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 McCarthy
Lab 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 & 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?

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.

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

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and Washable Walls (WITHDRAWN, NO REPLACEMENT)

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.

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 tbrown@cspa.org

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/

Happening Right Now!
CSPA DCC-17 Greasy Soil Test Method
Interlaboratory testing of 2 new proposed methodologies

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 Cleaners
CSPA DCC-16 Efficacy of bathroom 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 Clay
http://www.sdlatlas.com/Consumables/Home-Appliance
Where can I find spermacetti (sperm) wax?
City Chemical LLC
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 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

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 paper
White Ceramic
Tile
Black Ceramic
Tile
Lightness 90.38 91.34 9.7
60 ° 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 & Accessible
More Precise & Powerful
Flexibility & Options for data acquisition, handling & analysis

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
 

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 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”

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.

CSPA DCC-16 Evaluating the Efficacy of Bathroom 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 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?

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 temperatures
Wash/rinse cycle typically finished 10-13 minute range
TERG-O-TOMETER

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

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
ASTM D4265 - Standard Guide for Evaluating Stain Removal Performance in
Home Laundering

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.

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/

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 1
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 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%

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?

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
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
Color Loss & Transfer

Foam is not your Friend
It all starts and ends with customer.
Frustrates customer, wastes water , energy & time
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/

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

Test Methods for Cleaning Product Validation and Certification with CSPA

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