Candle Wax Product Quality

Candle Wax Product Quality A Technical Workshop for the World Candle Congress presented by ALAFAVE & the National Candle Association Orlando, FL 20,21-April- Presenters: Carl Hudson, ExxonMobil Ed Calcote, Shell Technical Workshop on Product Quality - Candle Waxes 1

Workshop Topics Produce Quality Wax on Spec Avoid Contamination During Shipping Maintain Product Quality Before/During Use Technical Workshop on Product Quality - Candle Waxes 2

Wax - Component in Candle System WAX: PROVIDES STRUCTURE; INFLUENCES APPEARANCE FRAGRANCE: MINIMUM ODOR FROM WAX; WAX HELPS HOLD & THROW FRAGRANCE CONTAINER OR HOLDER IF REQUIRED WICK - FUEL: NEED BALANCE FOR OPTIMUM BURNING GOAL = WAX + ADDITIVES ---> CO 2 + H 2 O COLOR: MINIMUM IMPACT FROM WAX COLOR QUALITY OF A CANDLE SYSTEM - RESULT OF OVERALL DESIGN & FORMULATION Technical Workshop on Product Quality - Candle Waxes 3

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 Technical Workshop on Product Quality - Candle Waxes 4

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 Technical Workshop on Product Quality - Candle Waxes 5

ASTM D87 Melt or D938 Congeal Methods Test Method Reproducibility Gives Range of Answers 131.0 Typical Reproducibility for ASTM D87 Melt Point, Deg F Spec. Range for MP Typically 3-5 degf CofA Value Typically Represents + / - 0.5 degf Deg F 130.5 130.0 129.5 129.0 128.5 128.0 127.5 127.0 126.5 126.0 Acceptable ASTM D87 Test Method Values Ranged from 127.4 to 128.8 degf Reproducibility Range ASTM Wax Crosscheck Program Sample - WX 0202 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 Technical Workshop on Product Quality - Candle Waxes 6

ASTM D87 Results for Mid-Melt Paraffin 18 Month Results Consistent Within Spec. Range Spec. Range 57.8-59.4 o C CofA Value Typically Represents + / - 0.5 degf 59.40 59.20 59.00 58.80 58.60 58.40 58.20 58.00 57.80 ASTM D87 Reproducibility Range 0 20 40 60 80 100 120 140 Technical Workshop on Product Quality - Candle Waxes 7

ASTM D721 Oil-in-Wax (OIW) Method Test Method Reproducibility Gives Range of Answers Typical Reproducibility for ASTM D721 OIW, wt% Spec. Range for FRW OIW Typically 0.0-0.5 % CofA Value Typically Represents + / - 0.15 % Deg F 1.6 1.4 1.2 1.0 0.8 0.6 0.4 0.2 0.0 ASTM Wax Crosscheck Program Sample - WX 0202 Valid ASTM D721 Test Method Values Ranged from 0.05 to 0.45% Reproducibility Range 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 Technical Workshop on Product Quality - Candle Waxes 8

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 +30 Semi-Refined Wax +20 to +30 Scale Wax +10 to +25 Slack Wax < +20 down to <-16 (ASTM scale) Technical Workshop on Product Quality - Candle Waxes 9

ASTM D1833 Cold Odor Method Odor Testing Can Be Very Subjective! Primary Odor Concerns: Dewaxing Solvent Contaminants Oxidation Demonstration: Odor Panel with Prepared Wax Samples Typical Odor Specs. [Scale 0-4; Reproducibility + / - 1] Fully Refined Wax 0 to 1 Semi-Refined Wax 0 to 1 Scale Wax > 1 Slack Wax > 2 Technical Workshop on Product Quality - Candle Waxes 10

Are All 130 o F MP Waxes The Same? NO! And, Here Are Some Reasons Why: Oil Content More oil lowers MP softens wax % n-paraffin Higher % n-par raises MP hardens wax % 14 12 10 8 6 4 Straight Cut: Nominal Carbon 27 PEN @ 40C 95 dmm 95% Cutwidth 13-14 Blended Wax: Nominal Carbon 31 PEN @ 40C 120 dmm 95% Cutwidth 19 Straight Cut or Blend 2 0 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 Technical Workshop on Product Quality - Candle Waxes 11

Wax Loading & Shipping Molten Wax by Truck Short Hauls (<600 mi); 45,000 lb Requires Immediate Unloading Concerns: Previous Load Contaminants; Particulates Molten Wax by Railcar Longer Hauls; 150,000 lb Can Be Heated for Offloading as Required Concerns: Previous Load Contaminants; Particulates; Oxidative Degradation from Overheating Solid Wax in Slabs, Pellets Concerns: Dust/Particulates; Discoloration (long-term); Previous Product Contamination (in packaging equip.) Technical Workshop on Product Quality - Candle Waxes 12

Wax Storage & Handling Recommended Bulk Storage Tank Temperature is 20-30 o F 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 Technical Workshop on Product Quality - Candle Waxes 13

Summary Points Produce Quality Wax on Spec Understand Wax Specifications / Properties Purchase Quality Wax from Dependable Supplier Avoid Contamination During Shipping Inspect / Analyze Wax Upon Arrival Check CofA vs. Wax Specifications Maintain Product Quality Before / During Use Unload & Store Wax Properly Avoid Overheating & Particulate Contamination Technical Workshop on Product Quality - Candle Waxes 14

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 process disclosed 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." Technical Workshop on Product Quality - Candle Waxes 15

Wax PQ Workshop - Back-Up Info Composition Influences Wax Properties Carbon Distribution by Wax GC Oil vs. Wax Defined by Solubility Test Dewaxing/Deoiling to Obtain Wax (from Lube Oils) Wax Oxidation Issues Others? Technical Workshop on Product Quality - Candle Waxes 16

Composition Influences Wax Properties Increasing Value Melting Point Hardness Shrinkage Typical Range Average Carbon Number 20-50 FRP 35-80 Micro n-paraffin Content, % 50-90% FRP < 10% Micro Carbon Number Spread 10-25 FRP 25-40 Micro Oil Content, % < 0.5 FRP 1-5 Scale 1-10 Micro Technical Workshop on Product Quality - Candle Waxes 17

Carbon Distribution by Wax GC 14 12 10 Total Paraffins Nominal Carbon 25 95% Cutwidth 13 1 3 % 8 6 4 n-paraffins - 80% iso-paraffins - 20% 2 2 0 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 1. CARBON NUMBER - WAX GRADE; MELT POINT 2. NORMAL TO ISO RATIO - IMPACTS HARDNESS; MP 3. 95% CUTWIDTH - IMPACTS HARDNESS; MP Technical Workshop on Product Quality - Candle Waxes 18

Oil vs. Wax - Defined by Solubility Test 1.0 g Wax 15 ml Methyl ethyl ketone < -30 o C with stirring Filter the wax ASTM D-721 WAX + MEK + OIL COLD! WAX MEK + OIL WARM! Remove solvent Weigh residual oil MEK EVAPORATES OIL NOTE: Temperature Determines Molecule Solubility, i.e., Oil Content is Defined by the Conditions of the Method. Technical Workshop on Product Quality - Candle Waxes 19

Dewaxing/Deoiling to Obtain Wax DEWAXING SOLVENT WAX & OIL WAX CHILLING/ WAX CRYSTALLIZATION ROTARY FILTRATION STAGE SOLVENT RECOVERY DEWAXED OIL 1st Stage SLACK WAX 5-30% OIL 2nd Stage SCALE / SEMI-REFINED WAX 1-5% OIL 3rd Stage REFINED WAX <1% OIL Technical Workshop on Product Quality - Candle Waxes 20

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 20-30 o F Above Melt/Congeal Point + Use Anti-Oxidants as Needed (e.g., BHT) Technical Workshop on Product Quality - Candle Waxes 21