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Technical Workshop on Product Quality - Candle Waxes 1
World Candle Congress Orlando, FL 20,21 Apr-2004
Candle Wax Product Quality
A Technical Workshop for the World Candle Congress
presented by ALAFAVE & the National Candle Association
Orlando, FL 20,21-April-2004
Presenters:Carl Hudson, ExxonMobil
Ed Calcote, Shell
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World Candle Congress Orlando, FL 20,21 Apr-2004
Workshop Topics
Produce Quality Wax on Spec
Avoid Contamination During Shipping
Maintain Product Quality Before/During Use
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Wax - Component in Candle “System”
WAX: PROVIDES STRUCTURE; INFLUENCES APPEARANCE
QUALITY OF A CANDLE SYSTEM -
RESULT OF OVERALL DESIGN & FORMULATION
WICK - FUEL: NEED BALANCE FOR OPTIMUM BURNING
GOAL =WAX + ADDITIVES ---> CO2 + H2O
FRAGRANCE:MINIMUM ODOR
FROM WAX;WAX HELPS “HOLD”
& “THROW”FRAGRANCE
COLOR: MINIMUM IMPACT
FROM WAX COLOR
CONTAINER OR HOLDER IF REQUIRED
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Wax Selection Tied to Candle Type
PILLAR & TAPER CANDLES+ FULLY REFINED WAX - HIGHER MELT POINT
– HARDER (HIGHER n-PARAFFIN %, NARROWER SPREAD)– LOWER OIL CONTENT
CONTAINER & JAR CANDLES+ FULLY REFINED, SCALE OR SEMI-REFINED WAX - LOWER MELT POINT
– SOFTER (LOWER n-PARAFFIN %, WIDER SPREAD)– CAN HAVE HIGHER OIL CONTENT
VOTIVE CANDLES+ FULLY REFINED, SCALE OR SEMI-REFINED WAX - LOWER MELT POINT
– SOFTER (LOWER n-PARAFFIN %, WIDER SPREAD)– OFTEN WITH HIGHER OIL CONTENT
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Characterization of Candle Waxes
MELT/CONGEAL POINT - TEMP. OF LIQUID/SOLID PHASE CHANGE OIL CONTENT - LIQUIDS SOLVENT EXTRACTED FROM CHILLED WAX
COLOR - COLOR OF LIQUID WAX (Saybolt or ASTM Scale)
ODOR - ODOR COMPARISON OF SOLID WAX
NEEDLE PENETRATION - MEASURES HARDNESS OF SOLID WAX
VISCOSITY - RESISTANCE TO FLOW OF LIQUID WAX
FLASH POINT - MINIMUM TEMPERATURE OF LIQUID WAX THAT PRODUCES FLAMMABLE VAPOR PHASE
FDA GRADE (PASS/FAIL) - UV ABSORBANCE TEST TO IDENTIFY PRESENCE OF POLYNUCLEAR AROMATICS
GAS CHROMATOGRAPHY (GC) - CARBON NUMBER DISTRIBUTION
DIFFERENTIAL SCANNING CALORIMETRY (DSC) - HEAT OF TRANSITION DURING LIQUID/SOLID PHASE CHANGES
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ASTM D87 Melt or D938 Congeal Methods
Test Method Reproducibility Gives Range of Answers Typical Reproducibility for ASTM D87 Melt Point, Deg F
126.0
126.5
127.0
127.5
128.0
128.5
129.0
129.5
130.0
130.5
131.0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25
Deg
F Reproducibility Range
ASTM Wax Crosscheck Program Sample - WX 0202
Acceptable ASTM D87 Test Method ValuesRanged from 127.4 to 128.8 degF
Spec. Range for MP Typically
3-5 degF
CofA Value Typically
Represents+ / - 0.5 degF
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ASTM D87 Results for Mid-Melt Paraffin
18 Month Results Consistent Within Spec. Range
Spec. Range57.8-59.4oC
CofA Value Typically
Represents+ / - 0.5 degF
57.80
58.00
58.20
58.40
58.60
58.80
59.00
59.20
59.40
0 20 40 60 80 100 120 140
ASTM D87 Reproducibility Range
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ASTM D721 Oil-in-Wax (OIW) Method
Test Method Reproducibility Gives Range of Answers
Spec. Range for FRW OIW Typically 0.0-0.5 %
Typical Reproducibility for ASTM D721 OIW, wt%
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25
Deg
F
Reproducibility Range
ASTM Wax Crosscheck Program Sample - WX 0202
Valid ASTM D721 Test Method ValuesRanged from 0.05 to 0.45%
CofA Value Typically
Represents+ / - 0.15 %
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ASTM D156 / 6045 Saybolt Color Method
Saybolt Color of +30 = Water White (no color)
Saybolt Color of +26 = Faint Straw
Saybolt Color of +24 = Light Straw Yellow
Saybolt Color of +20 = Straw Yellow
Demonstration: Representative Color Samples
Typical Spec. Saybolt Color Ranges (Reproducibility + / - 1)Fully Refined Wax +28 to +30Semi-Refined Wax +20 to +30Scale Wax +10 to +25Slack Wax < +20 down to <-16 (ASTM scale)
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World Candle Congress Orlando, FL 20,21 Apr-2004
ASTM D1833 Cold Odor Method
Odor Testing Can Be Very Subjective!
DewaxingSolvent
Primary Odor Concerns:
Contami-nants Oxidation
Demonstration: Odor Panel with Prepared Wax SamplesTypical Odor Specs. [Scale 0-4; Reproducibility + / - 1]
Fully Refined Wax 0 to 1Semi-Refined Wax 0 to 1Scale Wax > 1Slack Wax > 2
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Are All 130oF MP Waxes The Same?
NO ! And, Here Are Some Reasons Why:
Oil ContentMore oil
lowers MPsoftens wax
0
2
4
6
8
10
12
14
18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50
Carbon Number
%
Straight Cut:Nominal Carbon 27PEN @ 40C 95 dmm95% Cutwidth 13-14
Blended Wax:Nominal Carbon 31PEN @ 40C 120 dmm95% Cutwidth 19
% n-ParaffinHigher % n-Par
raises MPhardens wax
Straight Cut or Blend
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Wax Loading & Shipping
Molten Wax by Truck Short Hauls (<600 mi); 45,000 lbRequires Immediate UnloadingConcerns: Previous Load Contaminants; Particulates
Molten Wax by RailcarLonger Hauls; 150,000 lbCan Be Heated for Offloading as RequiredConcerns: Previous Load Contaminants; Particulates;Oxidative Degradation from Overheating
Solid Wax in Slabs, PelletsConcerns: Dust/Particulates; Discoloration (long-term);Previous Product Contamination (in packaging equip.)
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Wax Storage & Handling
Recommended Bulk Storage Tank Temperature is 20-30oF Above Wax Melt or Congeal Point
+ Helps Insure Homogeneous Product + Reduces Risk of Degradation Due to Oxidation
Smaller “Day or Run” Tank Recommended if Higher Temperature Needed for Manufacturing
Storage Tank Recommendations + Outlet 12” Above Tank Bottom + “Y” Duplex Strainers or Filters (60 mesh)+ Clean Filters Regularly (monthly)+ Drain Water from Tank Bottom Regularly
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Summary Points
Produce Quality Wax on SpecUnderstand Wax Specifications / PropertiesPurchase Quality Wax from Dependable Supplier
Avoid Contamination During ShippingInspect / Analyze Wax Upon ArrivalCheck CofA vs. Wax Specifications
Maintain Product Quality Before / During UseUnload & Store Wax ProperlyAvoid Overheating & Particulate Contamination
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Wax PQ Workshop - Legal Disclaimer
Please Note: "With respect to the information provided herein, neither Exxon Mobil
Corporation, Shell Oil Products US, Shell Global Solutions (US) Inc., nor their affiliates nor any of their employees makes any warranty, express or implied, including warranties of fitness for a particular purpose, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any apparatus, product or processdisclosed or represents that its use would not infringe on privately owned rights. In no event shall Exxon Mobil Corporation or Shell Oil Products US or Shell Global Solutions (US) Inc. be liable for any direct, indirect, incidental, punitive, or consequential damages of any kind whatsoever with respect to the materials and the products referenced in this presentation."
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Wax PQ Workshop - Back-Up Info
Composition Influences Wax PropertiesCarbon Distribution by Wax GCOil vs. Wax Defined by Solubility TestDewaxing/Deoiling to Obtain Wax (from Lube Oils)Wax Oxidation IssuesOthers?
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Composition Influences Wax Properties
Increasing Value Melting Point Hardness Shrinkage
Average CarbonNumber
n-Paraffin Content, %
Carbon NumberSpread
Oil Content, %
20 - 50 FRP35 - 80 Micro
Typical Range
10 - 25 FRP25 - 40 Micro
< 0.5 FRP1 - 5 Scale
1 - 10 Micro
50-90% FRP< 10% Micro
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Carbon Distribution by Wax GC
1. CARBON NUMBER - WAX GRADE; MELT POINT2. NORMAL TO ISO RATIO - IMPACTS HARDNESS; MP3. 95% CUTWIDTH - IMPACTS HARDNESS; MP
0
2
4
6
8
10
12
14
18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45
Carbon Number
%Total Paraffins
Nominal Carbon 25
95% Cutwidth 13
n-Paraffins - 80%
iso-Paraffins - 20%
1
2
3
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Oil vs. Wax - Defined by Solubility Test
ASTM D-7211.0 g Wax15 mL Methyl ethyl ketone< -30oC with stirring
COLD!
WAX+
MEK+
OIL
WARM!
WAX
MEK+
OIL
Filter the wax
MEK EVAPORATES
OIL
Remove solventWeigh residual oil
NOTE: Temperature Determines Molecule Solubility, i.e., Oil Content is Defined by the Conditions of the Method.
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Dewaxing/Deoiling to Obtain Wax
CHILLING/CHILLING/WAX CRYSTALLIZATIONWAX CRYSTALLIZATION
DEWAXING SOLVENTDEWAXING SOLVENT
WAX &WAX &OILOIL
DEWAXEDDEWAXEDOILOIL
SOLVENTSOLVENTRECOVERYRECOVERY
ROTARYROTARYFILTRATIONFILTRATION
STAGESTAGE
WAX
1st Stage SLACK WAX 5-30% OIL
2nd Stage SCALE / SEMI-REFINED WAX 1-5% OIL
3rd Stage REFINED WAX <1% OIL
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Wax Oxidation Issues
Wax Oxidizes Over Time at Elevated Temperature + Can Produce Yellow-Brown Color + Objectionable Odors Can Result+ Forms Heavy Molecules That Can Create Sludge
If Tank of Wax Becomes Oxidized, Complete Drain & Clean Sequence is Highly Recommended
To Minimize Detrimental Effects of Oxidation + Keep Wax Temperature as Low as Possible + Recommend 20-30oF Above Melt/Congeal Point+ Use Anti-Oxidants as Needed (e.g., BHT)