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Test Methods for Cleaning Product Validation and Certification with CSPA

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A review of the various test methods used to validate cleaning products and achieve various certifications including EPA Safer Choice, Green Seal and EcoLogo.

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Test Methods for Cleaning Product Validation and Certification with CSPA

  1. 1. dell tech laboratories ltd. 1 Product Evaluation/Test Methods Product Safety - Regulatory Affairs – Lab Services February 11, 2016 Joe McCarthy Lab Services Manager/Regulatory Affairs Specialist
  2. 2. dell tech laboratories ltd. 2 WHY Test? WHERE can you find test methods? WHO develops the methods ? HOW can you get involved? WHAT hints & tips can help with performing the methods?
  3. 3. dell tech laboratories ltd. 3 WHY Test? Formula development & screening Evaluate performance of new product formulations. Set a benchmark to compare future reformulations against. Claims validation/support Does is actually work? Are you making specific marketing or performance claims? National Brand Equivalency (NBE), how does it compare to other products?
  4. 4. dell tech laboratories ltd. 4 WHY Test? 3rd party certification EPA Safer Choice [formerly Design for the Environment (DfE)] UL Environment (Ecologo) Green Seal Nordic Ecolabel
  5. 5. dell tech laboratories ltd. 5 It all starts and ends with customer. Why buy a product that does not work? Why sell a product that does not work? WHY Test? So why NOT test?
  6. 6. dell tech laboratories ltd. 6 WHERE can we find Test Methods? Consumer Specialty Products Association http://www.cspa.org/product-category/publications/ Includes 13 different Methods across a range of product categories such as All Purpose Cleaners, Glass Cleaners, Bathroom Cleaners, Oven Cleaners , Dish Detergents & Laundry Detergents.
  7. 7. dell tech laboratories ltd. 7 Individual Methods also Available for; DCC-01- Machine Dishwashing Estimation of Foam DCC-03- Rug Shampoo DCC-05A- Deposition on Glassware during Mechanical Dishwashing DCC-09 Glass Cleaners DCC-10 Foam Stability of Hand Dishwashing Detergents DCC-12- Guidelines for Screening the Efficacy of Oven Cleaners: DCC-13 (A through F) Fabric Softeners DCC-14- Guidelines for Anti-Redeposition Properties of Laundry Products DCC-15 Measuring Degree of Surface Abrasion by Abrasive Cleaners DCC-16 Parts I & II Evaluating the Efficacy of bathroom cleaners DCC-17 Greasy Soil Test Method DCC-18 Neat Hand Dishwashing Detergents
  8. 8. dell tech laboratories ltd. 8 ASTM http://www.astm.org/ Commonly used or cited methods for Cleaning Products ASTM D5343 - Cleaning Performance of Ceramic Tile Cleaners ASTM D4265 - Evaluating Stain Removal Performance in Home Laundering ASTM D3556* Deposition on Glassware During Mechanical Dishwashing ASTM D4009* Foam Stability of Hand Dishwashing Detergents ASTM D4488 - Cleaning Performance of Products Intended for Use on Resilient Flooring and Washable Walls (WITHDRAWN, NO REPLACEMENT)
  9. 9. dell tech laboratories ltd. 9 Other Sources IKW (German Cosmetic, Toiletry, Perfumery and Detergent Association) http://www.ikw.org/haushaltspflege/downloads/ •Methods for Ascertaining the Cleaning Performance of Dishwasher Detergents • Recommendation for the Quality Assessment of the Cleaning Performance of Cleaners for Glass Ceramic Cooking Fields •Recommendations for the quality assessment of acidic toiler cleaners Patent Searches http://www.uspto.gov/patents-application-process/search-patents Product patents often include a reference or description of methods used to assess performance.
  10. 10. dell tech laboratories ltd. 10 WHO develops these methods? We Do! Volunteers from Member Companies
  11. 11. dell tech laboratories ltd. 11 YOU Can! WHO develops these methods?
  12. 12. dell tech laboratories ltd. 12 HOW can I participate? CSPA Members 1) Go to your member profile and subscribe to Cleaning Products – Scientific Committee 2) E-mail Tim Brown at tbrown@cspa.org
  13. 13. dell tech laboratories ltd. 13 What will you get through participation? •Ahead of the curve on new methods or revised methods •A chance for input on methods or introduce new methods •Learn from experience of others •Participate in Interlaboratory tests http://www.cspa.org/events/open-cspa-events/
  14. 14. dell tech laboratories ltd. 14 Happening Right Now! CSPA DCC-17 Greasy Soil Test Method Interlaboratory testing of 2 new proposed methodologies
  15. 15. dell tech laboratories ltd. 15 CSPA DCC-17 Greasy Soil Test Method Substantial changes including; Composition, preparation, application & curing of soil. New substrate. Addition of negative and positive controls. Directions of use for dilutables, liquids, powders, sprays & wipes
  16. 16. dell tech laboratories ltd. 16 Rust Removers Stainless Steel Cleaner/Polish
  17. 17. dell tech laboratories ltd. 17 HARD SURFACE CLEANERS & DISH DETERGENTS
  18. 18. dell tech laboratories ltd. 18 WHAT hints & tips help with performing the methods? Hard Surface Cleaner Test Methods CSPA DCC-09 Glass Cleaners CSPA DCC-16 Efficacy of bathroom cleaners CSPA DCC-17 Greasy Soil Test Method ASTM D5343 - Cleaning Performance of Ceramic Tile Cleaners ASTM D4488 - Cleaning Performance of Products Intended for Use on Resilient Flooring and Washable Walls
  19. 19. dell tech laboratories ltd. 19 All have methods use a common structure. 1) Recipe and method of application for soil 2) Directions for Cleaning 3) Means of Assessing Performance
  20. 20. dell tech laboratories ltd. 20 1) Recipe and method of application for soil - Where practicable have the same individual apply the soil to all tiles. Does the method call for Bandy Black Clay as a soil ingredient? Bandy Black Clay is no longer available, use Black Charm Research Clay http://www.sdlatlas.com/Consumables/Home-Appliance Where can I find spermacetti (sperm) wax? City Chemical LLC http://www.citychemical.com/
  21. 21. dell tech laboratories ltd. 21 1) Recipe and method of application for soil - Most methods will specify a shelf life for the soil and/or soiled tiles. - Soils tend to become more persistent with age Be consistent with timing between soil/soiled tile preparation & cleaning. (i.e. make today, use tommorow)
  22. 22. dell tech laboratories ltd. 22 2) Directions for Cleaning Typically calls for the soiled tile be scrubbed with a sponge, wipe or towel using a Straight Line Washability Apparatus. (aka Gardner Abrasion Tester or Gardco Linear Motion Test Equipment) Different make & models have different size sponge holders
  23. 23. dell tech laboratories ltd. 23 2) Directions for Cleaning May need to adjust weight of sponge holder to meet weight/sponge area ratio defined in the methods. Most methods will result in ~ 0.1 lbs/in2 pressure. May need to adjust volume of product to meet volume product/sponge volume depending on size of sponge holder. Method Sponge dimension h x l x w (in) Sponge holder mass (g) Volume of product used ASTM D4488-A2 1 x 3⅝ x 1½ 350 15 mL ASTM D4488-A5 1 x 3⅝ x 1½ 350 50 mL ASTM D5343 ⅝ x 2 ⅞ x 4 ⅝ 454 10-20 mL/ 1-5 g CSPA DCC-09 1.0 x 2.6 x 3.5 454 2 g CSPA DCC-16 1.0 x 2.6 x 3.5 454 1 g CSPA DCC-17 1 x 3⅝ x 1½ 350 15 g
  24. 24. dell tech laboratories ltd. 24 Preclean the sponges before use. Sponges are shipped with a small amount of Cationic surfactant as a preservative 2) Directions for Cleaning Do not use a HE washing machine or Dryer (let air dry). It may round the edges of the sponge. (Both these sponges are damp)  
  25. 25. dell tech laboratories ltd. 25 Does the method call for 2:1 Ca:Mg hard water but not give a formula? 2) Directions for Cleaning Look to ASTM D3050 – Measuring Soil Removal from Artificially Soiled Fabrics for recipe a for 2:1 Ca:Mg hard water Scrub perpendicular to direction of soiling. ASTM D5343 CSPA DCC-17 CSPA DCC-17 CSPA DCC-17 (Today) (Proposed #1) (Proposed #2)
  26. 26. dell tech laboratories ltd. 26 Make sure the template/shims used to hold the tile in place are the same thickness as the tile. 2) Directions for Cleaning Template/shim is too low Template/shim is too high. Uneven template & tile may cause product to be squeezed out with each cycle. Uneven template & tile may cause tearing of sponge/wipe/towel
  27. 27. dell tech laboratories ltd. 27 2) Directions for Cleaning Uneven template & tile may cause sponge holder to catch and break machine.
  28. 28. dell tech laboratories ltd. 28 Ensures even contact & pressure between sponge and tile and smooth action Template & tile are level 2) Directions for Cleaning Be consistent with timing. How long between applying product to tile and starting scrubbing cycle? Longer dwell time = better performance
  29. 29. dell tech laboratories ltd. 29 3) Means of Assessing Performance Technique Pros Cons Where cited? Visual Rating System Easy, economical, reflects consumer perception Subjective, requires trained observers, limited data pool for statistics ASTM D5343 ASTM D4265 CSPA DCC-09 Gravimetric Quantitative data, useful for statistical analysis Labor intensive, does not easily translate to visual experience, subject to error if samples poorly handled none Reflectance (Instrumental) Quantitative data, useful for statistical analysis, Similar to consumer perception Expensive Almost every method
  30. 30. dell tech laboratories ltd. 30 Reflectometer (Colorimeter) 3) Means of Assessing Performance Measures Color, not reflectance (gloss) L = Lightness (100 = Pure white, 0 = Pure Black) a = Red/green b = Blue/yellow
  31. 31. dell tech laboratories ltd. 31 Lightness Reflectance is not the same as Gloss Reflectance 3) Means of Assessing Performance Printer paper White Ceramic Tile Black Ceramic Tile Lightness 90.38 91.34 9.7 60 ° Gloss 4.2 98.5 98.6
  32. 32. dell tech laboratories ltd. 32 “Take three reflectance readings each on three separate soiled tiles” 3) Means of Assessing Performance Methods define R as “reflectance”, it means Lightness (L) % Cleaning Efficiency = R(cleaned) – R(soiled) R(initial) – R(soiled) R(initial) R(soiled) R(cleaned)
  33. 33. dell tech laboratories ltd. 33 ASTM D5343 Soiled Tiles 3) Means of Assessing Performance 0% 60% 70% 80% 90% 100%
  34. 34. dell tech laboratories ltd. 34 3) Means of Assessing Performance CSPA DCC-17 PHOTOS 0% 60% 70% 80% 90% 95%
  35. 35. dell tech laboratories ltd. 35 What creative disruption may drive change for test methods & product evaluation? Digital Photography & Image Analysis Software Cheaper & Accessible More Precise & Powerful Flexibility & Options for data acquisition, handling & analysis
  36. 36. dell tech laboratories ltd. 36 METHOD SPECIFIC TIPS CSPA DCC-05/ ASTM D3556 Deposition on Glassware during Mechanical Dishwashing Use straight wall glasses, not curved glasses Wear gloves when handling so that you do not get fingerprints on the glasses  
  37. 37. dell tech laboratories ltd. 37 METHOD SPECIFIC TIPS CSPA DCC-10/ASTM D4009 Foam Stability of Hand Dishwashing Detergents Share the load & have different technicians do replicates washes for each soil/product. Marketing Reality
  38. 38. dell tech laboratories ltd. 38 METHOD SPECIFIC TIPS Latex painted masonite tiles Method directs to“Double-coat masonite tiles with latex paint using a paint roller” CSPA DCC-17/ASTM D4488-A2 Greasy Soil Test Method Apply 1 coat of primer allow to dry then “apply two coats of paint”
  39. 39. dell tech laboratories ltd. 39 Cut edges are sharp & will grab the sponge and cause it to skip or tear wipes/towels Sand edges over which sponge/wipe/towel will travel.
  40. 40. dell tech laboratories ltd. 40 CSPA DCC-16 Evaluating the Efficacy of Bathroom cleaners ASTM D5343 - Cleaning Performance of Ceramic Tile Cleaners METHOD SPECIFIC TIPS Are not the same methods, soils or substrates, but are used for the same product type. CSPA DCC-16 tends to favour acidic products. ASTM D5343 tends to favour alkaline products
  41. 41. dell tech laboratories ltd. 41 ASTM D5343 “8.2.1 Remove the tray of tiles from the oven immediately prior to soil application. Tiles can be soiled while hot or allowed to cool to room temperature.” Applying the soil to hot tiles (80 °C/175 °F) results in a more even coating, helps prevent the trim brush from getting gummed up. The soil is waxy when cooled 8.2.2 ....... It is easiest to soil an entire row of tiles with one stroke of the applicator (line the tiles up in a row so that the tile edges are touching each other and apply the soil with a broad stroke of the applicator). How many is an entire row? METHOD SPECIFIC TIPS
  42. 42. dell tech laboratories ltd. 42 LAUNDRY TESTING
  43. 43. dell tech laboratories ltd. 43 ASTM D3050 Standard Guide for Measuring Soil Removal from Artificially Soiled Fabrics A laboratory scale bench top evaluation of detergents. Allows for rapid screening of formulations and/or water conditions. Automatic control of agitation and water temperatures Wash/rinse cycle typically finished 10-13 minute range TERG-O-TOMETER
  44. 44. dell tech laboratories ltd. 44 Pros Cons Quick assessment Terg-o-Tometer $$$ Run multiple product/test conditions simultaneously Reflectometer (Colorimeter) $ Recommends use of standard soiled fabrics Evaluates performance Instrumentally using only Reflectance value of the stain Less specific on testing considerations (fabric types, soils, orientations, pretreatment of fabrics for ballast of soiled swatches) % Improvement in Reflectance = Reflectance of soil swatch after washing - Reflectance of soil swatches before washing X 100 Reflectance of unsoiled swatch before washing - Reflectance of soil swatches before washing ASTM D3050 Standard Guide for Measuring Soil Removal from Artificially Soiled Fabrics
  45. 45. dell tech laboratories ltd. 45 ASTM D4265 - Standard Guide for Evaluating Stain Removal Performance in Home Laundering A full scale evaluation of performance with Household Washers & Dryers. Correlates more closely with the Consumer Experience Allows flexibility in the choice of testing conditions including; Washing Machines (Traditional Top loader, HE Front Loader, HE Top Loader) Fabric Selection (Cotton, Cotton/Poly blend, synthetics, knits, woven) Stains (Proteins, Starchy, Bleachable, Fats, Oils, Grease) Water Temperature & Hardness Evaluation (Visible, Instrumental)
  46. 46. dell tech laboratories ltd. 46 Pros Cons Uses Household machines Longer times to run product/test condition Evaluation visually or Instrumentally Infrastructure to support multiple machines Instrumental evaluation uses compete color scale More effort required to adjust water conditions (Temperature and hardness) More detailed guidance on test conditions such as fabric types, soils, orientation, pretreatment of fabrics for ballast & soiled swatches. Reproducibility. Different machines have inherent variables. Wash times, wash & rinse volumes, agitation size etc. Guidance for preparing stained fabrics ASTM D4265 - Standard Guide for Evaluating Stain Removal Performance in Home Laundering
  47. 47. dell tech laboratories ltd. 47 ASTM D4265 - Standard Guide for Evaluating Stain Removal Performance in Home Laundering Stain considerations – manually prepared stains ASTM D4265 includes 2 annexes to provide guidance on manually preparing stains. Presents a challenge for 1) Repeatability: different individuals will prepare stains slightly differently (time/volume/pressure) 2) Reproducibility: different Labs will have different sources of stains, particularly natural stains like grass & blood 3) Time/Labour Intensive: Takes time precondition/cut/stains and cure swatches.
  48. 48. dell tech laboratories ltd. 48 ASTM D4265 - Standard Guide for Evaluating Stain Removal Performance in Home Laundering Stain considerations – Standard Soiled Fabrics Standard soiled fabrics in a wide range of stains and fabrics are commercially available CFT CS-15 EMPA 111 CFT CS-32 EMPA 114 Fruit Juice Blood, not aged Sebum w. Carbon black Red Wine, not aged www.testfabrics.com http://www.sdlatlas.com/
  49. 49. dell tech laboratories ltd. 49 Cotton-Jersey with 15 different stains: Make-up, Curry, Red wine, Tomato sauce, Blood, Dessert (chocolate), Peat, Tea, Beta-Carotene, Grass, Animal fat/red dye, Baby-food, Clay, Butter, used Engine oil EMPA (Swiss Federal Laboratories for Materials Science & Technology) Stain Monitor 102
  50. 50. dell tech laboratories ltd. 50 How is Performance Evaluated? Instrumentally Reflectometer (Colorimeter) Measures Color, not reflectance (gloss) L = Lightness (100 = Pure white, 0 = Pure Black) a = Red/green b = Blue/yellow
  51. 51. dell tech laboratories ltd. 51 How is Performance Evaluated? Instrumentally Stain removal Index (SRI) The SRI is a 0-100 scale, with 0 = no stain removal and 100 = complete stain removal SRI = 100 x ΔE*(US-UF) - ΔE*(WS-UF) ΔE*(US-UF) Where: US = Unwashed stain area UF = Unwashed (unstained) fabric area ΔE*(US-UF) = Delta-E color difference between the unwashed stain and the unwashed fabric Δ E*(WS-UF) = Delta-E color difference between the washed stain and the unwashed fabric. The value ΔE (absolute color difference) is calculated as: ΔE* = √ΔL*2+ Δa*2+ Δb*2 Where: L = reflectance, a = redness/greenness, b = yellowness/blueness,
  52. 52. dell tech laboratories ltd. 52 How is Performance Evaluated? Visually Using a 1 to 5 Rating Scale by comparing stains after washing against the AATCC 130 Stain release Replica. 1 = Residual stain equivalent to Replica 1 2 = Residual stain equivalent to Replica 2 3 = Residual stain equivalent to Replica 3 4 = Residual stain equivalent to Replica 4 5 = No residual stain
  53. 53. dell tech laboratories ltd. 53 Trick is to judge intensity of the stain. Challenge is in applying a monochromatic scale to colored stains. Original Intent of AATCC 130 was to evaluate the ability of fabrics to release oily stains (Corn oil) Many stains are intensely colored or saturated and rate lower than 1.0 How do you rate these stains? (Chocolate/curry/red wine) How is Performance Evaluated? Visually
  54. 54. dell tech laboratories ltd. 54 How is Performance Evaluated? Image Analysis Uses a combination of digital scanning/photography along with Image Analysis software.
  55. 55. dell tech laboratories ltd. 55 How is Performance Evaluated? Summary of Techniques Stain Before After ASTM D4265 Colorimeter Stain removal index (Lightness, red/green, blue/yellow) AATCC 130 visual rating (5 judges) ASTM D3050 % Improvement in reflectance (Lightness only) Motor oil 76.6% 1.5 48.9% Animal fat & red dye 64.4% 2 49.9% Tomato Sauce 82.3% 3.5 74.4%
  56. 56. dell tech laboratories ltd. 56 How is Performance Evaluated? Summary of Techniques Method of Evaluation Pros Cons Instrumental Quantitative data NIST traceable calibration Used in published standard methods History as Industry Standard Factors measurement of stain before washing in calculations Cost of Colorimeter Limited area of measurement without taking multiple readings across stain area. Visual Economical Quick Subjective Does not factor in intensity of stain before washing in rating Monochromatic scale Requires a panel of judges (≥3) Image Analysis Quantitative data Economical & Accessible Complete Stain area selection color scale Calibration traceability?
  57. 57. dell tech laboratories ltd. 57 Color loss susceptibility Dye swatch ID Heavy Nylon 6.6 dyed Acid red 151, Medium Cotton Print Cloth Direct Blue 1 Light Cotton Print Cloth Direct Blue 90 ASTM D5548 Standard Guide for Evaluating Color Transfer or Color Loss of Dyed Fabrics in Laundering This test method evaluates the degree of color loss from a dyed fabric and or color transfer to undyed fabric. Uses 3 different standard dyed swatches prone to heavy, medium or light color loss along with undyed cotton print cloth to accept released dye. Each dyed swatch is washed separately in a Terg-o-tometer But can be modified to use a household machine as in ASTM D4265 How is Performance Evaluated? Color Loss & Transfer
  58. 58. dell tech laboratories ltd. 58 Color Loss (or Color Transfer) is measured as absolute Color change ΔE ΔE = √ (Lw - Lo)2 + (aw – ao)2 + (bw - bo)2 Where: L = reflectance, a = redness/greenness, b = yellowness/blueness w = fabric before washing o = fabric after washing How is Performance Evaluated? Color Loss & Transfer
  59. 59. dell tech laboratories ltd. 59 Foam is not your Friend It all starts and ends with customer. Frustrates customer, wastes water , energy & time How is Performance Evaluated? Foaming
  60. 60. dell tech laboratories ltd. 60 FOAMING ASTM D1173 Standard Test Method for Foaming Properties of Surface-Active Agents (Ross Miles Foam Test) ASTM D3519-Standard Test Method for Foam in Aqueous Media (Blender Test) Assess both how much foam is produced immediately and how quickly it knocks down
  61. 61. dell tech laboratories ltd. 61 Looking for more on Formulation & Testing? Consumer Specialty Products Association hosts a Cleaning Products Fundamentals Course every 2 years at its mid-year meeting. CSPA is planning an Intermediate Course for May 2016 in Washington D.C. Presented by leading Companies and industry Professionals Curriculum includes surfactants, builders, additives, solvents, formulations, testing, sustainability & regulatory issues. Look for information & registration at http://www.cspa.org/events/cspa-event-directory/
  62. 62. dell tech laboratories ltd. 62 Thank YouQuestions / Comments / Contact Presented by: Joe McCarthy Lab Services Manager/Senior Regulatory Affairs Specialist jmccarthy@delltech.com 519-858-5024 www.delltech.com Product Safety - Regulatory Affairs – Lab Services

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