-1620
01-075-1862
01-075-1620
01-074-1132;
00-043-1022
01-074-1132;
00-043-1022
01-075-1862;
01-080-2173
01-075-1862;
01-075-1620
01-074-1132;
01-085-1327;
00-022-1235
00-004-0587
01-075-1862
01-075-1862;
01-086-2270
01-074-1132;
01-085-1327;
00-022-1235
01-077-2064;
01-086-2270
F-365
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 366 of 478
Pos. [°2Th.]
45.4902
46.9545
47.3219
49.7617
50.1119
52.4982
52.6032
53.7729
55.6125
56.3407
56.5512
57.4141
57.5813
58.5765
59.2816
59.4395
61.2350
62.4293
65.1702
65.3505
66.1013
66.3551
68.1006
68.2971
69.6617
Height [cts]
23286.25
1347.14
1055.61
1639.23
2379.38
3881.65
2469.82
1412.15
1629.71
9749.35
5435.00
8478.55
4667.90
1513.53
6816.08
5811.97
1009.99
475.51
8801.68
7846.01
6379.70
6126.87
4506.46
2673.63
436.17
FWHM
[°2Th.]
0.0720
0.1680
0.1680
0.1440
0.0960
0.1440
0.0960
0.0840
0.2880
0.1680
0.1080
0.1440
0.0960
0.2400
0.2160
0.1200
0.1080
0.1920
0.1200
0.1440
0.0960
0.2400
0.1320
0.0960
0.1920
d-spacing [A]
1.99728
1.93355
1.91940
1.83085
1.81888
1.74168
1.74277
1.70336
1.65129
1.63166
1.63013
1.60368
1.60340
1.57460
1.55754
1.55764
1.51245
1.48636
1.43032
1.42681
1.41241
1.40762
1.37573
1.37566
1.34867
Rel. Int. [%]
31.07
1.80
1.41
2.19
3.17
5.18
3.29
1.88
2.17
13.01
7.25
11.31
6.23
2.02
9.09
7.75
1.35
0.63
11.74
10.47
8.51
8.17
6.01
3.57
0.58
Matched by
00-004-0864;
01-086-2270
01-086-2270
01-075-1620
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-022-1235;
01-080-1385
01-075-1862
01-077-2064
01-074-1132;
00-004-0864;
01-086-2270
01-077-2064
01-075-1862
00-004-0587
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862;
01-086-2270
00-043-1022
01-074-1132;
01-085-1327
01-074-1132;
01-086-2270
01-077-2064;
01-075-1620
01-075-1862;
00-004-0587;
01-077-2064;
01-080-2171;
01-080-1385
01-075-1862;
00-022-1235
01-074-1132;
01-075-1620
F-366
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 367 of 478
Pos. [°2Th.]
71.3553
72.5221
72.9320
73.5834
75.1491
75.3704
76.7562
77.3306
78.1541
79.3808
80.6048
82.5277
83.8185
83.8737
84.0965
85.6995
86.2182
87.5487
88.8778
89.1654
90.2458
90.5426
91.0857
91.3368
93.9720
94.4249
95.1199
95.4011
99.2707
Height [cts]
1297.00
633.96
804.88
1150.84
8364.28
4975.27
1575.11
1407.18
678.24
198.86
464.76
764.95
5053.95
5009.65
3013.24
208.78
349.59
233.78
467.97
245.83
427.21
412.61
830.01
470.28
1143.02
1288.91
1461.80
810.94
620.05
FWHM
[°2Th.]
0.1920
0.1920
0.0960
0.1440
0.1560
0.0840
0.0960
0.1680
0.1920
0.1440
0.1920
0.1440
0.0840
0.0720
0.1440
0.3840
0.1920
0.2400
0.1680
0.1440
0.1200
0.1440
0.1200
0.1440
0.2400
0.1920
0.1920
0.1440
0.3360
d-spacing [A]
1.32076
1.30236
1.29927
1.28617
1.26321
1.26318
1.24072
1.23293
1.22199
1.20616
1.19090
1.16796
1.15322
1.15261
1.15012
1.13266
1.12717
1.11344
1.10019
1.10012
1.08704
1.08425
1.07919
1.07955
1.05349
1.04963
1.04379
1.04404
1.01097
Rel. Int. [%]
1.73
0.85
1.07
1.54
11.16
6.64
2.10
1.88
0.90
0.27
0.62
1.02
6.74
6.68
4.02
0.28
0.47
0.31
0.62
0.33
0.57
0.55
1.11
0.63
1.52
1.72
1.95
1.08
0.83
Matched by
01-075-1620;
01-080-2173;
01-086-2270
01-075-1620
00-004-0587;
00-022-1235
01-077-2064
01-075-1862
01-074-1132
01-085-1327;
00-022-1235
01-075-1862
01-074-1132;
01-085-1327;
01-086-2270
01-077-2064
01-077-2064
01-075-1862;
01-077-2064;
01-086-2270
01-074-1132;
01-075-1620;
01-086-2270
01-075-1862
00-004-0587;
01-080-2171;
01-080-2172;
01-080-2173;
00-004-0864;
01-080-1385
01-075-1862;
01-086-2270
00-022-1235
00-022-1235
00-043-1022
00-004-0587;
00-004-0864
F-367
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 368 of 478
Pos. [°2Th.]
100.9469
103.1483
104.6818
107.6057
109.8479
109.9444
Height [cts]
2304.68
191.31
98.64
593.61
2774.35
2114.96
FWHM
[°2Th.]
0.2160
0.1920
0.4800
0.2160
0.0840
0.0720
d-spacing [A]
0.99866
0.98326
0.97302
0.95453
0.94124
0.94068
Rel. Int. [%]
3.07
0.26
0.13
0.79
3.70
2.82
Matched by
00-043-1022
00-043-1022
Secondary Aluminum Processing Waste: Salt Cake Characterization and Reactivity
10. APPENDIX D: Temperature Profiles of Salt Cake
Table of Contents
1 Facility B
2 Facility C
3 Facility D
4 Facility E
5. Facility F
6. Facility H
7. Facility!
8. Facility L
9. Facility M
lO.FacilityN
369
371
372
373
375
378
382
385
388
392
List of Appendix D Tables
Table 1-1: The Temperature Pattern of Facility B 369
Table 2-1: The Temperature Pattern of Facility C 371
Table 3 -1: The Temperature Pattern of Facility D 372
Table 4-1: The Temperature Pattern of Facility E 374
Table 5-1: The Temperature Pattern of Facility F 375
Table 6-1: The Temperature Pattern of Facility H 378
Table 6-2: Effect of Particle Size on the Temperature Change of Salt Cake at 37 °C 379
Table 6-3: Effect of Chemical Composition of liquids on the Temperature Change of Salt Cake at 37 °C 379
Table 7-1: The Temperature Pattern of Facility J 383
Table 8-1: The Temperature Pattern of Facility L 386
Table 9-1: The Temperature Pattern of Facility M 388
Table 10-1: The temperature pattern of Facility N 392
List of Appendix D Figures
Figure 1-1: Temperature profile of four salt cakes fromFacility B at 37 °C.
Figure 1-2: Temperature profile of four salt cakes from Facility B at 50 °C.
Figure 2-1: Temperature profile of two salt cakes fromFacility C at 37 °C.
Figure 2-2: Temperature profile of two salt cakes from Facility C at 50 °C.
370
370
371
372
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 369 of 478
Figure 3-1: Temperature profile of four salt cakes fromFacility D at 37 °C. 373
Figure 3-2: Temperature profile of four salt cakes from Facility D at 50 °C. 373
Figure 4-1: Temperature profile of two salt cakes fromFacility E at 37 °C. 374
Figure 4-2: Temperature profile of two salt cakes from Facility E at 50 °C. 375
Figure 5-1: Temperature profile of five salt cakes fromFacility F at 37 °C. 376
Figure 5-2: Temperature profile of five salt cakes from Facility F at 50 °C. 376
Figure 5-3: Effect of particle size of salt cake 2502-F on the temperature profile at 37 °C. 377
Figure 5-4: Effect of particle size of salt cake 2502-F on the temperature profile at 50 °C. 377
Figure 5-5: Effect of chemical composition of liquids on the temperature profile of salt cake
2502-F at 37 °C. 378
Figure 6-1: Temperature profile of five salt cakes fromFacility H at 37 °C. 380
Figure 6-2: Temperature profile of five salt cakes from Facility H at 50 °C. 380
Figure 6-3: Effect of particle size of salt cake 2046-H on the temperature profile at 37 °C. 381
Figure 6-4: Effect of chemical composition of liquids on the temperature profile of salt cake
2555-H at 37 °C. 381
Figure 6-5: Effect of phosphorus species in liquids on the temperature profile of salt cake
2046-H at 37 °C. 382
Figure 6-6: Effect of mix solid phosphorus compounds on the salt cake 2046-H temperature
profile at 50 °C. 382
Figure 7-1: Temperature profile of four salt cakes fromFacility J at 37 °C. 383
Figure 7-2: Temperature profile of four salt cakes from Facility J at 50 °C. 384
Figure 7-3: Effect of particle size of salt cake sample 2512-J on the temperature profile at 37 °C. 384
Figure 7-4: Effect of particle size of salt cake 2512-J on the temperature profile at 50 °C. 385
Figure 7-5: Effect of phosphate solution on the temperature profile of salt cake 2512-J. 385
Figure 8-1: Temperature profile of five salt cakes fromFacility L at 37 °C. 386
Figure 8-2: Temperature profile of five salt cakes from Facility L at 50 °C. 387
Figure 8-3: Effect of phosphate solution on the temperature profile of salt cake 2490-L at 37 °C. 387
Figure 9-1: Temperature profile of four salt cakes fromFacility M at 37 °C. 388
Figure 9-2: Temperature profile of four salt cakes from Facility M at 50 °C. 389
Figure 9-3: Effect of chemical composition of liquids on the temperature profile of salt cake
2613-Mat37°C 389
Figure 9-4: Effect of phosphorus species in liquids on the temperature profile of salt cake 2613 -M. 3 90
Figure 9-5: Effect of 0.2 M Na2HPC>4 on the temperature profiles of the selected high reactivity
salt cake samples. 390
Figure 9-6: Effect of 0.2 M NaH2PO4 on the temperature profiles of the selected high reactivity
salt cake samples. 391
Figure 10-1: Temperature profile of four salt cakes fromFacility N at 37 °C. 392
Figure 10-2: Temperature profile of four salt cakes from Facility N at 50 °C. 393
Facility B
Facility B has four samples, which were collected on Feb 24, 2010 and March 19, 2010, respectively. The highest
temperature increase was Sample 2478-B-SC (27.8 °C @ 50 °C, and 14.9 °C @ 37 °C).
Table 10-1: The Temperature Pattern of Facility B
Sample ID
2452-B-SC
2454-B-SC
37 °C
ATmax
(°C)
10.4
8.5
tmax-T
(h)
2.6
2.3
50 °C
A I. max
(°C)
13.2
13.1
tmax-T
(h)
1.3
1.2
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Date: June 6 2013
Revision No.: 1
Page 370 of 478
2468-B-SC
2478-B-SC
11.2
14.9
1.5
2.2
18.2
27.7
0.8
0.7
Maximum
Minimum
Average
14.9
8.5
11.3
2.6
1.5
2.1
27.7
13.1
18.1
1.3
0.7
1.0
2454-6,3-19-10
2452-6,2-24-10
2468-6,2-24-10
2478-6,2-24-10
80
Figure 10-1: Temperature profile of four salt cakes from Facility B at 37 °C.
2452-SC
2454-SC
2468-SC
2478-SC
80
Figure 10-2: Temperature profile of four salt cakes from Facility B at 50 °C.
F-370
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Date: June 6 2013
Revision No.: 1
Page 371 of 478
Facility C
Facility C has two samples, which were collected on November 25 and December 28, 2009, respectively. The highest
temperature increase was Sample 2435-C-SC (6.9 °C @ 50 °C, and 14.5 °C @ 37 °C).
Table 10-2: The Temperature Pattern of Facility C
Sample ID
2433-C-SC
2535-C-SC
Maximum
Minimum
Average
37 °C
ATmax
(°C)
3.4
10.0
10.0
3.4
6.7
tmax-T
(h)
4.1
0.9
4.1
0.9
2.5
50 °C
ATmax
(°C)
4.4
6.9
6.9
4.4
5.7
tmax-T
(h)
2.0
2.1
2.1
2.0
2.0
2433-C, 11-25-09
2435-C, 12-28-09
80
Figure 10-3: Temperature profile of two salt cakes from Facility C at 37 °C.
F-371
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Facility D
10
o
8 -
6 -
4 -
2 -
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 372 of 478
ATmax = 6.90Q
(@50°C, 10g/10ml)
2433-SC11-25-2009
2435-SC 12-28-2009
20
40 60
Time (h)
80
Figure 10-4: Temperature profile of two salt cakes from Facility C at 50 °C.
Facility D has four samples, which were collected on November 5, 2009, and January 15, February 24, and March 19,
2010, respectively. The highest temperature increase was Sample 2538-D-SC @ 50°C (20.4 °C) and Sample 2536-D-
SC@37°C(14.4°C).
Table 10-3: The Temperature Pattern of Facility D
Sample ID
2532-D-SC
2536-D-SC
2538-D-SC
2540-D-SC
Maximum
Minimum
Average
37 °C
ATmax
(°C)
11.8
14.4
11.8
10.4
14.4
10.4
12.1
tmax-T
(h)
1.4
1.7
0.8
1.7
1.7
0.8
1.4
50 °C
ATmax
(°C)
17.7
17.1
20.4
17.7
20.4
17.1
18.2
tmax-T
(h)
0.5
0.7
0.3
0.6
0.7
0.3
0.5
F-372
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Facility E
WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 373 of 478
16
O
14 -
12 -
10 -
8 -
ATmax=14.5°C
(@37 C, 10g/10ml)
2532-D, 11-5-09
2536-D, 1-15-10
2540-0,3-19-10
2538-0,2-24-10
20
40
Time (h)
60
80
Figure 10-5: Temperature profile of four salt cakes from Facility D at 37 °C
25
20
ATmax = 20.5°C
(@50°C, 10g/10ml)
2532-SC
2536-SC
2538-SC
2540-SC
80
Figure 10-6: Temperature profile of four salt cakes from Facility D at 50 °C.
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Facility E has two samples, which were collected on February 24 and 25, 2010, respectively. Their behaviors were
very similar. The higher temperature increase was Sample 2437-E-SC (23.2 °C @ 50 °C) and Sample 2439-E-SC
(16.1°C@37°C).
Table 10-4: The Temperature Pattern of Facility E
Sample ID
2437-E-SC
2439-E-SC
Maximum
Minimum
Average
37
ATmax
(°C)
16.0
16.1
16.1
16.0
16.1
°C
tmax-T
(h)
1.0
1.2
1.2
1.0
1.1
ATmax
(°C)
23.2
22.6
23.2
22.6
22.9
50 °C
tmax-T
(h)
0.7
0.9
0.9
0.7
0.8
2439-E-SC, 2-24-10
2437-E-SC, 2-25-10
20
40 60
Time (h)
80
Figure 10-7: Temperature profile of two salt cakes from Facility E at 37 °C.
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20
40 60
Time (h)
80
Figure 10-8: Temperature profile of two salt cakes from Facility E at 50 °C.
Facility F
Facility F has five samples, which were collected from November 20, 2009 to April 6, 2010. They were very similar
and the strongest temperature response was sample 2510-F-SC, which had more than 50 °C increase, both under 37 °C
and 50 °C environmental conditions.
Table 10-5: The Temperature Pattern of Facility F
Sample ID
2502-F-SC
2504-F-SC
2506-F-SC
2508-F-SC
2510-F-SC
Maximum
Minimum
Average
37
ATmax
(°C)
50.9
48.0
52.9
39.4
56.1
56.1
39.4
49.5
°C
tmax-T
(h)
1.1
0.9
0.7
1.2
0.8
1.2
0.7
0.9
50 °C
ATmax
(°C)
48.7
44.8
47.4
48.3
52.4
52.4
44.8
48.3
tmax-T
(h)
0.6
0.5
0.4
0.5
0.4
0.6
0.4
0.5
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2504-F, 12-28-09
2502-F, 11-20-09
2506-F, 12-28-09
2508-F, 2-24-10
2510-F, 4-6-10
80
Figure 10-9: Temperature profile of five salt cakes from Facility F at 37 °C.
60 -i
ATmax = 53.20C
50 -I (@50°C,10g/10ml)
2502-SC
2508-SC
2506-SC
2504-SC
2510-SC
20
40 60
Time (h)
80
Figure 10-10: Temperature profile of five salt cakes from Facility F at 50 °C.
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As expected, the particle size significantly influenced the reaction of salt cake with water, both the degree of
temperature increases as well as the intensity of reaction (Table 6-2, Figure 5-3, and Figure 5-4).
Figure 10-11: Effect of particle size of salt cake 2502-F on the temperature
Particle size effect
2502-F @37 °C
60
40
20
ATmax(°C) t_maxT(h)
9mm 19.17 2.33
2mm 50.95 1.07
0.05mm 67.12 0.67
10
20
30
Time (h)
40
50
profile at 37 °C.
Particle size effect
2502-F@50°C
50 •
40 •
30 •
20 •
10 -
0
0.05 mm, ATmax (°C) t-maxT (h)
- 2mm, i, 53.98°C, 0.27 h
• 9mm, 49.16°C, 0.50 h
- a mm, 24.77°C, 1.23h
20
40
60
Time (h)
80
100
60
120
Figure 10-12: Effect of particle size of salt cake 2502-F on the temperature
profile at 50 °C.
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Some trail experiments were conducted to explore the effect of chemical composition of liquids on the temperature
changes, including the pH effect (0.1 M HC1 and 0.1 M H3PO4, acidic condition; 0.1 M NaOH, base condition),
aluminum ligands effect, including phosphate (0.2 M NaH2PO4, and 0.2 M Na2HPC>4), and a leachate from landfill. All
of these primary results indicated that chemical composition of liquids can significantly change the temperature
patterns of salt cake reaction with liquids (Figure 5-5, and Table 6-3).
Facility H
12.42
12.43
49.78
31.94
54.88
Landfill leachate
DIW
0.1MHCI
O.IMNaOH
10
15
20
Time (h)
Figure 10-13: Effect of chemical composition of liquids on the temperature
profile of salt cake 2502-F at 37 °C.
Facility H has five samples, which were collected from November 13, 2009 to March 12, 2010. The strongest
temperature response was Sample 2046-H-SC (23.9 °C @ 37 °C; and 55.8 °C @ 50 °C). We also made four
replications for sample 2046-H at 50 °C environment.
Table 10-6: The Temperature Pattern of Facility H
Sample ID
2046-H-SC
2544-H-SC
2555-H-SC
2559-H-SC
2568-H-SC
Maximum
Minimum
Average
37 °C
ATmax
(°C)
23.9
20.3
16.5
14.3
16.7
23.9
14.3
18.3
tmax-T
(h)
1.7
2.2
2.7
2.7
2.9
2.9
1.7
2.4
50 °C
ATmax
(°C)
55.8
40.0
33.7
37.4
34.8
55.8
33.7
40.3
tmax-T
(h)
0.8
1.2
1.0
1.1
0.9
1.2
0.8
1.0
Similar to the trail experiment on 2502-F, the effect of particle size and chemical composition of liquids to the
temperature for sample 2555-H or 2046-H at 37 °C were also conducted (Table 6-2 and 6-3).
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Table 10-7: Effect of Particle Size on the Temperature Change of Salt Cake at 37 °C
Sample ID
Particle
size
9 mm
2 mm
0.05mm
2502-F
19.2
50.9
67.1
ATmax (°C)
2512-J
4.1
9.2
96.2
2046-H
12.4
23.9
55.6
2502-F
2.33
1.07
0.67
tmax-T (h)
2512-J
1.63
0.81
0.23
2046-H
2.20
1.33
1.56
Table 10-8: Effect of Chemical Composition of liquids on the Temperature Change of Salt Cake at 37 °C
1 1
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O
2555-H, 12-14-09
2544-H, 11-13-09
2046-H, 03-12-10
2568-H, 02-12-10
2559-H, 01-11-10
40 60
Time (h)
80
Figure 10-14: Temperature profile of five salt cakes from Facility H at 37 °C.
ATmax = 55.80C
(@50°C,10g/10ml)
O
40
30
20
10 -
2559-SC
2568-SC
2555-SC
2544-SC
2046-SC
Replication 2046-H-SC
2046-R1
2046-R2
2046-R3
2046-R4
20
40
Time (h)
60
80
Figure 10-15: Temperature profile of five salt cakes from Facility H at 50 °C.
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60
50 -
Particle size effect:
ATmax (°C) t-maxT (h)
9mm, 12.41 2.20
2 mm, 23.86 1.33
0.05mm, 55.61 1.56
60
Figure 10-16: Effect of particle size of salt cake 2046-H on the temperature
profile at 37 °C.
25
2555-H-SC Chemical treatments
(@37°C, 1 :1)
0.1MHCI
DIW
0.1M NaOH
0.1 M H3P04
Landfill leachate
O
10
50
100 150
Time (h)
200
Figure 10-17: Effect of chemical composition of liquids on the temperature profile
of salt cake 2555-H at 37 °C.
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30 -i
2046-H-SC,Na2HPO4
2046-H-SC, NaH2PO4
2046-H-SC, DIW
20
40
60
Time (h)
80
100
120
Figure 10-18: Effect of phosphorus species in liquids on the temperature profile of
salt cake 2046-H at 37 °C.
25 -
2046-H
2046-H with 1% NaH2PO4
2046-H with 5% NaH2PO
2046-H with 10% NaH2PO4
2046-H with 20% NaH2PO4-l
2046-H with 20% NaH2PO4-
15
20
Time (h)
Figure 10-19: Effect of mix solid phosphorus compounds on the salt cake 2046-H
temperature profile at 50 °C.
The results further confirmed that chemical composition of liquids significantly changed the pattern of temperature
change. Phosphate solution or the high amount of DOC leachate (pH6.2, DOC 20,000 mg/L) from the landfill, two
different type of ligands for aluminum complex, might have reduced the temperature increase from the reaction of salt
cake with water.
Facility J
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Facility J has four samples, which were collected from November 20, 2009 to Feb 5, 2010. Their temperature
responses were quite similar at the 37 °C environmental condition, but changed at the higher temperature (e.g. 50 °C)
(Figure 7-2). The size effect is also very significant, the response of the small particle is very intensive (Table 6-2, and
Figure 7-3). Phosphate in the liquids can also significantly reduce the temperature increase at the short time scale (up
to 5 days), but with multiple peaks (Figure 7-4).
Table 10-9: The Temperature Pattern of Facility J
Sample ID
37 °C
AT
tmax-1
(h)
50 °C
AT
tmax-T
(h)
2512-J-SC
2515-J-SC
2517-J-SC
2519-J-SC
Maximum
Minimum
Average
9.2
7.8
8.4
6.6
9.2
6.6
8.0
0.9
1.1
1.5
1.1
1.5
0.9
1.1
22.5
11.6
15.6
9.4
22.5
9.4
14.8
1.1
0.8
0.9
0.6
1.1
0.6
0.8
2517-J, 01-08-10
2515-J, 12-02-10
2519-J, 02-05-10
2512-J, 11-20-09
20
40 60
Time (h)
80
Figure 10-20: Temperature profile of four salt cakes from Facility J at 37 °C.
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25
20
ATmax = 22.4°C
OoC, 10g/10ml)
2512-J
2515-J
2517-J
2519-J
80
Figure 10-21: Temperature profile of four salt cakes from Facility J at 50 °C.
AT
100
80
O
60
40
20
Particle size effect
2512-J @37°C
100 n
80 -
60 -
40 -
20 -
9mm,
2mm,
0.05mm,
4.12
9.21
96.11
1.63
0.81
0.23
10
20
30
Time (h)
40
50
60
Figure 10-22: Effect of particle size of salt cake sample 2512-J on the temperature
profile at 37 °C.
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60 -
50 -
40 -
O
o
30 -
20 -
10 -
0 -
Particle size effect
2512-J(S)500C
ATmax(°C) t-maxT(h)
0.05mm, 58.79 0.13
2mm, 16.77 0.53
9mm, 16.07 1.83
20
40
60
Time (h)
80
100
120
Figure 10-23: Effect of particle size of salt cake 2512-J on the temperature profile
at 50 °C.
12
10
2512-J-SC,Na2HPO4
2512-J-SC, NaH2PO4
2512-J-SC, DIW
20
40
60
Time (h)
80
100
120
Figure 10-24: Effect of phosphate solution on the temperature profile of salt cake
2512-J.
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Facility L has five samples, which were collected from December 2, 2009 to April 6, 2010. The highest increased
temperature was Sample 2482-L-SC (51.3 °C @ 50 °C, and 44.0 °C @ 37 °C). Note that orthophosphate salt in the
solution, a strong inorganic ligands of aluminum, can significantly reduce the absolute temperature increase, but with
multiple peaks of temperature
Table 10-10: The Temperature Pattern of Facility L
Sample ID
37 °C
AT
tmax-T
(h)
50 °C
AT
tmax-T
(h)
2482-L-SC
2484-L-SC
2486-L-SC
2488-L-SC
2490-L-SC
Maximum
Minimum
Average
44.0
36.0
15.1
28.7
22.2
44.0
15.1
29.2
1.0
1.1
1.9
1.9
1.5
1.9
1.0
1.5
51.3
40.8
28.0
38.1
28.0
51.3
28.0
37.2
0.4
0.7
0.9
0.7
0.7
0.9
0.4
0.7
O
2490-L, 04-06-10
2488-L, 02-02-10
2484-L, 12-28-09
2482-L, 12-02-09
2486-L, 02-02-10
20
40
80
Time (h)
Figure 10-25: Temperature profile of five salt cakes from Facility L at 37 °C.
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60
ATmax = 51.2°C
50 "* (@50°C,10g/10ml)
O
30 -I
20 -I
10 -
Replication 2490-L-SC
2486-SC
2484-SC
2482-SC
2488-SC
2490-SC
2490-R1
2490-R2
2490-R3
20
40 60
time (h)
80
Figure 10-26: Temperature profile of five salt cakes from Facility L at 50 °C.
2490-L-SC,Na2HPO4
2490-L-SC, NaH2PO4
2490-L-SC, DIW
120
Figure 10-27: Effect of phosphate solution on the temperature profile of salt cake
2490-L at 37 °C.
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Facility M
Facility M has four samples, which were collected from February 24 to May 14, 2010. The highest increased
temperature was Sample 2601-M (56.3 °C @ 50 °C, and 64.2 °C @ 37 °C). It is confirmed that the chemical
composition of liquids significantly change the pattern of temperature, an index of reactivity of salt cake. Inorganic
ligands, e.g., phosphate, is an example to reduce the intensity of reaction at the short term (but only short term).
Table 10-11: The Temperature Pattern of Facility M
Sample ID
37 °C
ATm£
tmax-T
(h)
50 °C
ATmax
tmax-T
(h)
2601-M-SC
2605-M-SC
2609-M-SC
2613-M-SC
Maximum
Minimum
Average
64.1
19.5
46.0
40.0
64.1
19.5
42.4
0.5
1.7
1.0
1.0
1.7
0.5
1.0
56.3
22.4
50.8
39.9
56.3
22.4
42.3
0.3
0.9
0.3
0.5
0.9
0.3
0.5
60 -
o
o
40
< 30 -
20 -
10
ATmax=64.2°C
l@37 C,10g/10ml)
o
%
70 i
60 -
50 -
40 -
30 -
20 -
10 -
0
2609-M-SC, 03-08-10
2601-M-SC, 02-24-10
2605-M-SC, 02-24-10
2613-M-SC, 05-14-10
20
40 60
Time (h)
80
Figure 10-28: Temperature profile of four salt cakes from Facility M at 37 °C.
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60
50 -
ATmax = 56.40C
(@50°C,10g/10ml)
60
2609-SC
2605-SC
2601-SC
2613-SC
O
10
20 30 40
Time (h)
50
60
Figure 10-29: Temperature profile of four salt cakes from Facility M at 50 °C.
60 -i
2613-M-SC
(37°C, 1:1)
0.1 MH3P04
landfill leachate
DIW
0.1MHCI
O.IMNaOH
20
40
time (h)
60
Figure 10-30: Effect of chemical composition of liquids on the temperature profile
of salt cake 2613-M at 37 °C
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2613-M-SC,Na2HPO4
2613-M-SC, NaH2PO4
2613-M-SC, DIW
120
Figure 10-31: Effect of phosphorus species in liquids on the temperature profile of
salt cake 2613-M.
0.2 M Na0HPO
2502-F-SC
2613-M-SC
2046-H-SC
2512-J-SC
2490-L-SC
100
120
Figure 10-32: Effect of 0.2 M NaiHPCh on the temperature profiles of the selected
high reactivity salt cake samples.
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10 -
5 -
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0.2M NaH2PO4
2502-F-SC
2613-M-SC
2046-H-SC
2512-J-SC
2490-L-SC
20 40 60 80
Time (h)
100
120
Figure 10-33: Effect of 0.2 M NaEhPCh on the temperature profiles of the selected
high reactivity salt cake samples.
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Facility N
Facility N has four samples, which were collected from December 28, 2009 to April 6, 2010. The highest increased
temperature was in Sample 2494-N (12.3 °C @ 37 °C) and 2498-N (18.0 °C @ 50 °C). Note some variations among
replications of 2498-N are presented in Figure 10-2, both at 37 °C and 50 °C.
Table 10-12: The temperature pattern of Facility N
Sample ID
37 °C
ATmax
tmax-T
(h)
50 °C
ATmax
tmax-T
(h)
2492-N-SC
2494-N-SC
2496-N-SC
2498-N-SC
Maximum
Minimum
Average
7.1
12.3
6.7
7.2
12.3
6.7
8.4
1.9
1.3
2.9
2.9
2.9
1.3
2.3
7.0
17.1
12.1
18.0
18.0
7.0
13.6
1.4
0.7
1.2
1.9
1.9
0.7
1.3
O
2494-N, 02-02-10
2496-N, 03-08-10
2498-N, 04-06-10
2492-N, 12-28-09
80
Figure 10-34: Temperature profile of four salt cakes from Facility N at 37 °C.
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ATmax=16.9°C
(@50°C,10g/10ml)
2496-SC
2494-SC
2492-SC
2498-SC
Replication for 2498-N-SC
2498-R3
2498-R1
2498-R2
10
20
30 40
Time (h)
50
60
Figure 10-35: Temperature profile of four salt cakes from Facility N at 50 °C.
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Secondary Aluminum Processing Waste: Salt Cake Characterization and Reactivity
11. APPENDIX E: Gas Productivity of Salt Cake
Table E-l Total generated gas volume and composition from salt cake reactivity
Sample ID
2452-B
2454-B
2468-B
2478-B
243 3 -C
2435-C
2532-D
2536-D
2538-D
2540-D
2437-E
243 9-E
2502-F
2504-F
2506-F
2508-F
2510-F
2046-H
2544-H
2555-H
2559-H
2568-H
2512-J
2515-J
2517-J
2519-J
2482-L
2484-L
2486-L
2488-L
2490-L
260 1-M
2605-M
2609-M
2613-M
2492-N
2494-N
2496-N
2498-N
Generated Gas
Volume (ml g"1)
12
7.5
19
30
31
25
25
1.6
24
22
43
28
58
44
45
31
60
15
18
12
22
9.1
35
28
23
19
40
31
13
1.5
13
78
47
210
170
12
21
19
19
CH4
36
35
25
24
14
15
17
90
32
14
14
16
16
8.8
17
12
15
24
18
22
31
21
7.3
16
15
20
24
22
42
49
12
8.7
6.8
3.1
0.5
11
15
14
21
H2
63
63
75
76
86
83
82
0.0
67
84
85
84
83
91
83
88
85
74
81
76
66
77
92
84
84
79
75
78
57
47
88
91
93
97
99
88
83
85
79
(ppbv)
3,600
4,900
1,100
400
230
140
88
18,000
1,600
510
50
78
65
49
95
160
520
210
160
180
150
2,800
70
120
130
2,700
80
1,300
1,800
1,500
170
510
240
20
31
180
160
420
190
NHs-gas
0.96
2.2
0.66
0.83
0.30
1.6
0.81
9.9
0.21
1.8
0.68
0.42
0.67
0.09
0.30
0.23
0.08
2.6
1.4
1.8
2.2
2.1
0.33
0.27
0.64
0.39
0.71
0.43
1.4
3.8
0.001
0.15
0.28
0.04
0.06
0.50
1.8
0.23
0.07
NH4+-liquid
(nigL1)
1,200
730
1,000
1,100
740
250
30
840
170
620
210
880
380
1,100
51
730
1,100
240
740
540
460
1,400
170
110
200
580
260
1,500
1,500
290
95
660
450
350
500
230
310
490
110
*L/S =10:1, 10 g SC, < 2 mm, 100 ml DIW, @ 50 °C, 5 d.
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Secondary Aluminum Processing Waste: Salt Cake Characterization and Reactivity
12. APPENDIX F: Quality Assurance Project Plan (QAPP)
National Risk Management Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
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Amendment 2
Quality Assurance Project Plan
Category IV Measurement Project
Management Options for the Safe Deposit
of Secondary Aluminum Processing Waste
Original QA ID: L-13928
U.S. Environment Protection Agency Contract No. EP-C-11-006
Work Assignment No. 2-26 (1-26, 0-26)
Prepared for:
Thabet Tolaymat, PhD, Principal Investigator
Robert Ford, PhD, Co-Principal Investigator
U.S. Environmental Protection Agency
Office of Research and Development
National Risk Management Research Laboratory
Land Remediation and Pollution Control Division
5995 Center Hill Ave, Cincinnati, Ohio, USA
Prepared by:
Xiaolan Huang, PhD
Pegasus Technical Services, Inc.
Cincinnati, OH 45219
Revision 1
June 6, 2013
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SUMMARY OF WORK ASSIGNMENT 2-26 AMENDMENT 2
QUALITY ASSURANCE PROJECT PLAN CHANGES
The Work Assignment (WA) 1-26 Amendment 2 Quality Assurance Project Plan (QAPP) titled
Management Options for the Safe Deposit of Secondary Aluminum Processing Waste, dated
February 19, 2013, QA ID No. L-13928, is being revised to address the deficiencies identified
during the EPA QA Audit that was conducted on April 9, 2013.
The following Sections in this QAPP have been revised:
Quality Assurance Project Plan Approval List
Section 2.1.2 (page 10, 11)
Section 3.4.1 (page 16)
Section 3.4.3 (page 20, 22)
Section 3.6.4 (page 25)
Section 3.6.5 (page 26)
Section 4.5 (page 27)
Section 6.1 (Table 6.1) (page 35, 36)
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Quality Assurance Project Plan Approval List
Pegasus Technical Services, Inc. Concurrences:
1. Raghu Venkatapathy, PhD, On-Site Technical Manager
Signature Date
2. Xiaolan Huang, PhD, WA Leader
Signature Date
3. Steven Jones, ASQ CQA/CQE, Contract Quality Assurance Manager
Signature Date
U.S. Environmental Protection Agency Approval for Implementation:
1. Thabet Tolaymat, PhD, Principal Investigator
Signature
2. Robert Ford, PhD, Principal Investigator
Signature Date
3. Jim Voit, LRPCD Quality Assurance Manager
Signature Date
Distribution List:
- Dr. Thabet Tolaymat, Principal Investigator , NRMRL, U.S. EPA.
- Dr. Robert Ford, Co-Pi, NRMRL, U. S. EPA.
- Mr. Stephen Wright, Project Officer, NRMRL, U.S. EPA.
- Mr. Jim Voit, QA Manager, LRPCD, U. S. EPA.
- Mr. David Carson, Branch Chief, NRMRL, U.S. EPA*.
Dr. Raghu Venkatapathy, On-Site Technical Manager, PTSI.
Mr. Steven Jones, Contract QA Manager, Shaw Environmental & Infrastructure, Inc.
Dr. Xiaolan Huang, Dr. Mahendranath Arambewela, Ms. Wenwen Yang, Ms. Renata
Adkins and Dr. Amro El Badawy, On-Site Contractors, PTSI.
Mr.Cluxton Phillip, On-Site Contractor
- Mr. Casey Warren, U.S. EPA Student Contractors.
* These individuals are receiving copies of the QAPP and subsequent revisions at their request.
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TABLE OF CONTENTS
List of Tables
List of Figures
1.0 Project Description and Objectives
1.1 Proj ect Description
1.2 Project Objectives
2.0 Organization and Responsibilities
2.1 Project Personnel
2.2 Proj ect Schedule
3.0 Scientific Approach
3.1 Site Identification and SAP Waste Sampling
3.2 Sample Processing
3.3 Sample Characterization
3.4 SAP Waste Reactivity Testing
3.5 Toxicity Characteristic Leaching Procedure (TCLP) of SAP Waste
3.5 Model Thermal Change in landfills Accepting SAP Waste
4.0 Sampling Procedures
4.1 Site Preparation
4.2. Sample Procedures
4.3 Sample Containers/Quantities
4.4 Sample Preservation/Hold Time
4.5 Sample Identification
5.0 Measurement Procedures
5.1 SAP Waste Characterization
6
7
10
10
11
12
12
12
12
14
23
24
26
26
26
26
26
26
28
28
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5.2 Experimental Sampling 29
5.3 Measurement Methods 30
6.0 Quality Metrics (QA/QC Checks) 32
6.1 Data Quality Objectives and Criteria 32
6.2 Types of QC Samples 36
6.3 Model Calibration and Validation 37
7.0 Data Analysis, Interpretation and Management 38
7.1 Data Reporting 38
7.2 Data Handling and Disposal 3 8
7.3 Data Reduction and Validation 39
7.4 Data Storage 39
8.0 Reporting 40
9.0 Reference 41
10.0 Appendix SOP 43
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LIST OF TABLES
Table 2.1 Project Organization and Responsibilities 12
Table 3.1 Test Results of the Gas Volume Measurement Using Syringe 18
Table 3.2 The Relation of Heat Generation with Resistance, Current and Time 22
Table 5.1 Summary of Solid Sampling and Schedule 28
Table 5.2 Sample Containers, Preservation and Storage Time 28
Table 5.3 Summary of Sampling of the Waste Reactivity Testing 29
Table 5.4 Outline of Analysis Methods 30
Table 6.1 Summary of QA/QC Checks 33
Table 6.2 MDL, Precision and Accuracy for ICP-AES Method 6010B 36
Table 7.1 Reporting Units 38
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LIST OF FIGURES
Figure 2.1 Project Schedule 12
Figure 3.1 Temperature Generation Potential Apparatus 18
Figure 3.2 Reactivity Test Apparatus for Gas Production 19
Figure 3.3 Gas Volume Verification Test Apparatus 20
Figure 3.4 Reactivity Test Apparatus for Measuring Heat Change 22
Figure 3.5 Example: Calibration Curve of Generated Heat and the Sum of 23
Temperature Change
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SECTION 1.0
PROJECT DESCRIPTION AND OBJECTIVES
1.1 Project Description
Secondary aluminum processing (SAP) wastes result from the smelting of primary aluminum (Al)
waste and processing of recycled aluminum. These wastes include 'saltcake,' and air pollution
control filter dust (bag house dust) that might contain oxidized aluminum, small particles of
aluminum metal, aluminum nitrides, aluminum carbides, and metal oxides. In 1999, it was
reported that approximately 2 billion pounds of SAP waste was disposed of in U.S. landfills (U.S.
DOE, 1999).
The disposal of vast amounts of SAP wastes containing various Al species can pose a potential
threat to the management of landfills. This is because SAP waste can react with water and
generate heat as well as flammable gases such as hydrogen and methane. Additionally, when
placed in a municipal waste landfill, this reaction may be sufficiently exothermic to initiate the
combustion or pyrolysis of other waste materials.
Some municipal waste landfills across the country have experienced significant problems
attributed to the SAP wastes in landfills. Some of these events are subsurface heating, excessive
subsidence and slope instability, engineering component failure, and dangerous onsite working
conditions. Aside from these potential impacts, there may be environmental and community health
impacts associated with air emissions, surface water, and groundwater releases.
In light of these problems, the U.S. Environmental Protection Agency (EPA) is initiating a
collaborative research effort to examine safe management practices for SAP wastes. The EPA is
seeking to better understand SAP waste material, its potential risk, and strategies to prevent, arrest,
or exhaust potential peril for safe management of municipal landfills. It is expected that inroads
will be made towards the creation of technologies or management practices whereby SAP wastes
can be safely deposited in landfills, avoiding future problems.
The EPA has established a coordinating committee to provide technical assistance and project
guidance through project advisory meetings, report reviews, and participation in an online research
collaboration website.
1.2 Project Objectives
The current study aimed at exploring the chemical composition and mineral phase of the waste
from SAP industry. Furthermore, temperature change and gas generation after reaction with water
or landfill leachate is studying the potential reactivity in laboratory setting. This allows for a better
understanding of the behavior of the SAP wastes when disposed in landfills. Additionally, this
work provides the methodology to investigate such reactions and thus provides the criteria for
determining whether a particular sample of salt cake or baghouse dust can be landfilled.
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It is noted that this is a preliminary study. The potential relationship between the chemical
composition and reactivity, either gas or heat generation, will be tested and identified in the
laboratory setting. Based on the findings, further research will be carried out to investigate and
validate the relationships identified in this work.
The specific objectives of the study are:
• To identify and characterize the metal constituents in SAP wastes.
• To identify and semi-quantify the dominant mineral phase present in the SAP wastes using
XRD analysis.
• To evaluate temperature change after SAP wastes exposure to water and/or landfill
leachate.
• To identify and characterize the generated gas quantity and quality when SAP waste reacts
with water and/or landfill leachate.
• To investigate the metal composition of SAP waste leachate after SAP reaction with water
and /or landfill leachate.
• To conduct Toxicity Characteristics Leaching Procedure (TCLP) to evaluate the possibility
of heavy metal leaching from SAP waste.
• To evaluate heat generation after SAP wastes exposure to water and/or landfill leachate.
• To simulate the thermal changes in Municipal Solid Waste (MSW) landfills as a result of co-
disposal of SAP waste with MSW using the TEMP/W model.
• To develop methodology to assess the potential risk of SAP reaction with water and /or
landfill leachate.
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SECTION 2.0
ORGANIZATION AND RESPONSIBILITIES
2.1 Project Personnel
2.1.1 EPA Staff
The EPA Principal Investigators (PI)_for this project are Dr. Thabet Tolaymat and Dr. Robert Ford.
Dr. Tolaymat is responsible for overseeing the paperwork associated with the management of the
project, and the research procedures associated with total metals analysis. Dr. Ford is responsible
for overseeing and conducting research procedures associated with X-ray diffraction, Fourier-
transformation infrared spectroscopy, scanning electron microscopy, and thermogravimetric
analysis. Dr. Tolaymat and Dr. Ford will also be responsible for coordinating the collection of
SAP waste samples through the Aluminum Association and the Environmental Research and
Education Foundation. Dr. Tolaymat and Dr. Ford will meet monthly to discuss the progress of
the research. Mr. Stephen Wright is the EPA Project Officer for EPA Contract No EP-C-05-056.
Mr. Jim Voit is the EPA Land Remediation and Pollution Control Division (LRPCD) Quality
Assurance (QA) Manager responsible for approving the Quality Assurance Project Plan (QAPP).
Mr. Casey Warren, EPA Student Contractors, and Mr.Cluxton Phillip, EPA On-Site Contractor,
are responsible for providing support to the PTSI WA Leader and EPA WA Manager for operation
of the experiment, data collection, analysis and reporting.
2.1.2 PTSI Staff
Dr. Karen Koran is the Pegasus Technical Services, Inc. (PTSI) Project Manager. Dr.
Raghuraman Venkatapathy, PTSI On-Site Technical Manager, is responsible for
supervision of the PTSI staff. Mr. Steven Jones, ASQ CQA/CQE, of Shaw Environmental
& Infrastructure, Inc. (Shaw), a subcontractor to Pegasus in this contract, is the PTSI
Contract QA Manager and is responsible for oversight PTSI quality program
implementation and the review of this QAPP. Dr. Xiaolan Huang ,the Pegasus WA Leader,
is responsible for preparation of the QAPP, setup and operation of the experiment, data
collection, analysis and reporting. Dr. Mahendranath Arambewela, Ms. Wenwen Yang, Ms.
Renata Adkins and Dr. Amro El-Badawy, PTSI On-Site Technical Staff, are responsible
for providing support to the PTSI WA Leader for operation of the experiment, data
collection, analysis and reporting. Dr. Mahendranath Arambewela is also responsible for
ICP and AA analysis, and Ms. Wenwen Yang for 1C and GC analysis.
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Table 2.1 _Project Organization and Responsibilities
Name
Mr. Stephen Wright
Dr. Thabet Tolaymat
Dr. Robert Ford
Mr. Jim Voit
Mr. Steven Jones
Dr. Karen Koran
Dr. Raghu Venkataphathy
Dr. Xiaolan Huang
Dr. Amro El Badawy
Dr. Mahendranath
Arambewela
Ms. RenataAdkins
Ms. Wenwen Yang
Mr.Cluxton Phillip
Mr. Casey Warren
Phone/email
(513)569-7610
wright.stephen@epa.gov
(513)487-2860
tolaymat.thabet@epa.gov
(513)569-7501
robert. ford@epa.gov
(513)487-2867
voit.jim@epa.gov
(513)782-4655
Steve . S . Jones@shawgrp .com
(513)569-7304
Koran.Koren@epa.gov
(513)569-7077
Venkatapathy.Raghuraman@epa.gov
(513)569-7409
Huang. Xiaolan@epa.gov
(513)569-7688
el-badawy.amro@epa.gov
(513)569-7127
mahendranath.arambewela@epa.gov
(513)487-2127
adkins. renata@epa.gov
(513)487-2559
yang.wenwen@epa.gov
(513)487-2875
Cluxton.phillip@epa.gov
(513)569-7257
Warren . Casey@epa.gov
Responsibilities
EPA Project Officer
EPA Principal Investigator
EPA Co -Principal Investigator
EPA LRPCD QA Manager
PTSI Contract QA Manager
PTSI Project Manager
PTSI On-Site Technical
Manager
PTSI On-Site Staff
PTSI On-Site Staff
PTSI On-Site Staff
PTSI On-Site Staff
PTSI On-Site Staff
On-Site Contractor
Student Contractor
2.2 Project Schedule
The projected schedule and the main activities are shown in Figure 2.1.
Activities
QAPP/HASP writing
Samples being produced
Sample characterization
Modeling
Report/manuscript writing
Sept.-10
May-11
Sept-11
May-12
=
Sept-12
May-13
Sept.-13
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SECTION 3.0
SCIENTIFIC APPROACH
3.1 Site Identification and SAP Waste Sampling
Facilities that generate SAP wastes will be identified in collaboration with the Aluminum
Association and the Environmental Research and Education Foundation. Each facility will sample
both salt cake (SC) and bag house dust (BHD) at different times. The average number of samples
to be obtained from each facility is 4. The number of SC samples to be obtained will be at least 35
and the number of BHD samples will be at least 50.
3.2 Sample processing
Upon receipt, samples will be logged and then stored in a Hazardous Storage Unit located at the
EPA Center Hill Laboratory (CHL) Facility. The storage unit is equipped with a chemical fire
suppression system in case any unintended SAP waste reaction occurs. The fire extinguishing
system is a chemical system that does not use water since the samples may be water reactive.
Within two weeks of receipt, in order to obtain representative subsamples, the individual samples
will be processed as follows:
• The samples will be placed in a stainless steel pan and crushed to pass a 9-mm sieve.
• After thorough mixing, approximately 0.5 kg of the 9-mm sieved materials will be further size
reduced down to a size of 2 mm using a grinding machine (Preiser Scientific).
• Approximately 50 gm of the 2 mm size SAP waste will be further reduced to a size of 0.05 mm using
a sealed stainless steel jar mill equipped with zirconia grinding beads. The jar mill will be rotated at
20 rpm for 24 hours.
• The 2- mm size will be used for the chemical and physical analysis (pH, conductivity, moisture
content and water holding capacity) in the laboratory and the 0.05-mm size will be used for the
chemical and XRD analysis.
3.3 Sample Characterization
3.3.1 Physical Characterization
3.3.1.1 Moisture Content (MC)
The moisture content of the salt cake samples will be determined. The oven temperature will be set at 105 °C
following ASTM Method D-2216 (refer to SOP 4).
3.3.1.2 Water Holding Capacity
Following the principles of ASTM Method F1815-06 (SOP 5), approximately 10 g of sample will be placed into a
cylinder and cold water (Temperature < 12 °C) will be added to make it saturated. The saturated samples will be
placed on top of an absorbent membrane until the excess water is drawn away by gravity. Once equilibrium is reached
(usually 16 h, overnight), the water holding capacity will be calculated based on the weight of the water held in the
sample versus the sample dry weight.
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3.3.1.3pH and Conductivity (EC)
The salt cake samples will be reacted with water (1:20, 5 gram/100 ml DIW) and will be incubated
for a week at 50 °C. At the end of the incubation period, the samples will be filtered using a 0.45 jim
PVDF media and the pH and EC will be determined (SOP 3).
3.3.2 Metal Composition
• The SAP waste will be acid digested using EPA SW846 Method 3051A, Microwave assisted acid
digestion of sediments, sludges, soils and oils. Following the suggestion of 3051A, the mixed acid
(1 HCI and 3 HNO3) will been employed instead of concentrated HNO3 only, a temperature will be
set as 185 °C instead of 175 °C, and hold time will be extended from 10 to 30 minutes. The amount
of SAP waste to be digested will be 0.1 g instead of 0.5 g because of the high metal content (refer
to SOP 8).
• The macro-elements (Al, Ag, Ba, Fe, Mn, Cu, Zn, K, Na, Ca, and S) will be determined by EPA
Method 6010B using a Thermo ICP-AES located at the Kirby laboratory at the EPA Center Hill
Facility. Trace metals (Pb, Cd, Cr, As and Se) will be analyzed by a Perkin-Elmer graphite furnace AA
separately (refer to SOP 9) or Thermo ICP-AES.
3.3.3 Mineral Phase
Mineral phase of the 0.05 mm size SAP waste (prepared as described in section 3.2) will be
investigated using a Philips X'Pert-MPD system at the EPA CHL Facility (refer to SOP 10). The
XRD will be operated under the following conditions:
Scan Axis Gonio
Start Position [°2Th.] 10.0000
End Position [°2Th.] 106.7800
Step Size [°2Th.] 0.0100
Scan Step Time [s] 5.0000
Scan Type Pre-set time
Offset [°2Th.] 0.0000
Irradiated Length [mm] 10.00
Specimen Length [mm] 10.00
Receiving Slit Size [mm] 0.1000
Anode Material Cu
K-Alphal [A] 1.54060
K-Alpha2 [A] 1.54443
K-Beta[A] 1.39225
K-A2 / K-A1 Ratio 0.50000
Generator Settings 40 mA, 45 kV
Diffractometer Type XPert MPD
Goniometer Radius [mm] 200.00
Dist. Focus-Diverg. Slit [mm] 91.00
Incident Beam Monochromator No
Spinning Yes
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The powder diffraction file (PDF) patterns database from the International Centre for Diffraction
Data (ICDD) will be employed for the search, match, and identification. A subset of reference
patterns will built for all studied salt cake samples. The semi-quantitative phase analysis will used
by the X'Pert HighScore Plus software, based on the CHUNG Normalized RTR Method [66]. The
relative intensity of each phase is given by the scale factor, which is determined by least squares fit
through all matching reference pattern lines in X'Pert HighScore. The concentration X of phase a is
calculated using:
DID irel
KIK«'(hkl)K
where RIRoc is Reference Intensity Ratio, based on the relative net peak height ratio of the strongest
line (Irel = 100%) of the phase and of the strongest line of corundum, measured with copper Ka
radiation in a mixture of equal weight percentages and I(hkl)K is Intensity of reflection of hkl in phase
a. hkl is reflection indices.
It is important to note that the normalization used in this method assumes that the sum of all
identified phases is 100%. This means that there are no unidentified crystalline phases or an
amorphous phase present in the sample. Only under these conditions can meaningful, semi-
quantitative results be obtained.
3.4 SAP Waste Reactivity Testing
The reactivity of SAP waste with liquids will be evaluated using two approaches. The first one is
to quantify the temperature change and the second one is to measure the chemical changes
including gas and leachate quality. Different effects of key variables on the temperature change of
selected samples will be tested. The samples will be selected based on the mineral phase types
(i.e., high metallic aluminum, high aluminum nitride, high aluminum oxide and a combination of
the 3 mineral phases) obtained from the XRD analysis. These variables include the solid to liquid
ratio, particle size of salt cake, the chemical composition of the solution, and the environmental
temperature. Based on these preliminary investigations, a protocol of the temperature profile study
for all samples will be prepared. More details in regards to the evaluation of the impact of the
previously mentioned key variables on the temperature change upon liquid addition to the SAP
waste are described below:
A. Effect of Solid to Liquid Ratio and Mass of Aluminum Dross
The change in temperature will be influenced by the amount of liquid and the mass of SAP waste.
Four samples of SAP waste will be selected to investigate the effect of solid to liquid ratio on the
temperature change upon reaction with water. Three sets of experiments will be conducted at 50 °C.
The samples will be prepared as outlined in section 3.4.1 with the following changes as follows:
• Experiment 1: the solid mass is fixed (10 gm) and the liquid volume will be 3, 5, 10 and 15 ml of
preheated Dl water.
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• Experiment 2: the liquid volume is fixed (3 ml) and the solid weight will be 5, 10 and 15 gm.
• Experiment 3: The ratio of solid to liquid is fixed at 10:3, 10:5 and 1:1. For example in the case of
10:3 ratio the investigated amounts will be 5g:1.5 ml, 10g:3ml, 15g:4.5 ml and 20g:6ml of liquid.
B. Effect of Particle Size of Aluminum Dross
Particle size is another major factor that may have an impact on the temperature change upon the
reaction of SAP waste with liquids. The smaller the particle size the higher the surface area to
volume ratio and consequently the reactivity is expected to be higher. Four samples will be tested
as follows:
• Three different particle sizes will be tested (0.05 mm, 2 mm, and 9 mm) for salt cake.
• The environmental temperature will be maintained at 37°C and 50°C.
• The solid to liquid ratio will be 1 to 1 (lOg salt cake with 10 ml Dl water).
C. Effect of Liquid Chemical Composition
Once SAP waste is disposed in landfills, the chemical composition of the leachate (such as,
volatile fatty acids, organic matter, pH) will influence the reactivity of this waste. Therefore,
various chemical composition of the liquid will be investigated as follows:
• Dl water (pH 6.5), 0.1 M HCI (pH 1.0), 0.1 M NaOH (pH 13), 0.1M H3PO4 (pH1.65), 0.1M NaH2PO4
(pH 5.6),0.1M Na2HPO4 (pH 8.2), and landfill leachate (pH 6.2, DOC-20,OOOmg/L).
The ratio of solid to liquid will be fixed at 1 to 1 (10 g salt cake with 10 ml liquid).
D. Effect of Environmental Temperature
High temperature may trigger the reaction of metallic aluminum with liquid . Additionally, some
components of the SAP waste such as aluminum nitride and aluminum carbide can react at low
temperature. Thus, the impact of environmental temperature on the reactivity of SAP waste will be
evaluated as follows:
• The environmental temperatures to be investigated will be 20, 37 and 50°C.
• The solid to liquid ratio will be fixed at 1 to 1 (10 g aluminum dross with 10 ml liquid). Dl water will
be used as the liquid.
3.4.1. Temperature Generation Potential
Temperature increase is one of the key parameters indicating a reaction between salt cake and,
usually, water. The increase in temperature caused by the reaction of salt cake and baghouse dust
with liquid will be evaluated as follows:
• A sample of 10 gram of the size reduced salt cake (<2 mm) or baghouse dust will be placed in a 60
ml VOAvial.
• The vial will be sealed and purged with argon for 10 minutes.
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The vial will be then connected to a 1-L Tedlar bag (for pressure relief).
The VOA vial with the sample will be pre-heated to a certain temperature (37 and 50°C) for 6 hours
in order to achieve the required temperature.
The vial temperature will be monitored and logged using a thermocouple wire placed in the sample.
A 10 ml of pre-heated Dl water (same sample temperature) will be then added to the vial. The
temperature change will be recorded over time for at least 72 hours till no temperature change due
to the reaction.
After the reaction completion, the gas in the Tedlar Bag will be released in the hood.
Usually, 6 to 12 vials will be grouped as one set in an insulated box placed in a temperature
controlled system. For quality assurance, at least one control sample will be included with each
sample group. The control sample is composed of pure quartz sand having the same sample weight
and will be processed as the SAP waste samples. The temperature of the control should be within 2
degrees of the set temperature. It was assumed that the average temperature difference between the
control and sample was 0 in the last 10 hours of measurement. To isolate the heat transfer among
the vials insulation materials will be placed between the vials in the box. Figure 3.1 presents a
schematic as well as a photo of the experimental setup. Moreover, reference materials (sodium
chloride, potassium chloride, aluminum nitride, aluminum carbide, aluminum oxide and powder
metallic aluminum) will be tested to evaluate the interactions of pure aluminum compounds upon
liquid addition under the same experimental conditions. The evaluation will follow the same steps
outlined earlier for SAP waste samples.
3.4.2. Gas Generation and Leachate Chemistry
Gas production potential and leachate chemistry of salt cake as a result of liquid addition will be
evaluated under anaerobic conditions in order to mimic most MSW landfills conditions. The
experimental procedure for measuring the gas generation and leachate quality is summarized below
and schematic of the experimental setup is presented in Figure 3.2:
• A 5 g of size reduced SAP Waste Sample (salt cake sample (<2 mm) or baghouse dust) will be placed
into a 500 ml lined media bottle. Reference materials (sodium chloride, potassium chloride,
aluminum nitride, aluminum carbide, aluminum oxide and powder metallic aluminum) will also be
tested.
• The bottle will be then capped using a lypholization rubber stopper.
• The sealed bottle will be purged with argon for 10 minutes.
• A 100 ml of oxygen-free pre-heated Dl water (50°C ) will be added to the bottle.
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Temperature Data Logger
Thermocouple wire
1:1 Ratio of aluminum
dross
and Water
lOg solids: 10 ml water
Tedlar bag (gas
capture) for relief
pressure
SOmlVoAVial
Figure 3.1: Temperature generation potential apparatus.
A 1-L Tedlar bag will be connected to the bottle for the collection of the generated gas.
The bottle will then be incubated for 7 days at 50°C.
The Tedlar bag will be disconnected and equilibrated to room temperature and then the gas
quantity and quality will be measured. The gas quantity will be measured using a gas syringe and
the quality will be measured using Agilent Gas Chromatograph (SOP 1 and 2).
A 20 ml liquid sample will be taken (using a syringe) from the sealed bottle for liquid ammonia
analysis (SOP 7).
The rest of the liquid will be filtered using a 0.45 u.m PVDF filter media and the pH and conductivity
of leachate will be measured (SOP 3).
After measuring the pH and conductivity, the liquid samples will be used for anions and metals
analysis. The solution for metal analysis will be preserved by acidification using trace metal grade
nitric acid to a pH < 2.0 (SOP 9); the solution for anions analysis will be stored at 4°C (SOP 10).
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The experimental setup will be checked for leaks using a gas leak detection fluid ( e.g. LEAK-
SEEK®, or soap) before and after the experiment. If any leak is found, the experiment will
repeated.
Tedlar bag (gas capture) for off-
line analysis
Three-port teflon cap
One-way gas valve (^
n n
Headspace
Dl-Water
SAP Waste Sample or
Reference Materials
Figure 3.2: Reactivity test apparatus for gas production.
3.4.2.1 Gas Volume and Composition
The Gas quantity will be measured using a 60 ml air tight gas syringe per EPA OPPTS method
835.3400. The accuracy of measuring gas volume in a Tedlar bag using a syringe was confirmed in
our lab by performing the following test (the experimental setup mimics the test condition and the
schematic is presented in Figure 3.3):
• A 5 g of sand sample was placed into a 500 ml lined media bottle and 100 ml of Dl water was added
to the sand.
• The bottle was capped using a lypholization rubber stopper.
• The sealed bottle was connected to a 1 L Tedlar bag.
• The bottle was then purged with argon at a known flow rate for a certain time (Table 3.1). A flow
meter (Cole Parmer) calibrated to argon gas flow was used to measure the actual flow rate from an
argon gas cylinder.
• After purging, the gas volume in the Tedlar bag was measured using a syringe and the results were
compared to theoretical volume of argon purged.
• The results show that the difference between the actual volume of gas purged and the collected
volume using a syringe was < 5% (TableS.l).
Tedlar bag (gas capture)
One-way gas valve
Gas flow meter
', Gas flow direction
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Figure 3.3: Gas volume verification test apparatus. Green arrows show the gas flow direction
Table 3.1 Test results of the gas volume measurement using syringe
Gas flow rate
(ml per min)
120
120
117
117
115
115
Purging
time
(min)
4
4
4
4
2
O
Actual gas
volume
purged
(mL)
480
480
468
468
225
345
Gas
measured
using syringe
(mL)
495
505
480
465
230
345
%
Difference
3.0
5.0
2.5
0.6
2.2
0.0
The gas composition will be analyzed for CH4, CO2, N2, H2, Ch and N2O and IHbS. The CH4, CCh,
N2, H2 and O2 concentration will be measured using a GC TCD/FID, the N2O concentration will
be measured using GC/ECD (SOP 2) and the IHbS will be measured using a Jerome meter
(instrument manual). Additionally, the ammonia concentration in the gas will be measured using
an ammonia selective electrode.
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3.4.2.2 Leachate Quality Analysis
The leachate will be analyzed for pH, conductivity (SOP 3), ammonia (SOP 7) and metals (SOP
9). The pH and conductivity will be measured using pH and conductivity probes. The dissolved
ammonia in the leachate will be analyzed using Ammonia ion selective electrode. The metal
analysis will be performed using a Thermo ICP-AES or Graphite Furnace AA based on the metal
concentration. The target metals include Al, As, Cr, Cd, Pb, Se, Fe, Cu, Zn, K, Na, Ca, and Mn.
3.4.3. Heat Generation
Heat generation is one of the key parameters to access the safety of aluminum dross disposal in
landfills. A custom reaction calorimeter with double vessels has be designed and fabricated to
determine the heat generation rate from the aluminum dross reaction (Figure 3.4). In order to
obtain the isoperibol condition (constant temperature in the thermal jacket surrounding the reaction
vessel), the whole device will be set up in a temperature controlled environment (e.g. temperature
room 37.5°C or incubation oven, 50°C). Ethylene Glycol will be used as a thermal buffer since it
has a low specific heat capacity. The experimental procedure for measuring the heat generation is
summarized as follows:
• A sample of 5 gram of the size reduced salt cake (<0.05 mm) or baghouse dust or sand (as control)
will be placed in a 40 ml inner-vessel (e.g. 40 ml VOA vial with screw cap).
• The inner-vessel with sample will be capped and then put into an outer-vessel (custom made 250
ml vial with a three-port Teflon cap, see Figure 3.4), which contains pre-equilibrium 90 ml Ethylene
Glycol. Three thermocouple wires will be placed in the Ethylene Glycol solution. The Ethylene Glycol
solution temperature will be allowed to equilibrate overnight (16 h).
• The inner-vessel will then be connected to a 1-L Tedlar bag (for pressure relief).
• A 10 ml of pre-heated liquid (e.g., Dl water) (same sample temperature) will be then injected to the
inner-vessel by syringe into sample or sand (control). The Ethylene Glycol solution temperature will
be recorded over time for at least 72 hours till no temperature change is observed from the reaction.
• The Ethylene Glycol solution temperature will be monitored every two minutes and logged using
date logger.
• The average temperature readings from the three thermocouple wires in the outer vessel from the
test sample will be used to calculate the difference with the control (Sand) (AT). The sum of
temperature change with control ( ZAT) will be used to access the released heat from sample.
• After the reaction completion, the gas in the Tedlar Bag will be released in the laboratory hood.
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Tedlar bag, 1L
Temperature
datalogger |<3o*W8WS'"lte
Syringe pusher
Temperature
Controlled Room
Thermal buffer:
Ethylene Glycol Solution
Saltcake with
water, e.g.
5g/10mlDIW
Thermal insulation materials
Figure 3.4: Reactivity Test Apparatus for Measuring Heat Change
Table 3.2 (below) will be used for calibration as the standard heat generated in the experiments.
The heat from the resistance or from the reaction of aluminum dross will be monitored for
temperature change. The standard value of heat is based on resistance with different currents and
time. Figure 3.5 (below) is the standard curve from the sum of temperature change to the released
heat, which is based on the resistance (from Table 3.2). With the Table 3.2 and Figure 3.5, the
heat from the reaction of aluminum dross can be estimated.
• A calibration between the above mentioned sum of temperature change (IAT) and the input heat,
generated by a fixed resistance (R) with the adjustable electric current (I) with time. The power (P)
and voltage (V) was calculated as follows:
P = Ix V
V = IxR
• The generated heat (Q) from resistance is the function of power with time (Q = P x t). The
following Table 3.2 is the example of the input energy (released heat) with the adjusted current
and time, used for calibration.
• Relationship between the generated heat (Q) and the sum of temperature change (IAT) has
been demonstrated as linear, and it was also confirmed that there were no difference of ZAT
among the heat time with the same inputted heat (Q). The calibration curve in the current
laboratory setting at temperature room and input energy (generated heat Q, kJ) is as following:
Q = 0.006ZAT
Table 3.2 The Relation of Heat Generation with Resistance, Current and Time
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Energy
(Joules)
3000
5000
6000
10000
20000
30000
10000
20000
Time
Energized
(Minutes)
60
60
60
60
60
60
120
120
Power
Applied
(Watts)
0.8333
1.3889
1.6667
2.7778
5.5556
8.3333
1.3889
2.7778
Current
(Amps)
0.1349
0.1741
0.1908
0.2463
0.3483
0.4266
0.1741
0.2463
Potential
(Volts)
6.1779
7.9757
8.7369
11.2793
15.9513
19.5363
7.9757
11.2793
Resistance
(Ohms)
45.80
45.80
45.80
45.80
45.80
45.80
45.80
45.80
35 -
30 -
25
a20
4-»
" 15
J-J
10 -
5 -
0
y = O.OOSx
R2 = 0.993
0 1000 2000 3000 4000 5000
Sum of Temperature change ATsum (C/2min)
6000
Figure 3.5: Example of calibration curve of generated heat and the sum of temperature
change (37°C temperature controlled room)
Usually, 4 double-vessels will be grouped as one set in an insulated box placed in a temperature
controlled system. For quality assurance, at least one double-vessel will be included as standard or
control with each sample group. Two or three thermocouples will be placed in the control vessel.
The relative standard deviation of the temperature in the control vessel should be within 5%. If the
temperature of control fails, the experiment will be repeated. It was assumed that 0 heat generation
in the last 10 hours of measurement and the average temperature difference between the control
and sample was 0 in that period. The system will be verified every 6 months with one standard,
and the slope of £AT/ Q will be calculated. The variation limit of £AT/ Q is ± 15%. If the
verification fails, the heat experiment in that period will be repeated. To isolate the heat transfer
among the vials, insulation materials will be placed between the vials in the box.
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Similar to the temperature profile study, many factors might influence the heat generation process,
e.g. the mass of salt cake, particles size, composition of liquids, and environmental temperature.
These factors will also be tested.
Moreover, reference materials (sodium chloride, potassium chloride, aluminum nitride, aluminum
carbide, aluminum oxide and powder metallic aluminum) will be tested to evaluate the interactions
of pure aluminum compounds upon liquid addition under the same experimental conditions. The
evaluation will follow the same steps outlined earlier for SAP waste samples.
3.4.4 Hydrogen production from metallic aluminum — mechanism study
A pre-test study of reference materials indicated that the hydrolysis process of aluminum nitride
(A1N) can significantly enhance the reaction of metallic aluminum with water, even at room
temperature conditions. It was found that the rate of hydrogen generation can be quite high, e.g.
300 ml H2/min/0.5 g Al at 37C. The promotion effect of the product of A1N hydrolysis on the
rate of hydrogen generation from the reaction of metallic aluminum as well as the interaction of
salt will provide some insight for understanding the mechanisms of the reaction of SAP waste
with water. It is known that the product of A1N hydrolysis is related to time, the relation of
aging process and its promotion effect will be studied on the generated gas volume, composition
and rate.
• Experiment 1 (aging process of AIN hydrolysis): The product of AIN hydrolysis is changeable with
the aging process, different species of aluminum hydroxide or oxide might be formed. The pH in
the suspension will be monitor. The hydrogen generation from the reaction of metallic aluminum
with water will be studied with the different aged byproduct of AIN hydrolysis. The suspension of
AIN will be made as 1 g AIN with 20 ml Dl water in a closed container (e.g. 40 ml VOA vial with
screw cap). The aging time will be from less than 2 h , 24h, 72h, ... till 15 week. Adding aged AIN
suspension into the reactivity test apparatus (e.g. 60 ml VOA vial with screw cap) with metallic
aluminum, monitor the volume of gas generated using a gas syringe, and count the time. The pH
of the product generated from the aluminum reaction will be monitor after gas collection. The
experiment will be studied at the room temperature (25°C).
• Experiment 2 (the effect of mass of product of hydrolysis AIN): The amount of metallic aluminum
and the total volume of water will be fixed, the initial mass of AIN will be 0.5,1 and 2.0 gm (20 ml).
Adding aged AIN suspension into the reactivity test apparatus (e.g. 60 ml VOA vial with screw cap)
with metallic aluminum, monitor the volume of gas generated using a gas syringe, and count the
time. The reaction process will be repeated if the promotion effect is observed.
• Experiment 3 (the effect of mass of metallic aluminum): The amount of suspension of AIN and
total volume of solution will be fixed, the initial metallic aluminum mass will be 0.1, 0.5 and 1.0
gm. Adding aged AIN suspension into the reactivity test apparatus (e.g. 60 ml VOA vial with screw
cap) with metallic aluminum, monitor the volume of gas generated using a gas syringe, and count
the time. The reaction process will be repeated if the promotion effect is observed.
3.5. Toxicity Characteristic Leaching Procedure (TCLP) of SAP Waste
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The toxicity characteristic leaching procedure (TCLP) will be conducted on SAP waste to
determine if the SAP waste is characteristically hazardous. The TCLP will be performed according
to the EPA method 1311. The following minor modification to the test will be applied: 1) 10 g
SAP waste sample will be used instead of 100 g sample but the liquid to solid ratio will be 20:1 as
per the standard procedure, and 2) Whatman 0.45 |j,m PVDF filters will be used instead of the
0.7 |j,m glass fiber filters mentioned in the standard procedure. Other than those two modifications,
all other steps will be conducted according to the TCLP standard procedure.
3.6 Model Thermal Changes in Landfills Accepting SAP waste
3.6.1 Model Selection
The selected model will be used to estimate thermal changes in MSW landfills accepting SAP waste. The
model will not be used to make definitive conclusions, rather it will be used to provide information about
the trends that are likely to occur.
3.6.2 Model Attributes/Capabilities
To simulate the thermal changes in MSW landfills as a result of co-disposal of SAP waste with MSW, the
selected model must be able to run on an Intel Pentium Dual-Core processor and have the following
capabilities:
• Analyze steady-state and transient energy flow, 2-D energy flow in a cross section of in plan view
• Include boundary condition types such as temperature, flux, convective surfaces and imported
climate data.
3.6.3 Model to be Used
TEMP/W is a finite element CAD software product for analyzing thermal changes in the ground due to
environmental factors or the construction of facilities such as buildings or pipelines. The comprehensive
formulation makes it possible to analyze both simple and highly complex geothermal problems. TEMP/W
can be applied to the geothermal analysis and design of geotechnical, civil, landfill, and mining engineering
projects, including facilities subjected to freezing and thawing temperature changes. It was selected as the
model to be used for simulating thermal changes in MSW landfills as a result of co-disposal of SAP waste
with MSW.
A SOP for the TEMP/W is provided in Appendix A (see SOP 13).
3.6.4 Requirements, Parameters, and Assumptions
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The requirements needed for application of the selected model include information for input parameters
using characterization tests, literature, and other references.
The parameters involved TEMP/W Software include the thermal properties of the waste materials
(solid waste and SAP waste), liners and final covers in addition to the boundary conditions (e.g.,
climate, subgrade temperature, biological activity and chemical reactions of SAP with liquid).
These input parameters are classified to three types:
• Type 1: data for parameters that is generated in our laboratory under this approved QAPP
which means it is not secondary data.
• Type 2: data for parameters to be collected from peer-reviewed articles, text books and
interviews with regulators and facility owners/operators (secondary data).
• Type 3: data for parameters that is being assumed by the research team because there is lack
of information in the literature regarding those parameters.
For type 2 (secondary data): since textbooks and peer-reviewed articles have been through a rigorous
review process, it may be a valid if we assumed that the data are accurate. However, the research team
will take two actions to make sure the secondary data are accurate: 1) Try to identify more than one
source for the each input parameter and approve the value of the required parameter if 2 sources or more
agree on the value/range for that parameter, 2) contact experts in the field and get their opinion on that
obtained values for each parameters.
For type 3 data: the research team will conduct sensitivity analysis on the assumed parameters and if the
parameter prove to impact the results significantly then the team will try to find a justifiable value for the
parameter by further deep literature search or by contacting experts in the filed to get their
recommendations for the more realistic values for the required parameter. In the event there is still no
consensus on the value of the parameter, the model will be run based on 2-3 different scenarios for that
particular parameter (e.g., a low, medium and high value), and results from all three scenarios will be
presented.
• Assumptions and Explanations
o Only the parameters that have a large impact on the thermal changes over time in the
MSW landfills will be included as input into the model.
o MSW landfill cell that accepts 1000 tons per year of MSW over 2 years period of time.
o Two scenarios of disposing of SAP waste in MSW landfills will be assumed 1) the SAP
waste is being discharged at a dedicated spot within the landfill cell, and 2) the SAP waste
is being mixed with the MSW.
o The proportion of SAP waste to MSW will be varied in order to test different disposal
scenarios of SAP waste.
o The total heat generation from SAP waste (obtained from the experimental work) will be
converted to heat generation rates by assuming three possible scenarios: 1) the heat will
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be generated over a period of 1 month, 2) heat will be generated over a period of 1 year,
and 3) the heat will be generated over a period of 10 year.
3.6.5 Quality of the Model Output
The TEMP/W model does not generate any QC outputs. Nonetheless, in order to ensure the quality of the
model output, accuracy and precision will be checked as follows:
• The accuracy of the model output will be verified by using the TEMPW/W model to calculate the
thermal changes of a standard material. For example, the thermal changes of water as a result of
applying different ambient temperatures as boundary conditions will be tested using the TEMP/W
model. The output results will be compared to results from the literature.
• The output of model will be verified by another independent research laboratory with the
same input parameters and boundary conditions.
• The output of model is a report or paper or presentation related to the managment of
secondary aluminum dross.
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SECTION 4.0
SAMPLING PROCEDURES
4.1 Site Preparation
The main facilities that generate SAP wastes will be identified in collaboration with the Aluminum
Association and the Environmental Research and Education Foundation. The SAP waste samples
will be collected monthly from various secondary aluminum processing facilities. The selected
facilities have been identified by the Aluminum Association to cover a wide range of SAP
processes.
4.2 Sampling Procedures
In order to achieve a representative sampling of SAP wastes, double samples (BHD and SC) will
be taken from the facility directly. The SAP waste will be piled at the generation site per waste
type . After cooling (usually 72-120 hrs), each pile would be reduced following ASTM Method
C702 - 98 (2003) "standard practice for reducing samples of aggregate to testing size". Two
samples will be collected with pre-cleaned sampling equipment.
4.3 Sample Containers/Quantities
The first sample will be approximately 400 to 800 g sample collected in a tightly coved plastic
container that will be delivered to the EPA CHL Facility within 24 hours in a shipping container.
The second sample (10-20 kg) will be stored unpreserved in a tightly covered plastic container at
the test site or the sampling company (not at CHL facility) for further analysis, based on findings.
4.4 Sample Processing/Holding Times
Within two weeks of receipt, in order to obtain representative subsamples, the individual samples
will be processed as follows:
• The samples will be placed in a stainless steel pan and crushed to pass a 9-mm sieve.
• After thorough mixing, approximately 0.5 kg of the 9-mm sieved materials will be further size
reduced down to a size of 2 mm using a grinding machine (Preiser Scientific).
• Approximately 50 gm of the 2 mm size SAP waste will be further reduced to a size of 0.05 mm using
a sealed stainless steel jar mill equipped with zirconia grinding beads. The jar mill will be rotated at
20 rpm for 24 hours.
• The 2- mm size will be used for the chemical and physical analysis (pH, conductivity, moisture
content and water holding capacity) in the laboratory and the 0.05-mm size will be used for the
chemical and XRD analysis.
4.5 Sample Identification
The sample label should include the following:
1. Waste type (salt cake (SC) or baghouse dust (BHD))
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2. Sampling location (Each facility will be identified using a letter of the alphabet)
3. Sampling ID (4 digit)
An example label will be BHD-A-2452 meaning that the sample 2452 is a baghouse dust sample
collected from facility A.
Each generated sample will have a unique ID that describes and differentiates each sample. All
vials will also be labeled following the procedure explained above. Labels for samples to be
processed will contain the sample matrix (leachate or solid), sample port number or location, date
and time of sampling, the test (e.g., metals, NHs) that will be performed on this sample. A
laboratory notebook will be used to record the results of the analysis.
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SECTION 5.0
MEASUREMENT PROCEDURES
The following laboratory protocols will be carried out to achieve the research objectives as
required by the Aluminum Association and the Environmental Research and Education
Foundation.
5.1 SAP Waste Characterization
The experimental plan involves the determination of the total metal composition and mineral
phases for the SAP waste. Additionally, the moisture content, density and water holding capacity
will be measured for all SAP waste samples. The quantity of samples to be tested as well as the
frequency of sampling are summarized in Table 5.1. The samples containers specifications, the
preservation methods and holding times are presented in Table 5.2.
Table 5.1 Summary of Solid Sampling and Schedule
Parameter
Moisture
Water capacity
Metals
Mineral
Type of
measurement
Critical
Non-Critical
Critical
Non-Critical
Frequency
Once
Once
Once
Once
Total # of
samples
100
100
50
50
Table 5.2 Sample Containers, Preservation and Storage Time
Parameter
Amount of
sample
Vial type and
volume
Preservation
Max. holding
time
Matrix: Solid
Moisture
Metals
Mineral
10g
o.i g
2g
50 ml plastic vial
50 ml plastic vial
50 ml plastic vial
NA
HNO3,
refrigerate
NA
NA
6 months
NA
Matrix: Aqueous
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pH
Conductivity
Dissolved Metals
Anions (SO42~, Fs", and
cr)
Dissolved NEb
NA
NA
20ml
25ml
5ml
50 ml plastic vial
50 ml plastic vial
50 ml plastic vial
Plastic/Glass
50 ml EPA glass
vial
NA
NA
HNO3,
refrigerate
Cool @ 4 °C
H2S04,
refrigerate
<3h
<3h
6 months
28 days
7 days
Matrix: Gas
Composition and
concentration
20ml
Plastic/Glass
N/A
<3 hours
5.2. Experimental Sampling
The total number of samples and the sampling frequency for the gas and leachate generated from
the SAP waste reactivity testing presented in Section 3.4 are summarized in Table 5.3.
Table 5.3 Summary of Sampling of the Waste Reactivity Testing
Parameter
Temperature
Heat
Gas volume, ml
Gas Composition, %
(CH4, C02, H2, 02, N2)
N2O Concentration, ppm
NH3 (Gas)concentration,
Dissolved metal, mg kg"1
Dissolved ammonia, mg
kg1
TCLP metals (Ag, As, Ba,
Cr, Cd, Se, and Pb),mg kg'1
pH
EC
Type of
measurement
Critical
Critical
Critical
Critical
Non-Critical
Critical
Critical
Critical
Critical
Critical
Non-Critical
Frequency
Continuously
Continuously
Once
Once
Once
Once
Once
Once
Once
Once
Once
Total # of
samples
200
80
50
50
50
50
50
50
50
50
50
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5.3 Measurement Methods
The analytical methods for the SAP waste reactivity testing are outlined in Table 5.4. It is noted
that the temperature measurements will be recorded automatically and the results will be logged
directly to a 34970 Agilent data logger system. The recorded data can then be exported to
Microsoft Excel spreadsheets from the Agilent software program.
Table 5.4 Outline of Analysis Methods
Parameter
Measurement
Instrument
Analytical
Method/SOP
Leachate
pH
Conductivity
Ammonia (NfU in
solution)
Dissolved Metals
TCLP metals (Ag, As, Ba,
Cr, Cd, Se, and Pb)
Dissolved Anions
Critical
Non-Critical
Non-Critical
Critical
Critical
Non-Critical
Automatic Temperature and
Compensation electrode
Electrodless Toroidal
Conductivity Sensor
Orion 4-Star pH/ISE
Benchtop Meter
Thermo Elemental 61 E trace
analyzer ICP-AES
Thermo Elemental 6 1 E trace
analyzer ICP-AES
Ion Chromatograph (1C), using
AS- 18 Dionex chromatography
column.
I.M./EPA Method
150.1pH/SOP3
I.M./EPA Method
120. I/SOP 3
I.M., EPA method 350.3
Nitrogen-Ammonia /
SOP 7
SW-846 Method 601 OB
/SOP 9
SW-846 Method 6010B
/SOP 9
EPA Method 300 / SOP
#10
Solids
Temperature
Heat
Moisture
Density
Water Holding
Capacity
Total Metals
Crystallinity (XRD)
Critical
Critical
Critical
Non-Critical
Non-Critical
Critical
Non-Critical
Type T Thermocouple.
Type T Thermocouple.
4 digit balance and 105°C
oven
2 digit balance and 20.0 ml
cylinder
2 digit balance and 50 ml
cylinder
IRIS Intrepid ICP-AES
Philips instruments
X'Pert-MPD system
N.A./I.M.
N.A./I.M
SOP 4
SOPS
SOP 6
Method 3 051 for acid
digestion and Method
6010BforICP
analysis, SOP 8, and
SOP 9
N.A./I.M.
SOP 10
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X-ray Diffraction
Spectrometer
Gas
Gas volume
Gas Composition (CO2,
H2, O2, N2, CH4)
Gas Composition, N2O
Gas Composition, NHs
H2S
Critical
Critical
Non-Critical
Critical
Non-Critical
Gas Syringe
Gas Chromatograph (GC/TCD)
Agilent 6890 N Series
Gas Chromatograph (GC/ECD)
Agilent 6890 N Series
Orion 4-Star pH/ISE
Benchtop Meter
Jerome 63 IX Hydrogen Sulfide
Meter
N.A./I.M./EPA
method OPPTS
835.3400
SOP1
SOP 2
EPA method 350.3
Nitrogen-
Ammonia/SOP 7
I.M.
N.A: Not applicable
I.M: Instrument Manual
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SECTION 6.0
Quality Metrics (QA/QC CHECKS)
6.1 Data Quality Objectives and Criteria
The accuracy checks, precision, calibration of instrumentation, and the determination of detection
limits are used to ensure the quality control and the confidence level of the obtained results.
Precise, documented and valid data are needed for the ultimate decisions to be made. To ensure the
quality of the data, all instrumentation will be regularly calibrated. QA/QC checks will be done to
ensure the precision and accuracy of the data. Table 6.1 summarizes the QA/QC checks for each
monitoring parameter.
6.1.1 Definitions
Accuracy is the nearness of a test result to the true value (recovery). Both, standard addition
(spiking) and standard checks are common techniques for checking the accuracy. For matrix
spikes, the percent recovery could be calculated as follows:
Ca
Where: Cs = Concentration in spiked aliquot
Cu = Concentration in unspiked aliquot
Ca = Actual concentration of spike added
For standard checks, the percent recovery will be calculated as follows:
%^ = ^xlOO
Ca
Where: Cm = measured concentration of the check standard.
Ca = actual concentration of the check standard.
Precision is how repeated measurements closely agree with each other. Laboratory duplicates and
triplicates will be used to ensure precision; the relative percent difference (RPD) between
duplicates will be calculated as follows:
|C1 - C2|
%RPD = — — x 100
0.5(C1 + C2)
Where: Ci = Concentration of the analyte in the sample
C2 = Concentration of the analyte in the matrix duplicate
The relative standard deviation between replicates will be calculated as follows:
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%RSD = (—)xlOO
/
Where: S = Standard deviation
y' = Mean of the replicates
Method Detection Limit (MDL) is the lowest concentration that is different from zero with a 99%
level of confidence. To determine the MDL, the lowest standard concentration used for the
calibration will be injected number of times and the MDL will be calculated using the following
equation:
MDL = t(n-l, l-a = 0.99)xS
Where: n = the number of replicates
S = Standard deviation of the replicates
The MDLs for ICP-AES analysis performed at the EPA CHL Facility is provided in Table 6.2.
Table 6.1 Summary of QA/QC Checks
Parameter
pH
Conductivity
Ammonia
(NH4)
QC Check
Initial
Calibration*
Initial
Calibration*
Initial
calibration
Continuing
calibration
Precision
Blank
Accuracy
Method
2 point
calibration
1 point
calibration
4 point
calibration
Run mid
point
standard
Sample
duplicate
Laboratory
blank
Matrix
Spike
Frequency
At the
beginning
At the
beginning
As needed
Every 12
samples
Every 6 samples
Every 6 samples
Every 6 samples
Acceptance
Criteria
Within ±0.1 pHunit
of the correct value
Within ±2% of the
full range of the probe
R2 > 0.995
±20% of the actual
concentration
< 20% RPD
< Reported detection
limit
100 ±20% recovery
Corrective Action
1. Re-calibrate
1. Re-calibrate
1. Re-calibrate
1. Re-calibrate
1 . Re do triplicate
2. Investigate the
problem
1. Investigate
problem
2. Remove
contamination
3 . Check other
blanks
1 . Re-run spike
2. Check
calculations
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Metals
Anions (S042-
, F- and Q-)
Calibration
Precision
Blank
Accuracy
Calibration
Precision
Blank
Accuracy
4 point
calibration
Sample
Duplicate
Laboratory
blank
Check
Standard
4 point
calibration
Sample
duplicate
Laboratory
blank
Check
Standard
Before each run
Every 12
samples
Every 12
samples
Every 12
samples
As needed
Every 6 samples
Every 10
samples
Following
calibration and
every 10
samples
R2 > 0.995
< 15 %RPD for macro
elements (Al, Fe, Ca,
K, Na, S and Mg) and
< 25% for trace metals
(Ag, Ba, Cu, Mn, Zn
,Cd, As, Se, Cr and
Pb).
< Reported detection
limit
100 ±15% recovery
for major metals and
100 ±25% for trace
metals
R2 > 0.995
< 20% RPD
< Reported detection
limit
100 ±15% recovery
3. Re-run samples as
required
1. Re-calibrate
1. Re-analyze
2. Investigate the
problem
1. Investigate
problem
2. Remove
contamination
3 . Check other
blanks
1. Re-calibrate
2- Re-run samples
as required
1. Re-calibrate
1 . Re do triplicate
2. Investigate the
problem
1. Investigate
problem
2. Remove
contamination
3 . Check other
blanks
1. Re-run
2. Check
calculations
3. Re-run samples as
required
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Temperature
Heat
measurement
Moisture
Content
Density
Water
holding
capacity
Total metal
Crystallinity
(XRD)
Gas volume
Gas
Composition
*
Initial
Calibration*
Initial
Calibration*
Initial
Calibration*
Initial
Calibration*
Initial
Calibration*
Calibration
Precision
Accuracy
Calibration
Initial
Calibration*
Initial
Calibration
Precision
Accuracy
1 point
calibration
1 point
calibration
1 point
calibration
1 point
calibration
1 point
calibration
5 point
calibration
Sample
duplicate
Standard
check
Reference
standard
1 point
calibration
6 point
calibration
Sample
Duplicate
Standard
Check
At the
beginning, and
once a year
Every 6 month
At the
beginning
At the
beginning
At the
beginning
Before each run
Every 12
samples
With every run
Prior to sample
analysis
At the
beginning
Monthly
Every 12
samples
Twice a Week
Within±2%ofthe
full range of the probe
Within ±15%
Within±5%ofthe
full range of the probe
Within±5%ofthe
full range of the probe
Within±5%ofthe
full range of the probe
R2 > 0.99
< 25% RPD
75-125 % recovery
Within±5%ofthe
full range of the probe
R2 > 0.990
< 20% RPD
100 ±20% recovery
1. Use new
thermocouple (
within 1 year)
1. Re-do sample
2. Investigate the
problem- Flag data
1. Re-calibrate
1. Re-calibrate
1. Re-calibrate
1. Re-calibrate
1. Rerun
2. Prepare new
standards
2. Check
calculations
Re calibration
1. Re-calibrate
1. Re-calibrate
1. Re-do sample
2. Investigate the
problem- Flag data
1. Re-calibrate
* Calibration for the probes, electrodes, thermocouples and TDR.
* Calibration of the Gerome meter (for EhS) is performed annually by the manufacturer. Calibration
verification samples will be analyzed prior to each analysis using a known hydrogen sulfide standard
and must be within ± 20 % of the standard value. If the calibration verification sample exceeds the set
criteria, the meter will be sent to the manufacturer for NIST-traceable calibration.
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6.2 Types of QC Samples
Method Blank is a generated sample prepared from a clean matrix (generally deionized water and
it could be gas or solid according to the type of matrix), and it is treated exactly as a sample. It is
prepared to check for contamination.
Calibration Blank is a volume of reagent water without the analyze. The concentration of the
analyze should be less than three times the instrument detection limit
Matrix Spike is a sample with a known concentration of the analyze added to original sample and
is used to assure that the recovery of the target compounds is acceptable for the matrix involved.
Standard Check is a sample with a known concentration of the analyze is used to assure that the
recovery of the target compounds is acceptable for the matrix involved.
Table 6.2 MDL and Accuracy for ICP-AES Method
Metal
Name
Al
Ag
Ba
As
Ca
Cd
Cr
Cu
Fe
K
Mg
Mn
Na
P
Pb
S
Se
Zn
True
Value
(jig/ml)
0.040
0.010
0.020
0.050
0.100
0.020
0.050
0.020
0.040
0.100
0.100
0.008
0.100
0.100
0.050
0.050
0.050
0.008
Mean
Concentration
(jig/ml)
0.031
0.011
0.020
0.055
0.074
0.023
0.053
0.020
0.045
0.134
0.073
0.007
0.111
0.144
0.053
0.046
0.052
0.008
Accuracy
(%)
79%
108%
100%
110%
74%
113%
106%
98%
111%
134%
73%
93%
111%
144%
106%
93%
104%
94%
STDEV
(US/ml)
0.001
0.000
0.001
0.001
0.015
0.0002
0.0004
0.001
0.001
0.039
0.001
0.000
0.009
0.038
0.002
0.005
0.001
0.000
MDL
(US/ml)
0.004
0.001
0.002
0.004
0.048
0.001
0.001
0.004
0.002
0.123
0.004
0.001
0.027
0.119
0.005
0.015
0.003
0.000
MRL
(Hg/ml)
0.013
0.003
0.007
0.011
0.154
0.002
0.004
0.011
0.008
0.390
0.012
0.002
0.087
0.379
0.015
0.049
0.010
0.001
fThe results of As, Cd, Cr, Pb
based on the results of Nov,
and Se are based on the results of July, 2012 and the others are
2011.
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6.3 Model Calibration and Validation
Many authors have shown TEMP/W to be accurate at simulating thermal changes of various
problems as a result of changes in boundary conditions. The software has been successfully used
for many applications such as thermal design of roads and airstrips, ground freezing for soil
stabilization, insulation design for shallow buried piping, thawing or freezing beneath heated or
chilled structures, convective cooling of surfaces and many geotechnical applications (Thermal
Modeling with TEMP/W, 2007). Although the parameters and problem setup may vary from any
one specific study, the conclusion holds true that TEMP/W is a reliable program. For details of the
modeling procedure please see SOP 13.
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SECTION 7.0
DATA ANALYSIS, INTERPRETATION, AND MANAGEMENT
7.1 Data Reporting
Table 7.1 summarizes the reporting units for the various analyses. At the end, each monitoring
parameter will be averaged on treatment scale and analysis of variance will be carried out to
determine the effect of SAP on temperature and gas emission under different experimental
conditions.
Temperature will be recorded by the data logger system and transferred into Microsoft Excel ™
spreadsheets. The remaining analysis results will be recorded in a laboratory notebook and each page
will be dated and signed by the person who performs the analysis, then, those data will be fed manually
to Excel spreadsheets for statistical analysis. Calculations will be carried out on a computer and will
be checked initially by the analyst for gross error and miscalculation. The calculations and data
entered into computer spreadsheets will be checked by a second analyst for accuracy by printing
out the calculation or data spreadsheet and checking the calculation by hand or checking each entry
of data from the original. These copied spreadsheets will be initialed and dated by the second
analyst doing the checking, noting the errors.
Table 7.1 Reporting Units
Parameter
pH
Conductivity
Ammonia (NHs, Gas)
Metals
Anions
Crystallinity (XRD analysis)
Temperature
Moisture Content
Heat
Water holding capacity
Gas volume
Gas Composition
Unit
pH Units
uS/cm
ppmv
mg/L
mg/L
—
°C
%M/M
kJ/g
g/g
L or ml
% V/V or ppm
Statistical analysis and graphical representation of the data will be performed using Microsoft
Excel 2007, Software JMP9.0 and SigmaPlotl 1.0. The mean, standard error, minimum and
maximum values will be used to summarize the elemental composition, mineral phases, and the
temperature change as well as the gas composition, and productivity. For the correlations between
the temperature change and mineral phases, or relation between heavy metal content and
aluminum content, the Pearson product-moment correlation and Spearman's rank correlation will
be employed to calculate the p level. The Pearson product-moment correlation coefficient is a
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measure of the correlation (linear dependence) between two variables X and Y, giving a value
between +1 and -1 inclusive. Spearman's rank correlation coefficient is a non-parametric measure
of statistical dependence between two variables. It assesses how well the relationship between two
variables can be described using a monotonic function. If there are no repeated data values, a
perfect Spearman correlation of+1 or -1 occurs when each of the variables is a perfect monotone
function of the other. If p<0.05, it is assumed that the relation is significant; and if p<0.01, the
correlation is very significant. If p>0.05, it is believed that there is no correlation.
7.2 Data Handling and Disposal
Original project records that are generated by PTSI will be maintained by the WA Leader in
accordance with the ORD Policies and Procedures Manual, Section 13.2 Paper Laboratory
Records.
7.3 Data Reduction and Validation
Data reduction and validation will be done using Microsoft Excel spreadsheets to minimize the
calculation errors. A second reviewer will check the reduced data. The reviewed data will include
calibration and QC data. The reviewer will also review the laboratory notebooks on a monthly
basis. Any detected errors will be corrected before the data is released to the EPA.
7.4 Data Storage
Laboratory records will be maintained in accordance with Section 13.2, Paper Laboratory Records,
of the Office of Research and Development (ORD) Policies and Procedures Manual. Controlled
access facilities that provide a suitable environment to minimize deterioration, tampering, damage,
and loss will be used for the storage of records. Whenever possible, electronic records will be
maintained on a secure network server that is backed up on a routine basis. Electronic records that
are not maintained on a secure network server will be periodically backed up to a secure second
source storage media, transferred to an archive media (e.g., compact discs, optical discs, magnetic
tape, or equivalent), or printed. Electronic records that are to be transferred for retention will be
transferred to an archive media or printed, as directed by EPA.
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SECTION 8.0
REPORTING
8.1 Project Deliverables
Monthly reports will be prepared by the PTSI WA Leader and sent to the PTSI On-site Technical
Manager and Project Manager, and submitted to EPA on the 20th of every month. Every ten
months an interim report will be prepared to cover all aspects of the project such as the work
progress, a summary and discussion of the results, any problems encountered, the adopted solution
to the problem and any deviations from the procedures described in the QAPP.
8.2 Final Report
The final report will be prepared at the end of the project to summarize all the project aspects, give
the final results, the conclusions and the recommendations. The reports will be submitted in both
hard and electronic copies. All the reports will be submitted to the EPA Project Officer through the
EPA Work Assignment Manager.
8.3 Draft Manuscript
The produced final report will be the basis for draft manuscripts that will be produced by Dr.
Xiaolan Huang and the project personnel as directed by the EPA WA Manager.
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SECTION 9.0
REFERENCES
Bruckard, W.J., and Woodcock, J.T. (2007) Characterisation and treatment of Australian salt cakes by
aqueous leaching. Minerals Engineering 20, 1376-1390.
Chambino, T., et al. (2008) Aluminium Salts Hydrolysis Products from Industrial Anodising Sludges in
Wastewater Treatment. In Colloids for Nano- and Biotechnology, 65-69.
Davies, M., et al. (2008) Treatment of salt cakes by aqueous leaching and Bayer-type digestion.
Minerals Engineering 21, 605-612.
European-Commission, COMMISSION DECISION of 3 May 2000 replacing Decision 94/3/EC
establishing a list of wastes pursuant to Article l(a) of Council Directive 75/442/EEC on waste and
Council Decision 94/904/EC establishing a list of hazardous waste pursuant to Article 1(4) of
Council Directive 91/689/EEC on hazardous waste. InL226/3, European-Commission, Ed.
Official Journal of the European Communities, 2000; p 22.
Gil, A. (2007) Management of Salt Cake Generated at Secondary Aluminum Melting Plants by
Disposal in a Controlled Landfill: Characteristics of the Controlled Landfill and a Study of
Environmental Impacts. Environmental Engineering Science 24, 1234.
Hind, A.R., et al. (1999) The surface chemistry of Bayer process solids: a review. Colloids and
Surfaces A: Physicochemical and Engineering Aspects 146, 359-374.
Hiraki, T., et al. (2007) Process for Recycling Waste Aluminum with Generation of High-Pressure
Hydrogen. Environmental Science & Technology 41, 4454-4457.
IAI Global Aluminium Recycling: A Cornerstone of Sustainable Development; International
Aluminium Institute: 2009.
Kashcheev, I, et al. (2008) Secondary Aluminum Production Waste — A Raw Material for the
Refractory Industry. Refractories and Industrial Ceramics 49, 167-170
Lopez-Delgado, A., H. Tayibi and F. Lopez (2007) Treatments of Aluminum Dust-A Hazardous
Residue From Secondary Aluminum Industry. In Focus on Hazardous Materials Research (Mason,
E.G., ed), 1-52, Nova Science Publishers, Inc.
Manfredi, O., et al. (1997) Characterizing the physical and chemical properties of aluminum dross.
JOM Journal of the Minerals, Metals and Materials Society 49, 48-51.
Peterson, R. D.; Newton, L., Review of aluminum dross processing. Light Metals 2002, 1029-
1037.
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SINTEF In Roadmap from Europe and North America Workshop on Aluminum Recycling,
Roadmap from Europe and North America Workshop on Aluminum Recycling, Tronheim,
Norway, 2010; SINTEF, The Research Council of Norway, NTNU: Tronheim, Norway, 2010; p
28.
Schlesinger, M. E., Aluminum Recycling. CRC Press: Boca Raton, FL, 2007.
Thermal Modeling with TEMP/W 2007, An Engineering Methodology, Third Edition, March
2008, GEO-SLOPE International Ltd.
USDOE Recycling of aluminum dross/salt cake; Office of industrial technologies,Energy
Efficiency and Renewable Energy, U.S. Department of Energy: 1999; p 2.
Yoshimura, H.N., et al. (2008) Evaluation of aluminum dross waste as raw material for refractories.
Ceramics International 34, 581-591
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SOP1
SOP for Major Gas Analysis using Gas Chromatography (GC)
Refer SOP: LRPCD SOP M 02.0
NRMRL LRPCD M 02 0 GC Headspace Analysis for Bioreactor Landfill Gas.pdf
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SOP 2
SOP for N2O Gas Analysis using Gas Chromatography (GC-ECD)
Refer SOP: LRPCD SOP M 09.0
NRMRL LRPCD M 09 OAnalysisofNitrousOxideHeadspaceSamplesbvGC-ECD.pdf
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SOPS
PH/Conductivity measurement using the Accumet® Portable AP85 Waterproof Meter
Scope
This procedure is used to measure the pH and EC for samples generated during the different tests (
EPA methods 150.1 and 120.1).
Apparatus
pH and Conductivity meter, Accumet® Portable AP85 Waterproof Meter or equivalent
- pH electrode, Conductivity probe
- Disposable plastic container, 75 ml or larger
Reagents and materials
- Standard buffer, pH 4.01
- Standard buffer, pH 7.00
- Standard buffer, pH 10.01
Conductivity Standard Solution
Deionized water (DI)
Procedure
1. pH Calibration
It is recommend that calibration be done at least two buffers that bracket (one above and one below) the
expected sample range.
1.1. Preparing for pH calibration
This meter can calibrate up to 5 pH buffer values to ensure accuracy across the entire
pH range. Selection is made from the following buffer options:
USA: pH 1.68, 4.01, 7.00, 10.00, 12.45
NIST: pH 1.68, 4.01, 6.86, 9.18, 12.45
The meter automatically recognizes these standard buffer values, which makes pH calibration faster and
easier.
The protective electrode storage bottle or rubber cap of the probe is removed before calibration or
measurement. If the electrode has been stored dry, the probe is re-hydrated in tap water for 10 minutes
before use to saturate the pH electrode surface and minimize drift. The probe in rinsed with deionized
water after use, and stored in electrode storage solution. If storage solution is not available, pH 4.0 or 7.0
buffer is used.
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1.2. To calibrate for pH
1. If necessary, the MODE key is pressed to select pH measurement mode. The pH indicator
appears in the upper right hand corner of the display.
1.38
2. The pH electrode is rinsed thoroughly with deionized water or a rinse solution. Wiping the probe
is not advisable; this causes a build-up of electrostatic charge on the glass surface.
3. The pH electrode is dipped into the calibration buffer. The end of the probe must be completely
immersed into the sample. The probe is gently stirred to create a homogeneous sample.
Notes: The temperature element is in the conductivity cell. For temperature compensated
readings, the conductivity cell is dipped into the calibration buffer as well.
4. CAL/MEAS is pressed to enter pH calibration mode. The CAL indicator lights up. The primary
display shows the measured reading while the smaller secondary display indicates the pH
standard buffer solution.
lm lm jam* jfiiH
138
i,uu ""
5. The measured pH value is allowed to stabilize. If the READY indicator has been activated the
READY annunciator lights when the reading is stable.
1. Press ENTER to confirm calibration. The meter is now calibrated to the current buffer. The lower
display scrolls through the remaining buffer options.
> White performing a multipoint calibration, step 7 is followed next.
> While performing a one-point calibration, step 9 is followed next.
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2. The electrode is rinsed with deionized water or a rinse solution, and dipped in the next pH buffer.
3. Steps 5 to 8 are followed for additional calibration points.
4. When calibration is complete, CAL/MEAS is pressed to return to pH measurement mode.
t,UU
Notes:
To exit from pH Calibration mode without confirming calibration, ENTER is not pressed in step 6.
Instead CAL/MEAS is pressed.
If the selected buffer value is not within ±1.0 pH from the measured pH value: the electrode and buffer
icon blink and the ERR annunciator appears in the lower left corner of the display.
2. Conductivity calibration
Up to 5 conductivity points can be calibrated, using a maximum of one point per range (listed
below):
Range Conductivity:
Rl 0.00-19.99 nS
R2 0.00-199.90 ^S
R3 0.00-1999.0 nS
R4 0.00-19.99 mS
R5 0.00-199.9 mS
> While measuring in more than one range, it is made sure to calibrate each of the ranges being
measured. All new calibration data will over-ride existing stored calibration data for each
measuring range calibrated.
> While measuring in ranges near to or greater than 20 mS (10 ppt), or near to or lower than 100
US (50 ppm), the meter is calibrated at least once a week to get specified ±1% full scale accuracy.
> While measuring in the mid ranges and the probe is rinsed in deionized water and stored dry.
The meter is calibrated at least once a month.
> While taking measurements at extreme temperatures, the meter is calibrated at least once a week.
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2.1. Preparing for conductivity/TDS calibration
For best results, a calibration standard value close to the sample value being measured is selected.
Alternatively, a calibration solution value is used that is approximately 2/3 the full scale value of the
measurement range planned to be used. For example, in the 0 to 1999 j^S conductivity range, a 1413 j^S
solution is used for calibration.
Normalization temperature: The factory default value for normalization temperature is 25°C.
2.2. To calibrate conductivity:
1. If necessary, the MODE key is pressed to select conductivity mode.
r
)
. /:«
2. The probe is rinsed thoroughly with deionized water or a rinse solution, then with a small
amount of calibration standard.
3. The probe is dipped into the calibration standard. The probe tip is immersed beyond the upper
steel band. The probe is stirred gently to create a homogeneous sample.
Leare pfcbe
guard en
during
measurement
Immerse
probe beyond
ipfer steel j-""*
k tend -^
|
;r
s*
I
¥
i
_
a
4. The measured conductivity is allowed value to stabilize. If the READY indicator has been
activated the READY annunciator lights up when the reading is stable.
5. CAL/MEAS is pressed to enter conductivity calibration mode. The CAL indicator will appear
above the display.
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1
T *"" *-CAL ""•
|«L»r O_/0S
_f l_ , 1
\ ^% t:n.
L__ ___J
6. A or Tis pressed to change the value on the primary display to match the value of the
calibration standard. The secondary display shows the factory calibrated value.
—
o in
IAJ
___J
7. The calibration is confirmed by pressing ENTER. The meter returns to the MEAS
(measurement) mode.
8. Steps 1-7 are repeated for other ranges.
Notes: When entering calibration mode, the meter will display the factory default value. If the
meter was previously calibrated, the display may
switching from measurement to calibration mode.
'jump" to the factory default value when
To exit from Conductivity Calibration mode without confirming calibration, CAL/MEAS is
pressed without pressing ENTER. This will retain the old calibration data in the measuring range
of the calibration. The conductivity reading can be offset up to ±40% from the default setting. If
the measured value differs by more than ±40%,
probe is cleaned or replaced as needed.
3. Taking pH Measurements
To take readings:
1. The pH electrode is rinsed with deionized or distilled water before use to remove any impurities
adhering to the probe body. If the pH electrode has dehydrated, it is soak 30 minutes in electrode
storage solution, pH buffer, or a 2M-4M KC1 solution.
2. Meter is switched on by pressing ON.
3. The MODE key is pressed to select pH measurement mode. The MEAS annunciator appears on
the top center of the LCD. The ATC indicator appears in the lower right hand corner to indicate
Automatic Temperature Compensation.
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i READY
_ _ _
1 1 | |
oo
c,o
NOTE: For pH manual temperature compensation, the conductivity cell must be disconnected
from the 6-pin connector. The ATC indicator will disappear from the display. A manual
temperature compensation value also needs to be set for this (although this function will not be
used.)
4. The pH electrode is dipped into the sample. Since the conductivity cell contains the temperature
sensor, it is also immersed in the solution. When dipping the probe into the sample, the sensor or
the glass bulb of the electrode must be completely immersed into the sample. The probe is stirred
gently in the sample to create a homogenous sample.
5. The reading is allowed to stabilize. The reading on the display is noted. If the Ready indicator is
selected on, it will appear when the reading is stable.
6. The MODE key is pressed to toggle between pH and conductivity readings.
4. Taking Conductivity Measurements
To take readings:
1. The probe is rinsed with deionized or distilled water before use to remove any impurities
adhering to the probe body and is dried by shaking in air. To avoid contamination or dilution of
the sample, the probe is rinsed with a small volume of the sample liquid.
2. Meter is switched on by pressing ON.
3. The MODE key is pressed to select conductivity (or TDS) measurement mode. The MEAS
annunciator appears on the top center of the LCD. The ATC indicator appears in the lower right
hand corner to indicate Automatic Temperature Compensation.
O 3 LJ
J (_ I '
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4. The probe is dipped into the sample. When dipping the probe into the sample, the tip of the
probe must be immersed above the second steel band. The probe is stirred gently in the sample
to create a homogenous sample.
during
Inimerw
probe bfrtind
upper •-!—I
hmd
5. The reading is allowed to stabilize. The reading on the display is noted. If the Ready indicator
is selected on, it will appear when the reading is stable.
5. References
APHA. 1992. Standard methods for the examination of water and wastewater. 18th ed. American Public
Health Association, Washington, DC.
Hach Company. 1992. Hach water analysis handbook. 2nd ed. Loveland, CO.
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SOP 4
Moisture Measurement
Scope
This procedure is used to measure the moisture content of the samples during the characterization
(ASTM Method D-2216).
Apparatus
Mettler Toledo Model AL54 Balance or equivalent
Aluminum weighing dish
Spatula
Blue M(105°C Oven)
Procedure
1.0 Balance Calibration
1.1 Calibrate the analytical balance as described in Use of Analytical Balance SOP
No.05.SOP.009.00 of LRPCD.
2.0 Sample Drying
2.1 Place the weighing dish on the balance and tare the balance.
2.2 Weigh out about lOg net weight of the sample into a drying dish using a clean spatula.
Record it as Wi.
2.3 Dry sample at 105°C for 48 hours.
2.4 Weigh and record dried sample weight in lab book.
2.5 Return sample to oven for 6 hours.
2.6 Reweigh and record dried sample weight in lab book.
2.7 If weight is unchanged < 1%, continue to Step 3.0.
2.8 If weight changed > 1%, return to Step 2.5 and repeat the following steps until a <1%
change is observed.
3.0 Weighing
3.1 Record the final weight of the dried sample as W2.
Analysis
The moisture content of the sample can be found out using the formula:
% Moisture Content = (Wi-W2)/Wi x 100
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SOPS
Bulk Density Measurement
Scope
Bulk density is defined as the weight per unit volume of material. This procedure is used to measure
the bulk density of the samples during the characterization (ASTM method for Saturated Hydraulic
Conductivity, Water Retention, Porosity and Bulk Density of Putting Green and Sports Turf Root
Zones, 2006).
Apparatus
Mettler Toledo Model AL54 Balance or equivalent
Graduated Cylinder or equivalent
Procedure
1.0 Balance Calibration
1.1 Calibrate the analytical balance as described in Use of Analytical Balance SOP
No.05.SOP.009.00 of LRPCD.
2.0 Fill the sample into a known volume Cylinder
2.1 Measure Volume of cylinder ( V, cm3)
2.2 Place the Cylinder on the balance and tare the balance.
2.2 Fill in the sample through a funnel which is suspended above
the cylinder, and the excess material on top of the
measuring cylinder is scraped off with a straight edge.
(Figure 1)
3.0 Weighing
3.1 Record the net weight of sample in the cylinder as W (g)
Analysis
The bulk density of the sample can be found out using the formula:
Bulk density (g cm'3) = W/V
Since the variation of bulk density is usually high, five replications are required.
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SOP 6
Water Holding Capacity Measurement
Scope
Water holding capacity is defined as the solid that hold generous amounts of water are less subject
to leaching. This procedure is used to measure the Water holding capacity of the samples during the
characterization (ASTM Method F1815-06).
Apparatus
Mettler Toledo Model AL54 Balance or equivalent
Graduated Cylinder or equivalent
Absorbent membrane or equivalent
Procedure
1.0 Balance Calibration
1.1 Calibrate the analytical balance as described in Use of Analytical Balance SOP
No.05.SOP.009.00 of LRPCD.
2.0 Fill around 10 g sample into Cylinder and add the water to make it saturated. Put the saturated
sample with the cylinder into the absorbent membrane until the excess water is drawn away by
gravity. Once equilibrium is reached, the water holding capacity is
calculated based on the weight of the water held in the sample vs. the
sample dry weight.
2.1 Weight the cylinder with a saturated filtered paper as the
bottom, Wo
2.2 Fill around 10 gram sample into the known weight cylinder,
weight the total weight, Wi,
2.3 Make the Cylinder with sample saturated and then placed it on
an absorbent membrane until the excess water is drawn away by
gravity (see diagram at right).
2.4 Once equilibrium is reached (usually overnight), weight the
cylinder with sample again (W2).
Ab&orbe
Analysis
The water holding capacity of the sample can be found out using the formula:
Water holding capacity (g g'1) = (W2-Wi)/(Wi-Wo)
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SOP 7
SOP for Ammonia Measurement by ISE
Scope and Application
This method is applicable to the measurement of 0.03 to 1400 mg NH3-N/L in solution, e.g.
surface waters and domestic and industrial wastes (EPA method 350.3). High concentrations of
dissolved ions affect the measurement, but color and turbidity do not. Sample distillation is
unnecessary.
Summary of Method
The ammonia-selective electrode uses a hydrophobic gas-permeable membrane to separate the
sample solution from an electrode internal solution of ammonium chloride. Dissolved ammonia
(NH3(aq) and NH4+) is converted to NH3(aq) by raising pH to above 11 with a strong base. NH3(aq)
diffuses through the membrane and changes the internal solution pH that is sensed by a pH
electrode. The fixed level of chloride in the internal solution is sensed by a chloride ion-selective
electrode that serves as the reference electrode. Potentiometric measurements are made with the
Orion 95-12 gas-sensing electrode on the Orion Star meter or a pH meter with expanded millivolt
scale capable of 0.1 mV resolution between -700 mV and +700 mV or a specific ion meter, which
will determined ammonia content in solution directly. The method requires no titration and has no
turbidity or color interferences.
Sample Handling and Preservation
Refrigerate at 4°C for samples to be analyzed within 24 h. Preserve samples high in organic and
nitrogenous matter, and any other samples for longer storage, by lowering pH to 2 or less with
cone H2SO4.
Interferences
The problems with ISE measurements are variable stabilization times, changes in the measured
potential during repeated analysis, and the effect of variable ionic strength of the solutions. These
problems can be minimized by frequent re-calibration.
Apparatus and Reagents
1. Apparatus
a. Electrometer: Orion Star meter or a pH meter with expanded millivolt scale
capable of 0.1 mV resolution between -700 mV and +700 mV or a specific ion
meter.
b. Ammonia-selective electrode: Ammonia electrode (Orion 9512HPBNWP)
c. Magnetic stirrer, thermally insulated, with TFE-coated stirring bar (Orion 096019).
2. Reagents
a. Deionized water: Use for making all reagents.
b. Sodium hydroxide, ION ( e.g. Orion 951011).
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c. Stock ammonium chloride solution: Ammonia standard, 100 ppm ammonia as N (
e.g. Orion 951207).
Procedure for Ammonia analysis
1. Preparation of standards: Prepare a series of standard solutions covering the
concentrations of 1000, 100, 10, 1, and 0.1 mg NH3-N/L by making decimal dilutions of
stock NH4C1 solution with water.
2. Electrometer calibration: Place 100 mL of each standard solution in a 150-mL beaker.
Immerse electrode in standard of lowest concentration and mix with a magnetic stirrer.
Limit stirring speed to minimize possible loss of ammonia from the solution. Maintain the
same stirring rate and a temperature of about 25°C throughout calibration and testing
procedures. Add a sufficient volume of lOTVNaOH solution (1 mL usually is sufficient) to
raise pH above 11. If it is necessary to add more than 1 mL of NaOH solution, note volume
used, because it is required for subsequent calculations. Keep electrode in solution until a
stable millivolt reading is obtained. Do not add NaOH solution before immersing electrode,
because ammonia may be lost from a basic solution. Repeat procedure with remaining
standards, proceeding from lowest to highest concentration. Wait until the reading has
stablized (at least 2 to 3 min) before recording millivolts for standards and samples
containing < 1 mg NH3-N/L.
3. Preparation of standard curve: Using semilogarithmic graph paper, plot ammonia
concentration in milligrams NH3-N per liter on the log axis vs. potential in millivolts on
thelinear axis starting with the lowest concentration at the bottom of the scale. If the
electrode is functioning properly a tenfold change of NH3-N concentration produces a
potential change of about 59 mV.
4. Measurement of samples: Dilute if necessary to bring NH3-N concentration to within
calibration curve range. Place 100 mL sample in 150-mL beaker and follow procedure in
4&above. Record volume of lOTVNaOH added. Read NH3-N concentration from standard
curve.
References
1. BANWART, W.L., J.M. BREMNER & M.A. TABATABAI. 1972. Determination of ammonium in
soil extracts and water samples by an ammonia electrode. Comm. Soil Sci. Plant Anal.
3:449.
2. MIDGLEY, C. & K. TERRANCE. 1972. The determination of ammonia in condensed steam and
boiler feed-water with a potentiometric ammonia probe. Analyst 97:626.
3. BOOTH, R.L. &R.F. THOMAS. 1973. Selective electrode determination of ammonia in water
and wastes. Environ. Sci. Technol. 7:523.
4. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1979. Methods for Chemical Analysis of
Water and Wastes. EPA-600/4-79-020, National Environmental Research Center,
Cincinnati, Ohio. AMERICAN SOCIETY FOR TESTING AND MATERIALS. 1979. Method 1426-
79. American Soc Testing & Materials, Philadelphia, Pa.
5. Method 4500-NH3 D, E. Standard Methods for the Examination of Water and Wastewater,
20th Edition, 1998. APHA, AWWA, & WEF, Washington, D.C.
www.standardmethods.org
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SOPS
Microwave Acid Digestion
Scope
This procedure is used to prepare ICP-AES metal analysis sample generated during the different
experiments (EPA SW846-3051A).
Summary of Method
A representative sample of up to 0.1 g is digested in 12 ml of mixed concentrated HCl-HNCb for
30 min (for solid samples) using microwave heating with a suitable laboratory microwave unit.
The sample and acid are placed in a fluorocarbon (PFA or TFM) microwave vessel. The vessel is
capped and heated in the microwave unit. After cooling, the vessel contents are filtered,
centrifuged, or allowed to settle and then diluted to volume and analyzed by the appropriate SW-
846 method. .
Apparatus
Microwave Accelerated Reaction System (MARS) with Teflon holders
Fluorocarbon (PFA or TFM) digestion vessels (120 mL capacity) capable of withstanding
pressures up to 7.5 ± 0.7 atm (110 ± 10 psig) and capable of controlled pressure relief at pressures
exceeding 7.5 ± 0.7 atm (110 ± 10 psig).
Reagents and Materials
Cone. HNO3
Cone. HC1
Deionized (DI) water
Pipetter, 10 ml capacity
Interferences
Very reactive or volatile materials that may create high pressures when heated may cause venting
of the vessels with potential loss of sample and analytes. The complete decomposition of either
carbonates, or carbon based samples, may cause enough pressure to vent the vessel if the sample
size is greater than 0.25 g when used in the 120 mL vessels with a pressure relief device that has an
upper limit of 7.5 ± 0.7 atm (110 ± 10 psi). This is required to retain the heat characteristics of the
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calibration procedure. Limits of quantitation will change with sample quantity (dilution) as with
instrumentation."
Sample Collection, Preservation, and Handling
All sample containers must be prewashed with detergents, acids, and water. Plastic containers are
preferable. See SOP 10, Step 3.1.3 of this manual, for further information. Aqueous waste waters
must be acidified to a pH of < 2 with HNCb.
Procedure
1. Weigh a well-mixed sample to the nearest 0.001 g into the fluorocarbon sample vessel
equipped with a single-ported cap and a pressure relief valve. For SAP sample, no more
than 0.10 g sample will be used. This sample is added into the digestion vessel with the
number of the vessel recorded on the preparation sheet.
2. A reference standard and a master control without sample are treated in the same manner
along with spikes and duplicates.
3. Add 3 ± 0.1 mL concentrated HC1 firstly, then 9± 0.1 mL concentrated HNOs to the vessel
in a fume hood. Check to make sure the pressure relief disks are in the caps with the
smooth side toward the sample and start the caps a few turns on the vessels.
4. Evenly distributed the vessels in the carousel according to the manufacturer's
recommended specifications. Blanks are treated as samples for the purpose of balancing the
power input. When fewer than the recommended numbers of samples are digested, the
remaining vessels should be filled with 0.1 g of reference standards and!2 mL of mixed
HCl-HNCb to achieve the full complement of vessels.
5. Program the microwave unit according to the manufacturer's recommended specifications
and, if used, connect the pressure vessels to the central overflow vessel with PFA-
fluorocarbon tubes. The chosen sequence will bring the samples to 185 deg C ± 5 deg C in
30 minutes and will hold at 185 deg C during the second 30 minutes. Start the turntable
motor and be sure the vent fan is running on high and the turntable is turning. Start the
microwave generator.
6. At the end of the microwave program, allow the vessels to cool for at least 5 minutes in the
unit before removal to avoid possible injury if a vessel vents immediately after microwave
heating. The samples may be cooled outside the unit by removing the carousel and
allowing the samples to cool on the bench or in a water bath. When the vessels have cooled
to room temperature, weigh and record the weight of each vessel assembly. If the weight of
the sample plus acid has decreased by more than 10% discard the sample.
7. Complete the preparation of the sample by carefully uncapping and venting each vessel in a
fume hood. Transfer the sample to an acid-cleaned bottle. If the digested sample contains
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parti culates which may clog nebulizers or interfere with injection of the sample into the
instrument, the sample may be filtered.
8. Filtering: The filtering apparatus must be thoroughly cleaned and pre-rinsed with dilute
(approximately 10% V/V) nitric acid. Filter the sample through qualitative filter paper into
a second acid-cleaned container.
9. The concentration values obtained from analysis must be corrected for the dilution factor
from the acid addition. If the sample will be analyzed by ICP-MS additional dilution will
generally be necessary. The dilutions used should be recorded and the measured
concentrations adjusted accordingly.
Quality Control
1. For each analytical batch of samples processed, analytical reagent blanks (also field blanks
if they were taken) should be carried throughout the entire sample preparation and
analytical process. These blanks will be useful in determining if samples are being
contaminated.
2. Duplicate samples should be processed on a routine basis. A duplicate sample is a real
sample brought through the whole sample preparation and analytical process. A duplicate
sample should be processed with each analytical batch or every 20 samples, whichever is
the greater number.
3. Spiked samples or standard reference materials should be employed to determine accuracy.
A spiked sample should be included with each group of samples processed and whenever a
new sample matrix is being analyzed.
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SOP 9
ICP-AES Total Metals Measurement
Refer SOP: LRPCD SOP 08.0
NRMRL LRPCD M 08 0 ICP-OES Analytical Procedure for IRIS Intrepid.pdf
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SOP 10
SOP for Ion Chromatography (1C) Anions Measurement
Refer SOP: LRPCD SOP 07.0
NRMRL LRPCD M 07_0 Ion Chromatographic Analysis of Inorganic Anions in Aqueous
Samplesx.pdf
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SOPH
SOP for X-ray Diffraction Spectroscopy Measurements
1.0 Scope and Application
X-ray Diffraction (XRD) Spectroscopy is used to determine the crystalline structure of non-
amorphous materials.
2.0 Summary of Method
The three-dimensional structure of nonamorphous materials, such as minerals, is defined by
regular, repeating planes of atoms that form a crystal lattice. When a focused X-ray beam
interacts with these planes of atoms, part of the beam is transmitted, part is absorbed by the
sample, part is refracted and scattered, and part is diffracted. Diffraction of an X-ray beam by
a crystalline solid is analogous to diffraction of light by droplets of water, producing the
familiar rainbow. X-rays are diffracted by each mineral differently, depending on what atoms
make up the crystal lattice and how these atoms are arranged.
a
10 15 20 25 30 35 *0 45 50 SS 60 65 TO
O»gree» 2-ttwu
Figure X2. (a) Simplified configuration sketch of the X-ray source (X-ray tube), the X-ray
detector, and the sample during an X-ray scan. In this configuration, the X-ray tube and the
detector both move through the angel theta (9), and the sample remains stationary, (b) Example of
an X-ray powder diffractogram produced during an X-ray scan. The peaks represent positions
where the X-ray beam has been diffracted by the crystal lattice. The set of J-spacings (the distance
between adjacent planes of atoms), which represent the unique "fingerprint" of the mineral, can
easily be calculated by the 2-theta (29) values shown. The use of degrees 2-theta in depicting X-
ray powder diffraction scans is a matter of convention, and can easily be related back to the
geometry of the instrument, shown in Figure 5a. The angle and the J-spacings are related to
Bragg' s Law, as described in the text.
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3.0 Definitions
X-ray: A form of electromagnetic radiation with a wavelength in the range of 0.01 to 10
nanometers. X-rays are primarily used for diagnostic radiography and crystallography.
4.0 Sample Handling and Preservation
Samples will be collected in glass or plastic vials. Analysis of the collected sample will occur
within 48 hour of collection. No preservation techniques will be required after collection and
prior to analysis. Samples will be disposed of after analysis negating the need for further
preservation.
5.0 Apparatus
Philips Instruments X'Pert® MPD System X-ray Diffraction Spectrometer
6.0 Procedure for Crystal Structure Determination
In X-ray powder diffractometry, X-rays are generated within a sealed tube that is under
vacuum as in the Phillips X'Pert X-ray diffractometer employed in these studies. A current is
applied that heats a filament within the tube; the higher the current the greater the number of
electrons emitted from the filament. This generation of electrons is analogous to the
production of electrons in a television picture tube. A high voltage, typically 15-60 kilovolts,
is applied within the tube. This high voltage accelerates the electrons, which then hit a target,
commonly made of copper. When these electrons hit the target, X-rays are produced. The
wavelength of these X-rays is characteristic of that target. These X-rays are collimated and
directed onto the sample, which has been ground to a fine powder or deposited as a wet paste
onto filter paper. A detector detects the X-ray signal; the signal is then processed either by a
microprocessor or electronically, converting the signal to a count rate. Changing the angle
between the X-ray source, the sample, and the detector at a controlled rate between preset
limits is an X-ray scan (Figures X2a and X2b).
When an X-ray beam hits a sample and is diffracted, we can measure the distances between the
planes of the atoms that constitute the sample by applying Bragg's Law.
Bragg's Law is: n = 2Jsin
where the integer n is the order of the diffracted beam, is the wavelength of the incident X-ray
beam, d is the distance between adjacent planes of atoms (the d-spacings), and is the angle of
incidence of the X-ray beam. Since we know A, and we can measure 0, we can calculate the d-
spacings. The geometry of an XRD unit is designed to accommodate this measurement (Figure
5b). The characteristic set of d-spacings generated in a typical X-ray scan provides a unique
diffraction pattern for specific crystal structures. When properly interpreted, by comparison
with standard reference patterns and measurements, this "fingerprint" allows for identification
of the crystal structure and mineral phases present.
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7.0 Method
1. Mount sample in XRD sample cell and load in it into the instrument
2. Open the instrument software control package on the adjacent computer (X'Pert)
3. S el ect data acqui siti on
4. Input the parameters for the current measurement.
a. For the current project samples will be analyzed from 5 to 110 degrees 2 0
b. Data points will be collected every 0.1 degrees for 2 seconds
5. The resulting scan will be compared to a reference diffraction pattern data base provided by
Philips Instruments
8.0 Quality Control
- Prior to analyzing any samples the instrument will be calibrated using a reference material (Si
111 crystal) to ensure the angle measurements are correct.
References
Philips Instruments X'Pert® MPD System X-ray Diffraction Spectrometer Users Manual
Kittel, C. Introduction to Solid State Physics, Seventh Edition. J Wiley & Sons, Inc. New York.
NY. 1996.
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SOP 12
Laboratory Glassware Cleaning
Scope
This procedure is used to clean laboratory glassware for use in general laboratory activities that
include: acid digestions, bench-scale experiments, etc. Additional cleaning steps might be needed
for some particularly contaminated glassware or analytical procedures.
Summary
All the laboratory equipment and glassware that come in contact with the soil, extraction fluid or
leachate must be rinsed off and soaked in soap water for two hours, then soaked in 5% nitric acid
followed by rinsing with deionized (DI) water to remove any residual deposits. This equipment
includes supplies, utensils and containers or any surface that will come into direct contact with the
above materials.
Reagents and Materials
Cleaning Brush - Soft, non-damaging brush (e.g. Fisher Scientific or equivalent)
Detergent - viz: Sparkleen, Fisher Scientific or equivalent.
Reagent Grade Water - Deionized (DI) water with a resistivity of 18.2 mohm can be provided
by commercially available deionization systems (e.g., Milli-Q Plus, Millipore, or equivalent
grade).
5% Nitric Acid - Made by dilution of ACS grade nitric acid (e.g. Fisher Scientific or
equivalent grade) with DI water.
Procedure
1. Rinse loose debris from the surface of the object using tap water.
2. Wash the object thoroughly using a brush, soap and water. Triple rinse with tap water.
3. Soak the obj ect in a soap bath for two hours.
4. Triple rinse with tap water.
5. Soak the object in a 5% nitric acid bath overnight
6. Remove the object from the water bath and triple rinse all surfaces with DI water.
7. Dry the object using drying racks. Take care to limit the exposure of the objects to air-borne
particulates or any source of contamination.
8. Objects that are not of immediate use should be stored in an area where the exposure to air-
borne particulates is a minimum.
Acid Bath Neutralization
The acid bath needs to be periodically prepared in order to keep it clean. To assure the safe and
environmental disposal of the 5% nitric acid solution, it will be neutralized to obtain a pH in the
range of 6-9. The neutralization will be done with sodium carbonate and a pH-meter or pH-paper
will be used to verify the final pH.
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SOP 13
SOP for TEMP/W Modeling of Thermal Changes
1.0 Scope and Application
TEMP/W will be used to simulate thermal changes in MSW after disposal of SAP waste.
2.0 Background
TEMP/W is a finite element CAD software product for analyzing thermal changes in the
ground due to environmental changes or due to the construction of facilities such as
buildings or pipelines. The comprehensive formulation makes it possible to analyze both
simple and highly complex geothermal problems. TEMP/W can be applied to the
geothermal analysis and design of geotechnical, civil, mining and solid waste engineering
projects, including facilities subjected to freezing and thawing temperature changes.
a. Hardware Requirements
To run the program the following hardware requirements are necessary:
• Intel Pentium processor or higher
• 16 Mb RAM
• Hard disk with at least 20 Mb free disk space
• VGA graphics (High Color recommended)
• MS Windows 95, 98, NT, 2000, XP, Vista (32/64 bit) or Window 7 (32/64 bit)
3.0 Procedure and Parameters
For this work, the following parameters should be placed in the correct fields within the
TEMP/W program:
Geometry Information:
• Lan dfill cell sh ape
Materials Information:
• Thermal function
• Unfrozen and frozen water content
• Thermal conductivity
• Volumetric heat capacity
Boundary Conditions Information:
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• Specify the boundary conditions that describe the various landfilling scenarios of SAP
waste
• Assign boundary conditions to the appropriate regions of the landfill cell
Running TEMP/W
• Select the analysis type (steady state or transient)
• Select the run duration and the number of runs
• From the Tools Menu select Verify/Optimize and then select Solve Analyses
Results
• View the results through Contours from the Draw Menu and Graph from the Draw Menu
• View results as needed
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SOP 14
Test Method for Toxicity Characteristics Leaching Procedure
Scope
The TCLP is designed to determine the mobility of both organic and inorganic analytes present in
liquid, solid, and multiphasic wastes. This is a standardized test that determines the potential
mobility of contaminants in a liquid or solid under simulated landfill conditions. The TCLP uses an
acidic leachant (acetic acid) to depict a 'worst case scenario' of a hazardous waste co-disposed into
a municipal solid waste landfill.
Summary of Test Method
The TCLP procedure can be found in SW 846, Method 1311. In order to perform the TCLP analysis,
an initial pH measurement of the sample must be made in order to determine the appropriate
extraction fluid. Sample (< 9.5 mm) will be used in this test. The type of extraction fluid (pH=4.93
or pH=2.88) is decided based on the characteristics of the sample. The sample will be mixed with
the extraction fluid at a liquid-solid ratio (L/S) of 20, rotated in a tumbler at 30±2 rpm for 18±2
hours. The leachate will be filtered, acid digested and analyzed for the metal content.
Reagents
1. "Unless otherwise noted, it is assumed that ACS reagent grade chemicals or their
equivalent are used. Also, unless otherwise noted, references to water are understood to
mean reagent grade water as described in 05.SOP.011.00, Reagent Water Quality and
Monitoring."
2. D.I. water (ASTM Type 2)
3. Hydrochloric acid (IN), HC1
4. Nitric acid (IN), HNO3
5. Sodium hydroxide (IN), NaOH
6. Glacial acetic acid, CH3CH2OOH
Equipment
1. Analytical Balance
2. Bottle Extraction Vessel, 2000 mL HOPE bottles
3. pH meter and buffers
4. Agitation apparatus: The agitation apparatus must be capable of rotating the extraction vessel
in an end-over-end fashion at 30 ± 2 rpm.
5. Filter Holder
6. Borosilicate glass fiber filter.
7. Extraction Fluid Transfer Devices such as positive displacement unit.
8. Beaker or Erlenmeyer flask, glass, 500 mL.
9. Magnetic stirrer
Procedure
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 27 of 478
1.0 Particle size reduction
1.1 Particle size reduction to less than 9.5 mm will be performed as follows:
• The samples will be placed in a stainless steel pan and crushed to pass a 9-mm sieve.
• After thorough mixing, approximately 0.5 kg of the 9-mm sieved materials will be
further size reduced down to a size of 2 mm using a grinding machine (Preiser
Scientific).
• The 2 mm size samples will be used for the TCLP test.
2.0 Extraction fluid preparation
2.1 Extraction Fluid # 1: Add 5.7 mL glacial CH3CH2OOH to 500 mL of reagent water,
add 64.3 mL of IN NaOH, and dilute to a volume of 1 liter. When correctly prepared,
the pH of this fluid will be 4.93 ± 0.05.
2.2 Extraction Fluid # 2: Add 5.7 mL glacial CH3CH2OOH to 1L of reagent water. When
correctly prepared, the pH of this fluid will be 2.88 ± 0.05.
3.0 Preliminary TCLP preparation
3.1 pH measurement
3.1.1 Calibrate pH meter according to SOP 3.
3.1.2 Weigh out a small subsample of the solid phase of the waste, reduce the solid (if
necessary) to a particle size of approximately 1 mm in diameter or less, and transfer
5.0 grams of the solid phase of the waste to a 500 mL beaker or Erlenmeyer flask.
3.1.3 Add 96.5 mL of reagent water to the beaker, cover with a watchglass, and stir
vigorously for 5 minutes using a magnetic stirrer. Measure and record the pH. If
the pH is <5.0, use extraction fluid #1.
3.1.4 If the pH is > 5.0, add 3.5 ml N HC1, slurry briefly, cover with a watchglass, heat
to 50°C, and hold at 50°C for 10 minutes.
3.1.5. Let the solution cool to room temperature and record the pH. If the pH is <5.0, use
extraction fluid #1. If the pH is >5.0, use extraction fluid #2.
4.0 TCLP test
4.1 Weigh out 10 g of the sample in a 500 mL plastic bottle.
54.2 Add 200 mL of the extraction fluid to the sample bottle.
4.3 Rotate the bottle rotary agitator at 30 ± 2 rpm for 18 ± 2 hours.
4.4 Following the agitation, filter the extract using Whatman 0.45 |j,m PVDF filters..
4.5 Following filtration, acidify the sample to pH less than < 2 using concentrated nitric
acid and store at 4°C.
4.6 Analyze sample for total metals after acid digestion following method 3015A.
5.0 Precision and Controls
5.1 A duplicate sample will be prepared and processed every 15 samples.
5.2 Controls are provided by running the bottles with the extraction fluid but no sample in
them.
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WA 2-26, Amendment 2 QAPP Secondary Aluminum Processing Waste
Date: June 6 2013
Revision No.: 1
Page 28 of 478
Expression of Results
Compare the analyte concentrations in the TCLP extract with the levels identified in the appropriate
regulations to determine if sample is a hazardous waste or not.
Quality Control
The procedures given in EPA Method 1311 will be followed.
1. A minimum of one blank (using the same extraction fluid as used for the samples) must
be digested and analyzed for every 15 samples.
2. A sample duplicate will be conducted every 15 samples.
3. A standard check will be analyzed every 10 samples for the TCP analysis.
4. All analyses that fall outside the range for precision and accuracy will be repeated.
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