Test Methods for Cleaning Product Validation and Certification with CSPA

dell tech laboratories ltd. 1

Product Evaluation/Test Methods

Product Safety - Regulatory Affairs – Lab Services

February 11, 2016

Joe McCarthyLab Services Manager/Regulatory Affairs Specialist


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?


WHY Test?

Formula development & screeningEvaluate performance of new product formulations.Set a benchmark to compare future reformulations against.

Claims validation/supportDoes is actually work?Are you making specific marketing or performance claims?National Brand Equivalency (NBE), how does it compare to

other products?


WHY Test?

3rd party certification

EPA Safer Choice [formerly Design for the Environment (DfE)]

UL Environment (Ecologo) Green Seal Nordic Ecolabel


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?


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.

http://www.cspa.org/product-category/publications/


Individual Methods also Available for;

DCC-01- Machine Dishwashing Estimation of FoamDCC-03- Rug ShampooDCC-05A- Deposition on Glassware during Mechanical DishwashingDCC-09 Glass CleanersDCC-10 Foam Stability of Hand Dishwashing DetergentsDCC-12- Guidelines for Screening the Efficacy of Oven Cleaners:DCC-13 (A through F) Fabric SoftenersDCC-14- Guidelines for Anti-Redeposition Properties of Laundry ProductsDCC-15 Measuring Degree of Surface Abrasion by Abrasive CleanersDCC-16 Parts I & II Evaluating the Efficacy of bathroom cleanersDCC-17 Greasy Soil Test MethodDCC-18 Neat Hand Dishwashing Detergents


ASTM http://www.astm.org/

Commonly used or cited methods for Cleaning Products

ASTM D5343 - Cleaning Performance of Ceramic Tile CleanersASTM D4265 - Evaluating Stain Removal Performance in Home LaunderingASTM D3556* Deposition on Glassware During Mechanical DishwashingASTM D4009* Foam Stability of Hand Dishwashing DetergentsASTM D4488 - Cleaning Performance of Products Intended for Use on Resilient Flooring

and Washable Walls (WITHDRAWN, NO REPLACEMENT)

http://www.astm.org/


Other SourcesIKW (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 Searcheshttp://www.uspto.gov/patents-application-process/search-patents

Product patents often include a reference or description of methods used to assess performance.

http://www.ikw.org/haushaltspflege/downloads/

http://www.uspto.gov/patents-application-process/search-patents

http://www.uspto.gov/patents-application-process/search-patents


WHO develops these methods?

We Do!

Volunteers from Member Companies


YOU Can!

WHO develops these methods?


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 [email protected]


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/

http://www.cspa.org/events/open-cspa-events/


Happening Right Now!

CSPA DCC-17 Greasy Soil Test Method

Interlaboratory testing of 2 new proposed methodologies


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


Rust Removers Stainless Steel Cleaner/Polish


HARD SURFACE CLEANERS & DISH DETERGENTS


WHAT hints & tips help with performing the methods?

Hard Surface Cleaner Test Methods

CSPA DCC-09 Glass CleanersCSPA DCC-16 Efficacy of bathroom cleaners

CSPA DCC-17 Greasy Soil Test MethodASTM D5343 - Cleaning Performance of Ceramic Tile Cleaners

ASTM D4488 - Cleaning Performance of Products Intended for Use on Resilient Flooring and Washable Walls


All have methods use a common structure.

1) Recipe and method of application for soil

2) Directions for Cleaning

3) Means of Assessing Performance



- 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 Clayhttp://www.sdlatlas.com/Consumables/Home-Appliance

Where can I find spermacetti (sperm) wax?

City Chemical LLC http://www.citychemical.com/

http://www.sdlatlas.com/Consumables/Home-Appliance

http://www.citychemical.com/



- 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)



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



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


Preclean the sponges before use. Sponges are shipped with a small amount of Cationic surfactant as a preservative


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)


Does the method call for 2:1 Ca:Mg hard water but not give a formula?


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)


Make sure the template/shims used to hold the tile in place are the same thickness as the tile.


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



Uneven template & tile may cause sponge holder to catch and break machine.


Ensures even contact & pressure between sponge and tile and smooth action

Template & tile are level


Be consistent with timing. How long between applying product to tile and starting scrubbing cycle?

Longer dwell time = better performance



Technique Pros Cons Where cited?

Visual Rating SystemEasy, economical, reflects consumer

perception

Subjective, requires trained observers, limited

data pool for statistics

ASTM D5343ASTM D4265CSPA DCC-09

GravimetricQuantitative 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


Reflectometer (Colorimeter)


Measures Color, not reflectance (gloss)

L = Lightness (100 = Pure white, 0 = Pure Black)a = Red/green

b = Blue/yellow


Lightness Reflectance is not the same as Gloss Reflectance


Printer paperWhite Ceramic

TileBlack Ceramic

TileLightness 90.38 91.34 9.760 ° Gloss 4.2 98.5 98.6


“Take three reflectance readings each on three separate soiled tiles”


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)


ASTM D5343 Soiled Tiles


0% 60% 70%

80% 90% 100%



CSPA DCC-17 PHOTOS

0% 60% 70%

80% 90% 95%


What creative disruption may drive change for test methods & product evaluation?

Digital Photography & Image Analysis Software

Cheaper & AccessibleMore Precise & Powerful

Flexibility & Options for data acquisition, handling & analysis


METHOD SPECIFIC TIPS

CSPA DCC-05/ ASTM D3556Deposition 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



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



Latex painted masonite tilesMethod 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”


Cut edges are sharp & will grab the sponge and cause it to skipor tear wipes/towels

Sand edges over which sponge/wipe/towel will travel.


CSPA DCC-16 Evaluating the Efficacy of Bathroom cleanersASTM D5343 - Cleaning Performance of Ceramic Tile Cleaners


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


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 cooled8.2.2 ....... 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?



LAUNDRY TESTING


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 temperaturesWash/rinse cycle typically finished 10-13 minute range

TERG-O-TOMETER


Pros ConsQuick 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 stainLess 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


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)


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




Stain considerations – manually prepared stains

ASTM D4265 includes 2 annexes to provide guidance on manually preparing stains.

Presents a challenge for1) 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.



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.comhttp://www.sdlatlas.com/

http://www.testfabrics.com/

http://www.sdlatlas.com/


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


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


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,


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 12 = Residual stain equivalent to Replica 23 = Residual stain equivalent to Replica 34 = Residual stain equivalent to Replica 4

5 = No residual stain


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


How is Performance Evaluated? Image Analysis

Uses a combination of digital scanning/photography along with Image Analysis software.


How is Performance Evaluated?Summary of Techniques

Stain Before After

ASTM D4265Colorimeter

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%


How is Performance Evaluated?Summary of Techniques

Method of Evaluation Pros Cons

Instrumental

Quantitative dataNIST traceable calibration

Used in published standard methodsHistory as Industry Standard

Factors measurement of stain before washing in calculations

Cost of ColorimeterLimited area of measurement without

taking multiple readings across stain area.

Visual EconomicalQuick

SubjectiveDoes not factor in intensity of stain before

washing in ratingMonochromatic scale

Requires a panel of judges (≥3)

Image Analysis

Quantitative dataEconomical & Accessible

Complete Stain area selectioncolor scale

Calibration traceability?


Color loss susceptibility Dye swatch IDHeavy Nylon 6.6 dyed Acid red 151,

Medium Cotton Print Cloth Direct Blue 1Light 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-tometerBut can be modified to use a household machine as in ASTM D4265

How is Performance Evaluated?Color Loss & Transfer


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


Foam is not your Friend

It all starts and ends with customer.

Frustrates customer, wastes water , energy & time

How is Performance Evaluated?Foaming


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


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/

http://www.cspa.org/events/cspa-event-directory/


Thank YouQuestions / Comments / Contact

Presented by:Joe McCarthyLab Services Manager/Senior Regulatory Affairs [email protected]

www.delltech.comProduct Safety - Regulatory Affairs – Lab Services

mailto:[email protected]

http://www.delltech.com/