AATCC

®
R e v i e w
Journal for Textile Professionals Vol. 9, No. 6 JUNE 2009

Peer Reviewed:
• Improving Nerve Regeneration
Conduits with Plasma
• Obtaining Flame-Retardant
Cotton with Plasma

Colorfastness to Light:
Finding a Blue Wool
Equivalent
Up in Smoke:
Flammability of
Construction and
Building Textiles

Protecting Consumers!
40
(and brand reputations) e
le
b r at i
n
g
C

Years
1969 2009
ce
Publ

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in e
g Exc
“If you do the math, by 2050 there’s
not going to be a whole lot of land
left for anything other than people.”
— Dr. Jason Clay, SVP Market Transformation, World Wildlife Fund

Cotton is Critical to Feeding and Clothing the World’s Growing Population

AMERICA’S COTTON PRODUCERS AND IMPORTERS. ™ Service Mark/Trademark of Cotton Incorporated. © Cotton Incorporated, 2009.

Cotton Incorporated has just released a short film which discusses resource management solutions
that are being developed to serve the food and fiber needs of the expanding worldwide population.
Cotton and the Second Green Revolution examines how modern science is turning cotton into a food
crop as well as a fiber crop—one that makes better use of land, water, and labor resources as existing
technologies continue to evolve. Watch the video online at www.cottoninc.com/sustainability
or contact your Cotton Incorporated representative for a copy on DVD.

The Fabric of Our Lives®

 Con tents
Departments 38 Hydrophilicity and Cell Affinity of
Atmospheric-Pressure Plasma
4 Soapbox Jet-Treated Nerve
5 People Regeneration Conduit
8 A2 By Lin Lou, Jia Zhou,
and Nanliang Chen
20 Industry News
Determining the influence of
48 40 Years Ago… atmospheric-pressure
Cover 3 Ad Index plasma jet treatment on
hydrophilicity and cell affinity of
Feature three different nerve regeneration
22 Protecting the Brand conduits for repairing nerve injuries.
By Maria C. Thiry
Restricted substance lists protect Student Paper
consumers from coming into contact
with possibly harmful chemicals—and Competition
they also protect brands’ precious
reputations.
Winner
43 Colorfastness to Light:
Applied Technology Finding an L4 Equivalent
By Chelsea D’Andrea
29 Flammability of Construction
and Building Textiles The AATCC blue wool standard is vital for testing
colorfastness to light, but one of the two dyes used to color
By Dwayne Sloan
the blue wool is now unattainable. This study examines a wide
For fabrics and films within a building, flammability codes range of acid dyes in search of a replacement dye with fading
refer to National Fire Protection Association (NFPA) 701. characteristics comparable to those of the L4 standard after
lightfastness testing.
Peer Reviewed
32 Low Pressure, Nonequilibrium- Cover Photo: Kathleen O’Toole ©2009
Plasma-Assisted Generation of Flame
Retardant Cotton
By Vladimir Totolin, Majid Sarmadi, Sorin O. Manolache,
and Ferencz S. Denes
Generating a durable flame retardant treatment by depositing
sodium silicate layers onto clean cotton substrates and
crosslinking them using oxygen plasma.

AATCC Review (USPS 020-179) is published monthly by the AATCC; ISSN 1532-8813; Copyright © 2009. Copying for other
10-Time than personal and internal use without the express permission of AATCC is prohibited. To purchase article reprints, contact
Award Winner Production Manager Kathleen O’Toole; +1 919 549 3543; otoolek@aatcc.org. To photocopy or use any copyrighted
material owned by AATCC beyond the fair use provisions of the US Copyright Act, submit requests to Copyright Clearance Center
Inc., www.copyright.com or info@copyright.com, specify code number: 1532-8813. For permission to republish articles appearing
in AATCC Review in another publication, contact Publications Director Diana Wyman; +1 919 549 3539 or
wymand@aatcc.org. Annual Subscription Price: AATCC members: US$55 (50% of individual dues); nonmembers: US$200. Single
Copy Price: $25 each within the US and US$35 each elsewhere. Missing Issues? Contact: Circulation Manager Kathleen O’Toole;
+1 919 549 3543; otoolek@aatcc.org. Periodicals postage paid at Durham, N.C. and additional mailing offices. Postmaster: Send
address changes to AATCC Review, P.O. Box 12215, RTP, NC 27709-2215, USA.
Disclaimer: Mention of any trade name or proprietary product published in AATCC Review does not constitute a guarantee
or warranty of the product by the AATCC and does not imply its approval to the exclusion of other products that may
also be suitable.

JUne 2009 AATCC Rev i e w 1

 Review®
Serving the Textile Industry with Publishing Excellence for 40 years.

One Davis Drive, Research Triangle Park, NC 27709, USA; +1 919 549 8141; www.aatcc.org
AATCC Review® is the official publication of the American Association of Textile Chemists & Colorists
(AATCC). AATCC is the world’s leading not-for-profit organization serving the interests of textile
professionals since 1921. It now reaches a global audience of professionals working in textile design, fibers and
materials, processing, quality control testing, and merchandising in more than 60 countries around the world.

Publications Director Advertising Sales

Diana Wyman Chris Shaw UK
wymand@aatcc.org +44 1606 833891; US +1 919 549 3547
(Editorial Inquiries/Letters to the Editor) shawc@aatcc.org
Production/Circulation Manager Advertising/Membership Coordinator
Kathleen O’Toole Sandy Thomas
otoolek@aatcc.org thomass@aatcc.org
Managing Editor Assistant Editor/Web Editor
Maria Thiry J. Michael Quante
thirym@aatcc.org quantem@aatcc.org
Publisher/Executive Vice President Peer Review Coordinator
Jack Daniels Ann Holland
danielsj@aatcc.org hollanda@aatcc.org

Editorial Advisory Board

Keith R. Beck, North Carolina State University (Chair)

Richard Aspland, Clemson University Aaron Johnson, Global Textile Network

Henry Boyter, Institute of Textile Technology
Philip Brown, Clemson University
Jan Cardamone, US Dept. of Agriculture
H.M. Choi, Soongsil University
Nevin Gursoy, Istanbul Technical University
Kathryn Hatch, University of Arizona
Jean Hoskin, Macy’s Merchandising Group
Nelson Houser, M. Dohmen
Kerry King, [TC]2
Kim Kitchings, Cotton Incorporated
Ann Laidlaw, X-Rite
Mary Ann Moore, Florida State University
Seshadri Ramkumar, Texas Tech University
James Rodgers, US Dept. of Agriculture
Harrie Schoots, Celanese Chemicals
Harold Freeman, North Carolina State University
(Colour Index Editorial Board, non-voting)

American Association of Textile Chemists & Colorists

President, Fred Cook, Georgia Institute of Technology
President-elect, Mike Tyndall, Cotton Incorporated
Immediate Past President, Martin Bide, University of Rhode Island
Treasurer, Charles Gavin, MFG Chemical Inc.

2 AATCC R e v i e w www.aatcc.org June 2009

Reach further

—be innovative!
At Huntsman, social and environmental responsibility is a founding philosophy
based on the platform of Responsible Care®. Our innovations are designed to
be sustainable—by minimising inputs whilst maximising benefits. We support this
sustainable innovation with a global network of technical experts. They focus on
working with our partners towards achieving maximum process and effect
performance with minimum environmental impact.

www.huntsman.com/textile_effects

Responsible Care® is a registered trademark of the International Council of Chemical Associations (ICCA)
 The Soapbox
Innovative measures are
needed at the shop floor
as well. Mission-linked,
is a communication goal-oriented research and
development endeavors
forum for AATCC have to be carried out by
members to discuss, all stake holders. Mission-
linked approaches will be
from their own based on solid science that
will lead to products that
perspectives, matters have enhanced value.
Enhanced-value products
of interest and are achievable if there is
importance in the active collaboration between
R&D institutions and indus-
textile industry. try. There are real payoffs
from such collective efforts
for all parties involved,
including intellectual property, which can be commercialized to
create returns for the inventor, academia, and the industry.
Knowledge-gaining and -sharing is critical for innovation,
and is made possible through networking opportunities provided

Innovation is by professional societies such as AATCC. Conferences and

knowledge-gaining opportunities provided by AATCC can serve as

the Way Forward
By Seshadri Ramkumar, Texas Tech University
Functional textile materials are on our television screens these
days. Blue and white face masks have become familiar, thanks to
the unfortunate swine flu outbreak. What does this scenario reveal?
Textile materials are no longer just banal apparel products. They
are required to have multifunctional attributes such as protection
and performance. In other words, 21st century textile materials
should have value-added properties and applications across the
entire supply chain.
The next phase of the textile industry is global- and perfor-
mance-oriented. The textile industry in developed economies is
adjusting to this shift. Even in developing economies such as China
and India, the industry is not immune to the changes.
Low price is not a trump card anymore for the textile sector
of growing economies, as competition has become global. Value-
addition is the need of the hour for segments of the industry—from
fiber to fashion.
The path forward for the textile industry is innovation. The
industry has to be nimble and cater to customer needs by investing
in process and product innovations. Our industry has to employ
multidisciplinary talents in developing products such as comfort
rich synthetics, light-weight military clothing, bug resistant filters,
and facemasks, to name a few.
a platform for initiating global collaborations. This is particularly
critical these days, when research investments are shrinking and
there is a need to share resources and gather outside knowledge.
AATCC has realized the importance of providing cost-effective
and high-quality knowledge-sharing platforms for its members
and interested parties via a number of outlets such as its AATCC
Review journal that carries cutting-edge peer-reviewed papers,
broad based industry articles, and valuable news items.
AATCC is unique as it supports the textile industry across the
entire supply chain through its Materials, Chemical Applications,
and Concept 2 Consumer (C2C) interest groups. These groups
organize specialty symposia to help the industry gain new knowl-
edge and connect people around the world.
As our industry marches towards the next stage, AATCC serves
as a partner to aid innovation and growth. Mission-linked innova-
tion is the way forward and we all have a role to play. Let us all be
active participants and lead our industry to a productive future,
marching alongside AATCC.
To share your views, send 500
words or less to Managing Editor
Maria Thiry at thirym@aatcc.org.

4 AATCC R e v i e w www.aatcc.org June 2009

 Peo ple
AATCC Welcomes New Members
joining in April 2009 . . .
By Sandy Thomas

GULF COAST SECTION, USA NORTHWEST SECTION, USA

Students: Kelly V. Rothstein, Cassandra J. Schirra, Senior: Michel B. McClung, program coordinator, Intertek,
Sarah L. White, and Kelly M. Whitenack—Texas State Oak Brook, Ill.
University, San Marcos, Tex. PIEDMONT SECTION, USA
INDIA SECTION Senior: Floyd E. Hull IV, plant manager, International Textile Group
Associate: Deepika Sahu, quality assurance executive, Pratibha (ITG), Boykins, Va.
Syntex Pvt. Ltd., Indore. Proposed by Srinivasan Srinivasan. SOUTHEASTERN SECTION, USA
KONGU SECTION, INDIA Senior: Julian Aramburo, design assurance manager, Jarden
Senior: K. A. Vijayakumar, senior executive, SGS (I) Consumer Solution, Boca Raton, Fla.
Pvt. Ltd., Tirupur. Senior: Roland L. Cantrell, quality control manager, Mohawk
MIDWEST SECTION, USA Industries, Dalton, Ga.
Senior: Jacqueline A. Beck, owner, Jacque Textile Designs Ltd., Senior: Sam L. Fortenberry, lab manager, Mohawk Home,
Lino Lakes, Minn. Dalton, Ga.
Senior: Ronald E. Sutton, dyehouse manager, Mohawk Industries,
Dalton, Ga.

JUne 2009 AATCC Rev i e w 5

Peo ple
STUDENT CHAPTERS
Philadelphia University, Pa., USA: Elizabeth Maura Kirk.
University of Massachusetts–Dartmouth, USA: Sagar G. Patel.
INDEPENDENT MEMBERS–WORLDWIDE
Senior: Md. Zahir U. Chowdhury, DCM (technical and
production), Clifton Group, Chittagong, Bangladesh. Proposed by
Amanur Rahman.
Senior: Juwel Das, senior executive, Pacific Jeans Ltd.,
Chittagong, Bangladesh. Proposed by Amanur Rahman.
Senior: Chandan Kumar Deb, printing, Apex International,
Chittagong, Bangladesh. Proposed by Amanur Rahman.
Senior: Md. Nazrul Islam, knitting and dyeing manager, Multifabs
Ltd., Gazipur, Bangladesh. Proposed by Amanur Rahman.
Senior: Roksana S. Jahan, research and development officer,
Fatullah Fabrics Ltd., Narayaganj, Bangladesh. Proposed by
Amanur Rahman.
Senior: Abdul Wadud Khan, quality manager, Purbani Fabrics
Ltd., Gazipur, Bangladesh. Proposed by Amanur Rahman.
Senior: Dewalagama Mahathge Chandika H. Kumara, DT
manager, Pacific Jeans Ltd., Chittagong, Bangladesh. Proposed by
Amanur Rahman.
Senior: Mohammad Mostafizur Rahman, owner, Printing
Pro Design (Pvt.) Ltd., Chittagong, Bangladesh. Proposed by
Amanur Rahman.
Senior: Kevser Korhan Tayhaz, group leader, Department of
National Defence, Ottawa, Canada.
Senior: Jianbin Wu, director—testing center, Shanxi Huajin Textile
and Dyeing Co. Ltd., Huncheng City, China. Proposed by Grace Xie.
Associate: Tawfa Mehereen Ahsan, quality control officer,
Esquire Knit Composite Ltd., Tejgaon, Bangladesh. Proposed by
Amanur Rahman.
Associate: Abul Mansur Fazle Habib, general manager, Shahan
Colours Ltd., Dhaka, Bangadesh. Proposed by Amanur Rahman.
Associate: Jorge L. Inche, director–graduate school, Universidad
Nacional Mayor de San Marcos, Lima, Peru.
Associate: Jinfeng Jia, design center director, Anhui Garments
Import and Export Co. Ltd., Hefei City, China. Proposed by
Grace Xie.
Associate: Yingying Jl, testing center operator, Shandong Zouping
Changshan Textile and Dyeing Co. Ltd., Shandong, China. Proposed
by Grace Xie.
6 AATCC R e v i e w www.aatcc.org
Associate: Yanyan Liu, deputy director, Shandong Binzhou
Yaguang Washcloth Co. Ltd., Shandong, China. Proposed by
Grace Xie.
Associate: Ferdues Ara Satter, production manager,
Tamishna Yarn Dyeing Inc., Dhaka, Bangladesh. Proposed by
Amanur Rahman.
Associate: Yanting Wang, design center, Anhui Garments Import
and Export Co. Inc., Hefei City, China. Proposed by Grace Xie.
Associate: Jia Xin, Esmod Fashion Design School, Beijing City,
China. Proposed by Grace Xie.
Associate: Yan Xiong, technical leader, Jiangsu Danmao Textile Co.
Ltd., Danyang City, China. Proposed by Grace Xie.
Associate: He Zhao, purchasing department director, Dalian
Fushan Garment Co. Ltd., Liaoning, China. Proposed by Grace Xie.
Associate: Jiangqin Zhou, Shanxi Huajin Textile and Dyeing Co.
Ltd., Yuncheng City, China. Proposed by Grace Xie.
Students: Carlos Daza Alvarado, Roxana Alva Bazan, Nancy
Borreda, Arnaldo Peňa Cabello, Doris Gladys Crisologo
Carmona, Jose Elias Da Silva, Gonzalo Javier Escobar, Nora
Felices Arana, Gregoria Galindo Samanez, Rosario
C. Orellani, and Suhail Sanchez Berrospi, Universidad Nacional
Mayor de San Marcos, Lima, Peru.
Student: Ozkan Yapar, Suleyman Demirel University,
Isparta, Turkey.
CORPORATE MEMBER
M/S UNIVERSAL JEANS LTD.
M/S Universal Jeans Ltd. is a garment manufacturer,
producing six million jeans, casual shirts, and jackets
for men, women, and children annually. The company
is based in the Chittagong Export Processing Zone of
Bangladesh and employs more than 4,000 people.
June 2009

A2

Fabric and Apparel

Student Design Competition
Winners Announced
More than 100 individuals and teams entered AATCC’s annual
Concept 2 Consumer (C2C) design competition. Students of all
levels and disciplines, from 38 different institutions, participated.
The theme for the 2009 competition was Color Concepts; each
entry was inspired by one of Pantone’s Winter 2008/09
color palettes.
First place winners receive a US$1,000 cash award,
complimentary student registration for the 2010 AATCC
International Conference (IC), and a Pantone Cotton Passport with
fabric swatches in nearly 2,000 fashion
colors. The winner of the Product Design
category will also represent AATCC on an all-
expenses-paid trip to Goa, India to compete
for the Society of Dyers and Colourists’
(SDC) International Colour and Textile Award.
Second-place winners get US$500 cash and
registration for the 2010 IC.

Fabric Design Winners

1st Place: Let Freedom Reign by Miranda
Shilati, Syracuse University
Miranda Shilati 2nd Place: Pattern in Architecture by Eleanor
Hoffman, North Carolina State University

Eleanor Hoffman

8 AATCC R e v i e w www.aatcc.org June 2009

 A2
Product Design Winners
1st Place: Footsteps Maternity by Erika Neumayer,
Dominican University
2nd Place: Sweet Snowflakes by Wesley Kathryn Woods,
Auburn University

Special Thanks
Thank you to everyone who offered their time
and expertise to judge the many excellent entries.
• Cindy McNaull, Invista
• Heidi Woodacre, Casual Male Retail Group
• Jean K. Dilworth, Eastern Illinois University
• Jeana Fitzgerald, Cotton Incorporated
• Kerry Maguire King, Textile Clothing Technology
Corporation [TC]2
• Mary Brannon, Fashion Institute of Design & Merchandising
• Susan Matter, Nordstrom Product Group
• Yvonne Johnson, Cotton Incorporated

Thank you also to Pantone for access to inspiration palettes

and providing some of the awards.

Look like fun? Guidelines for entering

the 2010 competition will be announced
shortly. Watch AATCC Review and
www.aatcc.org for announcements.

Erika Neumayer

Wesley Kathryn Woods

JUne 2009 AATCC Rev i e w 9

A2

Committee Meetings
Attract Global Participation
More than 100 attendees from several countries took part in the
most recent round of AATCC committee meetings. Meeting topics
ranged from test method development to Association operations.
A summary report of the business discussed by the Executive
Committee on Research (ECR) and the Technical Committee on
Research (TCR) will appear in the July issue of AATCC Review and
online at www.aatcc.org/testing/committees.
At the conclusion of the meetings, several awards were
presented for service to AATCC.

Fred Cook (left) accepts an honorary membership in the Society of Dyers and
Colourists “in recognition of the long and fruitful co-operation between the
Society and the American Association of Textile Chemists and Colorists.”
The award was presented by Martin Bide (right).

Adi Chehna was announced as the first recipient of the TCR

Service Award. A profile of Chehna and a description of the award
appear in the April issue (AATCC Review, Vol. 9, No. 4, p11).
Ashley Bradham also received her plaque as the 2009 Outstanding
College Graduate of the Year (see story, p12).
Most of AATCC’s work is performed by the volunteers who
serve on the various committees. The chairs of each committee,
ECR members, and the board of directors are instrumental in
guiding this work. Each member completing a term as chair or
board member in 2008 received a certificate of service. Many of
these dedicated individuals served multiple terms or on
multiple committees.

President Fred Cook presented a plaque to

Immediate Past President Martin Bide in recognition
of his 2007-2008 tenure as AATCC president..

R. Stephen (Steve) Simonson receives the 2008 Harold

C. Chapin Award for outstanding service to AATCC. It was
presented by selection committee chair Preston Aldridge.

10 AATCC R e v i e w www.aatcc.org June 2009

 A2
Certificates of Service
Ann C. Laidlaw Chair, Concept 2 Consumer Interest Group (2 terms) 2005-2008
Bert Truesdale Southern Regional Board Member (2 terms) 2005-2008
Chair, Membership Committee 2008
Brooks Tippett Chair, Henry E. Millson Award for Invention Committee 2008
Carol T. Revels Chair, RA36, Color Measurement 2006-2008
David L. Ramey Chair, RA31, Antimicrobial Activity 2006-2008
Freddy Miller MidSouth Regional Board Member 2005-2008
(2 terms)
Heidi Woodacre New England Regional Board Member (2 terms) 2005-2008
J. Preston Aldridge Chair, Harold C. Chapin Award Committee 2008
James E. Rodgers III Chair, RA103, Spectroscopic Technologies 2006-2008
Jayakumar Gopalakrishnan International Regional Board Member (2 terms)
2005-2008
Kanti Jasani Central Atlantic Board Member (2 terms) 2005-2008
Kerry Maguire King Chair, RA80, Printing Technology 2006-2008
Mary N. Brannon Executive Committee on Research 2006-2008
Paul L. Johnson Chair, RA56, Stain Resistance 2006-2008
Roy Bamford Western Regional Board Member 2005-2008
(2 terms)
Chair, Olney Medal Award Committee 2008
Chair, Employee Benefits Committee 2006-2008
Sandeep Khatua Chair, RA23, Colorfastness to Water 2006-2008
Stephen B. Brooks Chair, Chemical Applications Interest Group (2 terms) 2005-2008
Susan A. Gassett Chair, RA38, Colorfastness to Crocking 2006-2008
Todd M. Wernicke Chair, RA61, Appearance Retention 2006-2008

Missing Your Newsletter?

As of this May, AATCC News is emailed only to individuals who have specifically indicated their interest in receiving it.
If you would like to subscribe to this electronic newsletter, full of feature articles, technical information, and event updates,
send a note with “Subscribe” in the subject line to newsletter@aatcc.org. In May, you missed stories on vascular
textiles, clothing comfort for seniors, twisting terminology, and student connections. In June, it was textiles under the
upholstery, antimicrobial testing, and student award winner interviews.

JUne 2009 AATCC Rev i e w 11

A2
Ashley Bradham is
Graduate of the Year
Each year, schools with AATCC student chapters nominate deserv-
ing seniors for the Outstanding College Graduate of the Year award.
One of these students is selected to receive the recognition and
a US$1,000 cash prize. The 2009 Graduate of the Year award
was presented to Ashley Bradham at the recent AATCC Technical
Committee on Research meeting. As part of her applications,
Bradham submitted a personal statement about her accomplish-
ments as a student and involvement in AATCC. For more about
Bradham’s accomplishments, see her profile in the May issue
(AATCC Review, Vol. 9, No. 5, p11).
My name is Ashley Elizabeth Bradham and I am a senior at
North Carolina State University (NCSU), studying Polymer and
Color Chemistry. I am from Dunn, a small rural community in
southeast North Carolina. This community once thrived on the
textile industry, but suffered as the local plant closed, leaving
hundreds without jobs and other small businesses without an
economic basis for survival. As a student at NCSU, majoring in
Polymer and Color Chemistry at the College of Textiles, people
from home have questioned me about my decision to study a
field that they believe is a dead end. It has been my mission
to inform and educate the community about textiles and the
current and future opportunities it will provide. Since I have
entered the Polymer and Color Chemistry program, I have had
many opportunities to tell the people in my community more
about my major and they are always amazed at how large the
textile industry really is.
12 AATCC R e v i e w www.aatcc.org
SASMIRA Student
Chapter Inaugurated
By S. Radhakrishnan, Colour Publications
The formal inauguration of the student chapter at SASMIRA
(Synthetic & Art Silk Mills’ Research Association) Institute in
Mumbai, India was held on April 8. Welcoming the attendees at the
event Dr. G. S. Nadiger, AATCC India Region board member, gave
a brief background of the AATCC India Section and its activities in
India. Nadiger also gave details about the formation of the chapter
and explained the benefits available to the students. He encour-
aged them to come forward and actively participate in the chapter,
sharing their ideas and suggestions.
Later, a technical lecture on AATCC test methods was
conducted by Mr. K. Venkatarayan, AATCC India Section chair. Mr.
G. Jayakumar, former AATCC International Region board member
and current AATCC and ASTM accredited trainer and service
associate, said that the membership service center in India would
provide prompt service to all members. He also explained an
offer of complementary membership in ASTM International for the
members of AATCC.
Mr. Bashir Doctor, SASMIRA, assured full support to the student
chapter and offered suggestions on the type of program and
lectures that could be arranged by the AATCC India Section for the
benefit of the students.
L-R, standing: Dr. Anand Modgekar (Faculty, SASMIRA), Dr. G. S. Nadiger, Mr.
K. Venkatarayan, Mr. Bashir Doctor (Principal I/C, SASMIRA). Seated: student
committee members.
June 2009
Keep Dye in the Bath—
and Out of the Air
Airborne dye dust can be Additional Collars (50):
dangerous, unhealthy, and a Item #08727
waste of resources. In less
than five minutes, you can Replacement Rating Scale:
determine which powder Item #08725
dyes may require
Evaluation of Dusting
extra care.
Propensity of Powder Dyes:
The Dye Dusting Apparatus TM170
is a specially-designed
www.aatcc.org/products
metal cylinder and funnel
phone +1 919 549 3526
set, 20 paper collars, and a
fax +1 919 549 8933
photographic rating scale.
jonesb@aatcc.org
Item #08726
Mark Your Calendar! Collaborative Design
Symposium Brings
July 31
Visual Gray Scale Color Change Academia and
Evaluation Proficiency Registration Due
www.aatcc.org/programs/prof
Industry Together
Connecting through Creativity, Technology,
August 12-13 and Business: Designers and Product Developers
Design and Product Development Symposium: Meet the Challenge Symposium
“Connecting through Creativity, Technology, and Business” August 12–13
www.aatcc.org/programs/workshops/0809designer_symp.cfm Philadelphia University
Three industry leaders, AATCC, [TC]2, and Philadelphia University,
August 14 are jointly sponsoring a symposium for professionals in the design
Fiber Identification Proficiency Registration Due and product development field. The program will bring together a
www.aatcc.org/programs/prof diverse range of individuals from the textile, apparel, home
furnishings, and related soft goods industries.
September 4
Appearance Proficiency Registration Due Philadelphia University
www.aatcc.org/programs/prof Philadelphia University is the oldest, and the only private,
institution of higher education in the US offering instruction and
September 30 – October 1 research supporting textile, apparel, and related industries.
Color Workshop This two-day program will be held at the newly-opened,
www.aatcc.org/programs/workshops/colormgt.cfm high-tech Tuttleman Center.

October 26-27
Innovations in Functional Materials, Sports & Defense Technologies,
and Composites Symposium; NTC Forum
www.aatcc.org/programs


Ongoing
UV Calibration Registration
www.aatcc.org/programs/calib


Test Method Training
www.aatcc.org/programs/global

Textile Fundamentals e-Learning


www.aatcc.org/programs/workshops/eLearning-text.cfm

June 2009

Keynote Speaker: Suzanne Tick
Suzanne Tick Inc. specializes in material development for
commercial and residential interiors including textiles, hard surfac-
ing, carpet, woven metal screens, and lighting. Tick’s presentation,
“Revolution Reality: Paralleling the Design Revolution of the Sixties
with Today” is an investigation of the parallels between the social
and design revolutions of the 60s era and the realities of today. The
concepts of super graphics, transparency, diffusion of light, tectonic
structures, modular thinking, contemplative fields, the hand, and
the machine are explored.
Tick has been design director, and created product, for several
high profile contract and residential fabric and carpet companies.
She has received numerous awards and participated in several
museum exhibitions with her work. Most recently, she was one of
10 inaugural recipients of the 2006 Women in Design award. Tick
received her BFA in woven design from the University of Iowa and
an associate degree in Applied Arts from the Fashion Institute of
Technology. She has been a member of the board of directors of
the Museum of Arts and Design, New York, N.Y., USA since 2007.
JUne 2009 AATCC Rev i e w 15
A2
Networking
In addition to more than 20 speakers, you will have the
opportunity to network with other professionals in the design field
and discuss technologies and business strategies that support
innovation, creativity, and sustainability in the development process
for soft goods.
Early-bird Discount
Sign up by July 28 to save US$50 off your registration fee!
Students—you pay only US$125. Take advantage of this profes-
sional opportunity while classes are out for the summer. For
registration or a complete list of presentations, visit
www.aatcc.org/programs.
Communicate Color
across Your Supply Chain
Color Management Workshop
September 30 – October 1
AATCC Technical Center
This workshop offers much more than just the basic principles of
color and lighting. Find out what you should consider when you
develop a color palette and how your choices affect cost, fashion,
durability, and dyeing reproducibility. Learn how to implement a
digital color program with suppliers, organize and manage color
data, and integrate the color process into PLM systems. Plus, have
YOUR questions answered by experts in color measurement and
communication. If you work in color approval, design, merchandis-
ing, manufacturing, product development, or retail, don’t miss this
opportunity! Attendance is limited so register early.
Break-out sessions will focus on illumination and observer
issues, sample analysis and measurement technique, creativity
with trends and virtual development, understanding color matching,
production evaluation and control, and execution of computer color
matching in the lab and in production. Presentations include:
• Fundamentals of Color Theory and Measurement, David Hinks,
North Carolina State University
• Color Trends and Forecast, Cotton Incorporated
• Color Choice: A Balancing Act between the DNA of the Dye and
Requirements, Donna D. Faber, JCPenney
• Describing Color Differences: How Good are Your Comments?
Carol Revels, Gap Inc.
• Color Communication: Getting Your Message Across, Roland L.
Connelly Sr., X-Rite Inc.
• Supplier Conformance: Why Don’t my Numbers Match Yours?
Ken Butts, Datacolor
• Tracking Color Performance, Keith D. Hoover, JCPenney
• Integration: Bringing it All Together, Speaker to be Announced
Visit www.aatcc.org/programs to reserve your spot.
A2
NTC Forum Joins AATCC
Materials Symposium
Innovations in Functional Materials,
Sports & Defense Technologies, and Composites Symposium
October 26-27
Hyatt Regency, Greenville, S.C., USA
Textile Education
on YOUR Terms
You decide when and where to learn with Textile Fundamentals
from AATCC and the TexEd department of North Carolina State
University. With 14 modules to choose from, you even control what
you learn. Textile Fundamentals is an online learning experience
with the advantages of a “hands-on” environment. Videos, digital
simulations, and detailed diagrams let you see and understand
each process. Save time and money—purchase only the modules
you need; no travel; no overnight stays. For a free preview, visit
www.aatcc.org/programs/workshops/eLearning-text.cfm.
16 AATCC R e v i e w www.aatcc.org
The annual National Textile Center (NTC) Forum will be held in
conjunction with AATCC’s fall symposium. The NTC Forum will
include a half-day poster session and opportunities to interact with
NTC faculty and students throughout the event. The poster session
will include currently-funded NTC projects on a variety of topics.
Project participants will be available for discussion and develop-
ment of technology transfer possibilities. The NTC Student Paper
Competition will also be part of the program.
Visit www.aatcc.org/programs for updates.
Modules includes:
• Fundamentals of Fibers
• Spun Yarn Manufacturing
• Texturing Fundamentals (Coming Soon)
• Fundamentals of Warp Preparation
• Fundamentals of Weft Knitting
• Fundamentals of Warp Knitting (Coming Soon)
• Weaving Fundamentals
• Fundamentals of Nonwovens
• Fundamentals of Fabric Preparation
• Color and Color Properties
• Dyestuffs and Dyestuff Applications
• Printing Fundamentals
• Chemical Finishing
• Mechanical Finishing
June 2009
 Sections
Delaware Valley

Section
Janet Brady +1 215 951 2757
bradyj@philau.edu

News Gulf Coast

Ioan I. Negulescu +1 225 578 1684
inegule@lsu.edu
Kongu
As the Kongu officers Hudson Mohawk
planned their April event, Raj Suhag +1 315 429 8551 ext. 212
they realized the economic rsuhag@gehringtextiles.com
climate would be a chal- India
lenge. They chose to K. Venkatarayan +91 982 185 1870
focus the program on the k.venkatarayan@gmail.com
Vivek Naidu, vice president customer economy itself, bringing
relationships, CitiBank, involved the Kongu
speakers from retail, Madhusudhana P. Reddy
audience in his discussion of the bankers’
perspective on the economic crisis. export, and banking sectors +91 421 4305555
Courtesy of Madhusudhana “Reddy” together at the Hotel pm.reddy@sgs.com
Ponakaladinne.
Gayathri in Tirupur, India.
Midwest
Yiqi Yang +1 402 472 5197
Northwest yyang2@unl.edu
The April 7 meeting in Portland, Oreg., USA featured a
presentation by Membership Services Director Birgit Patty. New England
Larry Bond, global sales manager for Atlas Materials Testing, Norann Warner +1 508 638 1793
concluded the meeting with his discussion of the “Fundamentals norann.warner@moderntestingservices.com
of Weathering.” Bond explained that light (quality and quantity), Northwest
water (quantity and phase), and heat (quantity and cycles) are the Nancy PeBenito +1 503 671 5825
three primary parameters to calculate for accelerated laboratory nancy.pebenito@nike.com
weathering, but secondary environmental parameters like gases
Pacific
(ozone, carbon monoxide, and sulfur dioxide) need to be considered Martin Bertalanitsch +1 704 561 3000
as well. He warned that a test should not be accelerated beyond bertalanitsch.martin@dystar.com
the point of correlation with real, outdoor weathering. “The faster
the test, the more likely it won’t correlate.” Factors that decrease Piedmont
correlation include: Kevin Jenkinson +1 704 841 2111
• Short wavelength exposure kjenkinson@carolina.rr.com
• High intensity exposure
• Continuous exposure to light
Interest Groups
Chemical Applications
• Unrealistic specimen temperatures
Peter Hauser +1 919 513 1899
• Unrealistic or non-existent temperature difference between
chemapps@aatcc.org
materials of different colors
• Unrealistic or non-existent moisture delivery Concept 2 Consumer
Mary Brannon +1 213 624 1200 ext. 3026
Upcoming Northwest Section Meetings c2c@aatcc.org
July (date to be determined) Seattle, Wash., USA
October 5 Portland, Oreg., USA Materials
Philip Brown +1 864 656 6072
New England materials@aatcc.org
About 50 people attended the March meeting to hear about “China
and the New Economy.” Nearly 300 are expected to turn out for the Membership Services
June golf outing. India, South, and Southeast Asia
Jayakumar Gopalakrishnan
Upcoming New England Section Meetings +91 938 502 2238
October 2 Roland Derby Color Series assist@aatcc.org
New England Regional Technical Symposium
November 20 Technical Meeting & Social Madhumitha Dinesh (Madhu)
+91 44 2615 1791
assist2@aatcc.org
JUne 2009
Too Many Job Applicants?

AATCC CareerSite is the answer!

Focuses specifically on textiles
• design
• materials
• processing
• testing

Reach serious applicants—

visit www.aatcc.org/career/career.cfm.

 A2
Outstanding Student Josh Ward,
Apparel-Derived Phthalates in Wastewater:
Research Proposals Evaluating the Need for Environmental Concern
Josh Ward, a Biochemistry major at Philadelphia University is
Funded by AATCC already conducting research
on “chemicals of concern”
Foundation and ITT. in children’s apparel. Ward
evaluated the phthalate levels
Two students were selected to receive the first round of in children’s apparel with
AATCC Foundation/Institute of Textile Technology (ITT) undergradu- embossed plastic decals,
ate research grants. The funded projects will be completed by detecting concentrations up
December 2009, with results presented at the April 2010 ITT to 3.5%. With the AATCC
annual meeting. Foundation/ITT grant, he will
expand his research with the
Kathleen M. Donley: Manufacturing of goal of assessing the degree
to which these phthalates are
Glass Nanofibers using Polymer Precursors for
liberated from apparel products
Fire and Thermal Protection Applications during the laundering process.
Kathleen (Katie) Donley is active in multiple academic, professional,
Ward’s research advisor and
social, and athletic groups at Cornell University where she is study-
department head, Jeffrey Ashley says, “very little research has
ing Fiber Science, with a concentration in Law and Society. Donley
been performed on this issue. This research would allow environ-
has worked as an intern for the International Trade Association and
mental scientists and engineers to assess whether there is need
CW-X Conditioning Wear. She also performed research for Cornell’s
for concern regarding the release of these potential contaminants
Human Ecology Research Group and G3I Technologies. Professor
in the waste stream.”
Juan Hinestroza says,
Public concern over toxic substances in consumer products has
Donley’s current research in
greatly increased in recent years. Ward explains, “Phthalates, a
glass fibers for fire protection
specific class of organic compounds used primarily as plasticizers
“may open a new and safer
in toys and clothing, have been identified as toxicants and linked to
avenue to produce fibers
a variety of reproductive problems, allergies, and eczema, particu-
capable of resisting higher
larly among children. Naturally, the question then arises as to the
temperatures. We anticipate
fate of these chemicals during the washing process. Phthalates are
that her findings will be
likely liberated from apparel products during laundering processes
highly relevant to the textile
and subsequently enter waste streams, ultimately accumulating in
and fiber community.”
receiving water bodies such as rivers.”
In Donley’s own words,
Ward’s research will allow him to calculate the concentrations
“The goal of the proposed
of phthalates that may enter waste waters and evaluate whether
research is to form glass
levels are high enough to be of environmental and human
nanofibers from polymer-
health concern.
ceramic precursors through
reactive electrospinning.” The
project is broken into four steps:
1) Identifying precursors that may be used to form
glass nanofibers
2) Creating a reactive electrospinning reactor
3) Electrospinning the polymer-ceramic nanofibers
4) Transforming the polymers into ceramic nanofibers Rising Juniors: Plan now to apply for 2010 grants!
via thermal treatment September 2009: Areas of interest announced
Donley predicts that glass nanofibers electrospun from polymer December 1, 2009: Proposals due
precursors will have high surface areas and the potential to January 2010: Funding dispersed
withstand extremely high temperatures. She also hopes to gain December 2010: Research complete
fundamental insights about high-temperature fiber formation February 2011: Final report due
processes through the proposed work. April 2011: Presentation at ITT

JUne 2009 AATCC Rev i e w 19

Ind ustry News

Textile Institute to Merge with SCI?

By the time you read this, the vote will have been taken at The Textile Institute’s Extraordinary General Meeting on May 14, and the
matter will be decided. At stake? The proposed merger of The Textile Institute (TI) with the Society of Chemical Industry (SCI). This pro-
posal “is possibly the most important issue raised since [the] formation of the Institute nearly 100 years ago,” says David Woolliscroft,
secretary of TI.
The SCI is composed of members from many chemical sectors as diverse as food, pharmaceuticals, biotechnology, and environ-
mental science. Established in 1881, the UK-headquartered society has individual members in more than 70 countries and offices in
the US, Canada, Australia, India, China, and Europe.
Several members of TI opposed the merger, saying that “the common thread and interest to all the membership is textiles, and we
believe that most members want this to continue and not be subsumed into an organization with no history or experience of textile
materials and manufacture.”
Under the terms of the merger, the TI Board would be elected by the TI membership; the TI Board will nominate a minimum of two
members to the SCI Board. After the merger, policy governing the TI would be set by the SCI Board (including the TI representatives).
However, “we’ll keep our own qualifications, our own publications, and our bi-annual textile conference as is,” says TI Council Chair
Subhash Anand.
“SCI approached us for the merger because we have a great synergy and complement each other,” says Anand. “Their members
will be able to become members of the Institute. They also want to expand into smart materials and performance materials, areas
where the TI is already strong.”
Andrew Ladds,
CEO of the SCI, says
that the merger
would benefit SCI
through “a greater
combined critical
mass of membership
and reach,” and a
“close synergy with
a complementary
sector.” He notes that
“The TI’s specialized
Diplomas Committee
(accreditation) is
sacrosanct and
would be retained in
its correct form.”
“The SCI is com-
mitted to investing
money to help us
grow,” says Anand.
“The Board and
Council of the TI feel
there is a synergy
with SCI. We want
to merge because
Andrew Ladds, SCI and Subhash Anand, TI. we want to flourish.”
If TI members vote
against the merger
with SCI, Anand says that the TI Board and Council will have to seek out another organization for merger. The TI’s financial situation is
such that, Anand says, “We sincerely feel that if we do not merge with another organization, we will not survive.”
For further updates on the decision, visit the TI website: www.texi.org

20 AATCC R e v i e w www.aatcc.org June 2009

 Ind ustry News
Temperature Control for Textiles
Bet you’ve never thought of controlling temperatures
with vegetable oil. Eric Lindquist, president of Entropy
Solutions and developer of PureTemp phase change
materials has. Phase change materials (PCMs)
maintain set temperatures by changing phases from
liquid to solid or vice versa, depending on external
temperature conditions. Performance and precision of
PCMs are tied to the purity level of the material—how
highly refined they are—according to Lindquist. Most
PCMs are petroleum-based, with a maximum purity
level of 85%. Lindquist says the vegetable-oil-based
PureTemp can reach a purity level (and therefore,
performance and temperature precision level) of 99%.
In addition to purity, PureTemp has a broader
range of set temperatures than petroleum-based
PCMs. “With petroleum molecules you’re limited to
approximately 20 different temperature ranges,” says
Lindquist. “PureTemp has a 210-degree temperature
range, from -40F to 310F.” So if something needs
to be kept very warm, or very cold, despite external
temperatures, that is now possible. The PureTemp
PCM can keep food and medication cool without
refrigeration. Different vegetable oils are used to
achieve the various temperature ranges.
Compared to standard PCMs, the vegetable-based
PCM is a green, renewable resource, which is highly
biodegradable. And, says Lindquist, an additional
benefit is the price stability of vegetable oils compared
to petroleum products. The vegetable oils are treated with a natural chemical process to eliminate oxygenation and prevent them
from going rancid. “The material performs the same every time,” says Lindquist. “We’ve tested 20,000 plus phase changes with zero
degradation in performance.” The new PCM is available in multiple forms—liquid, micro-encapsulated, and macro-encapsulated, and
can literally be “woven” into fabric.

Dangerous Components of FRs Defined

Certain brominated substances previously used in flame retardants (FRs) were recently added to the Persistent Organic Pollutants
(POPs) list maintained by the Stockholm Convention. The Convention is an international agreement of the United Nations
Environmental Program with the goal of identifying, evaluating, and eliminating POPs from the environment.
Commercial Penta-brominated diphenylether (Penta-BDE) was used as an FR in flexible polyurethane foam until most production
was voluntarily stopped in 2004. The Convention decided to list only the Tetra-BDE and Penta-BDE components of the commercial
mixture as POPs. Other constituent ingredients were not found to be POPs or precursors to POP formation. Hexa-BDE and Hepta-BDE
components of commercial Octa-BDE mixtures (used as FRs in electronic and electrical equipment) were also added to the list.
For more about restricted and dangerous substances in textiles, see the feature article, “Protecting the Brand” on p22.

Spread the word! If you have news or innovations of interest to textile professionals
around the world, send details and photos to Maria Thiry at thirym@aatcc.org.

JUne 2009 AATCC Rev i e w 21

Protecting
By Maria C. Thiry
 Fea ture
W
hen you hear about a textile “protecting” something, your thoughts probably go to
a firefighter’s uniform, or a soldier’s battle vest. You likely didn’t consider a humble
baby’s blanket, or an everyday t-shirt doing much in the way of protection. But those
common fabrics protect something every day—their brands’ reputation for selling safe, quality
goods. If that baby’s blanket is found to contain chemicals that irritate an infant’s skin, or that
t-shirt was processed with chemicals believed to cause cancer, then the reputation of the brand
that sold that product may be irreparably damaged.
“Brand reputation is everything. Once a brand loses its reputation, it costs a lot of time and
money to earn it back,” says John Eapen, vice-president of environment, health, and safety for
American & Efird, and chair of the American Apparel & Footwear Association (AAFA)

the Brand
environmental committee.

Protecting the Consumer

In this era of global sourcing, how do brands protect their precious reputations? The way many
companies protect their reputations is by specifying a restricted substances list—a list of chemical
substances they don’t want used in the manufacturing of their product—and using only suppliers
that comply with that list.
To protect consumers, governments around the world have banned the presence of suspected
harmful substances in finished products. Seemanta Mitra, director of technical services for testing
lab Intertek, notes “Many companies go above and beyond government regulations to ensure a
safe product for the consumer.”

JUne 2009 AATCC Rev i e w 23

BANNED SUBSTANCES
Charts courtesy of Hohenstein Institute.
“In principle, it must be said that most
textiles, garments, and fabrics, are
safe products and that most produc-
ers and traders [put] many efforts
into testing their products to be sure
that they [are] safe products,” says
Manfred Hartmann, researcher at the
textile research and testing labs of the
Hohenstein Institute.
And you can’t guarantee product
safety by using all-natural substances. Just because a substance
is considered “natural,” that’s no guarantee of its safety, says
Manfred Wentz, head of Oeko-Tex Certification Body (USA).
“Several ‘natural’ dyes or plants can be hazardous,” he notes.
“Natural does not equal safe. And synthetic does not
equal unsafe.”
Any substance can be harmful in sufficient quantities—water
is typically considered beneficial, but too much water and you’ll
drown. Even substances considered harmful above certain con-
centrations will be safe below those concentrations. It’s all about
threshold limits or unit risk numbers, says Wentz.
There’s also the matter of risk perception. “Risk perception
often drives [banned chemical] requirements rather than actual
risk,” says Wentz. “You must have context to analyze the real risk.
If some chemical compound is thought to cause five cases of
cancer per million, when the typical rate is one case per million,
the media will say that the compound causes ‘five times’ as much
cancer. But in truth, the actual rate is still very small.” In the case
of some chemicals, the benefits they bestow may be worth the
increased risk if there is no suitable alternative.
24 AATCC R e v i e w www.aatcc.org
”
Why Are Certain Substances Banned?
“Restricted substances are chemicals and other materials which
have been banned or otherwise restricted by legislation or by
brands in a particular manufacturing process,” says Mitra. The
substances restricted by government regulation are those believed
to present a substantial environmental, health, or safety risk
According to Ellen Roaldi, senior technical consulting specialist
at testing laboratory Bureau Veritas Consumer Products Services,
“Exposure to the substance will present a health hazard generally
in the form of a carcinogen, toxin, or sensitizer.” She notes that
restricted chemicals found in textiles often come in direct skin or
human contact and therefore present higher risks.
Threshold limit quantities are different for different
chemical substances. “These levels are [established] based on
research for the dosage level found harmful to living beings,” says
Nagaraj K., laboratory manager at TUV SUD South Asia Pvt. Ltd. “All
these regulations are driven by the case studies available on the
effects of certain substances to the human body,” he says.
“Repeated exposure is an issue as well,” Eapen says. Workers
may be more at risk from repeated exposure than consumers.
Some substances are restricted during textile production, while
other substances are allowed in production but their traces are
June 2009

“ ”
Charts courtesy of Hohenstein Institute.
” Chromium (III), and Chromium (VI). In textiles and
restricted in the finished fabric, says Nagaraj. So, some substanc-
es are banned to protect workers, others to protect consumers, or
sometimes both.
Which Substances Are Banned?*
*This list is not conclusive. Chemicals listed do not reflect all countries’
limits or bans. Thanks to Seemantra Mitra of Intertek and Ellen Roaldi of Bureau
Veritas for their assistance with this list.
Azo dyes are used to dye leather and certain fabrics. According to
Mitra, some of the amines cleaved from azo colorants are potential
carcinogens. Azo dyes are restricted in the European Union.
Alkylphenolethoxylate (APEOs) are a group of nonionic
surfactants used in leather tanning and in silk production. APEO
can also be present in some dye and pigment preparation and
in some polyester padding and down fillings. According to Mitra,
JUne 2009 AATCC Rev i e w 25
the surfactants’ anaerobic degradation are non-
ylphenols, which are thought to have effects on the
human hormonal system and fertility, as well as
being possibly carcinogenic and mutagenic.
Cadmium is a naturally occurring and abundant
metal often used for textile pigments, especially red,
orange, yellow, and green; and used as a coloring
agent for textile, leather, and plastic products.
It is thought to be carcinogenic, and to cause
reproductive problems, DNA damage, and damage
to the central nervous system. It is restricted in The
Netherlands and completely banned in Sweden.
Chromium is a naturally occurring metal.
It’s found in three main forms: Chromium (0),
apparel, chromium can be found in plastics, pig-
ments, and tanned leather. Cr (VI) and certain Cr
(VI)- containing compounds are corrosive and known carcinogens.
The use of chromium is restricted in Germany in leather.
Disperse dyes are a class of water-soluble dyes used for
synthetic or manufactured fibers (polyester, acetate, and nylon).
Some disperse dyes are suspected to cause allergic reactions.
They are restricted in Germany.
Flame retardants (FRs) are chemical compounds used to
prevent or control burning in fabrics. Various FRs can be found in
children’s sleepwear, upholstered furniture, protective clothing,
and tent fabrics (in coatings). Some flame retardants such as
Tris(hydroxymethyl)aminomethane (TRIS), Polybrominated biphenyl
(PBB), and Pentabromodiphenyl ether, Octabromodiphenyl ether,
and Decabromodiphenyl ether (penta-, octa-, and deca-BDE) are
thought to be persistent in the environment, and also suspected
of affecting the human immune system. TRIS is banned in the US,
Fea ture
and many US states ban penta-, octa-, and deca-BDE FRs. Europe
and Japan restrict or ban several FR substances. Trichloroethylene is also listed as a cancer-causing chemical under
Formaldehyde is a volatile compound released by some textile
finishes, such as those imparting wrinkle resistance. It is of par-
ticular concern when the garment is new. Formaldehyde-containing
finishes are most likely to be used on fabrics that otherwise crease
easily, such as cotton or wool. It’s an irritant to eyes, nose, lungs,
and mucous membranes; may cause headaches, difficulty breath-
ing, trigger asthma, and allergic reactions; and is a suspected
carcinogen. Formaldehyde is regulated in Japan, Norway, and
Finland, and the US Consumer Product Safety Commission has
begun a study on formaldehyde in textiles.
Heavy metals include antimony, arsenic, barium,
and selenium, which are thought to produce negative effects on
human health. They are associated with synthetic fibers and can
also be found in clothing trim and accessories..
Lead is a naturally occurring metal that may be found in plas-
tics, paints, inks, pigments, and metal components. Lead and its
compounds are thought to be carcinogens. It can affect the central
nervous system (particularly in children), and damage the kidneys
and immune system. Lead is regulated in the US for certain
product classes, both in substrates and in surface coatings.
Nickel is a naturally occurring metal, often combined with other
metals to create alloys with increased hardness and resistance
to corrosion. Nickel can be found in clothing trim and accessories
such as snaps, buttons, and zippers. It can cause allergic reactions
and is a suspected carcinogen. Its use is restricted in Europe.
Organotin compounds combine tin and organics such as butyl-
and phenyl groups. Organotin compounds can be found in biocides
(antibacterials), plastics, inks, paints, and heat transfer materials.
They are suspected to be endocrine disrupters and are restricted in
Japan and South Korea.
Organic solvents are used for textile finishing, cleaning, and
printing agents, and in other processes where they are needed to
dissolve and dilute fats, oils, and adhesives. They are also used in
consumer aftercare of garments, such as for drycleaning. Organic
solvents are highly volatile, and many are thought to harm human
health. According to Mitra, “Trichloroethylene [sometimes used as
a degreaser or drycleaning agent] is a chlorinated hydrocarbon,
a cancer-causing agent, and is in the top 15 priority pollut-
ant list compiled by the US Environmental Protection Agency.
California’s Proposition 65.” Japan restricts tetrachloroethylene,
perchloroethylene, and both Germany and Japan restrict pen-
tachloroethane; carbon tetrachloride; 1,1,1,2-tetrachloroethane;
1,1,2,2-tetrachloroethane; chloroform; 1,1,2-trichloroethane;
1,1-dichloroethylene; and 1,1,1-trichloroethane.
Pentachlorophenol (PCP) is a polychlorinated compound
used as a preservative and antifungal in textiles and leather prod-
ucts. PCP is thought to cause cancer and its combustion releases
dioxins. The use of PCP is restricted in Switzerland and Germany.
Traces of pesticides are sometimes found in natural fibers
(typically cotton), especially Dieldrin and DTTB that may have been
applied to natural fibers during growth and storage. Pesticides can
be absorbed through the skin, and some are suspected carcino-
gens. Pesticides in textiles are regulated in Japan and Switzerland.
Phthalates are added to plastics to increase their flexibility,
and can be found in garments with flexible plastic components,
trim, and screen prints. Some phthalates are considered to affect
the neurological system, disturb the hormone system, and are
suspected carcinogens. Certain phthalates are regulated in Europe
and the US.
Polyvinyl chloride (PVC) is a thermoplastic that can be soft
or hard, transparent or colored. PVC can be found on garments
in findings, trim, and coatings. PVC can often be found in screen
prints and inks. Many of the compounds involved in PVC produc-
tion and in PVC products are toxic or suspected to be toxic. PVC
items are environmentally persistent, and their manufacture and
disposal often results in highly toxic wastes such as dioxins. PVC is
regulated for certain product classes in some states in the US.
PROTECTING CONSUMERS
How do retailers protect their customers (and their own reputations)
from possibly harmful substances? “Material specification and a
comprehensive auditing scheme are the most important tools the
supply chain has for ensuring material integrity,” says Joe Walkuski,
president of compliance software company TEXbase. He says that
specifications are typically used to control quality, but they are
also a perfect tool for controlling what substances are—and are
not—used on fabric and trim. “A properly-defined specification

will dictate what happens in production,” says Walkuski. But what
should go into those specifications?
To protect themselves, retailers must research which sub-
stances are considered a risk. “Retailers sell internationally. It’s a
good thing to know about banned substances all over the world,”
says Ellen Uyenco, manager of product safety and reliability for
retailer Williams-Sonoma. She says that it’s important that retailers
research beyond the minimum local requirements. “You never know
when regulations may change or become more strict,” Uyenco
says. “For example, many retailers and manufacturers weren’t
prepared for the Consumer Product Safety Improvement Act’s
(CPSIA’s) new requirements, and it cost them more money
for testing.”
Walkuski says that a comprehensive approach to materials
development is paramount to developing compliant products, and
the evaluation of each component is critical. “If you’re vigilant on
the individual pieces throughout the product development process,
you logically end up with a compliant product,” he says. “If a
company fails to pay attention to the product development process,
then they will always be reactive to regulatory changes. Conversely,
if a company is already managing data correctly and already has
their product development under control, complying with legislation
like CPSIA is much less of a challenge.”
According to Nagaraj, different retailers adopt different strate-
gies to monitor the quality of the products throughout the process,
whether by testing, process audits, or getting a letter of guarantee
from material suppliers. He says that retailers sometimes specify
particular material suppliers so quality will be uniform throughout
the supply chain and testing can be streamlined. Uyenco says that
her company requires its vendors to seek third-party certifications,
such as Oeko-Tex.
Restricted Substance Lists
As one way to control high-risk substances, many companies adopt
restricted substance list (RSL) programs that limit the exposure of
consumers to particular substances and also limit the substances’
impact on the environment, says Roaldi. “The purpose of an RSL is
to clearly set forth for suppliers those chemicals that are restricted
or banned from finished products,” says Mitra. RSLs have been
adopted as part of companies’ corporate sustainability and social
Fea ture
and environmental responsibility practices. “Managing the risk
of using these chemicals…has been adopted as part of ‘best
practices’ for the textile industry,” says Roaldi. “Companies publish
RSLs to ensure that suppliers and vendors, as well as corporate
officials, understand restricted substances requirements.”
Retailers handle RSLs through three main avenues:
AAFA RSL The American Apparel & Footwear Association (AAFA)
maintains an RSL available to the entire industry on its website.
“The goal is to make [the RSL] as common as possible, and not
too cumbersome or unwieldy,” says Eapen. “Today, nobody makes
a product just to sell in Europe or North America; they want to sell
all over the world.” So the AAFA designed its RSL to have a global
scope—it lists banned chemicals along with which countries have
relevant regulations and the maximum threshold limits established
for those substances. The list is updated every six months. The
AAFA RSL lists regulated chemical substances, but leaves testing
and compliance up to the manufacturers.
According to Eapen, the benefits of the AAFA RSL are that “It’s
an industry-wide list. A supplier can refer to one list, rather than
trying to keep up with 50 different customer lists. All the chemicals
on the list are restricted in one country or another. If a chemical is
restricted in more than one country, the AAFA list reflects the most
stringent regulatory limits.”
Eapen says that the AAFA RSL committee is a nine-person
task force that meets every six months to review the list. “The task
force has representatives from international laboratories, OekoTex,
manufacturers, and brands. Representatives include individuals
from Asia, Europe, and North America,” says Eapen. He says that
every six months, the RSL is reviewed by a peer group of non-AAFA
organizations, and then by the 100-member AAFA
environmental committee.
Apparel & Footwear International RSL Management
Working Group (AFIRM Group) is a group of 13 large brand
name companies that deal with RSL issues together, although each
company has its own RSL. The companies include Ann Taylor, Gap
Inc., H&M, TESCO, REI, Puma, Nike, New Balance, Levi Strauss
& Co., C&A, Adidas, Timberland, and s. Oliver. The companies of
AFIRM have regular meetings where they discuss RSL issues.
AFIRM has developed a toolkit that describes where the restricted
chemicals can be found, a flowchart for implementation, a factory
Fea ture

chemical management plan, and RSL testing. AFIRM has held RSL
seminars in several countries.
Private RSLs Some companies, like Marks & Spencer, have
their own private RSLs apart from any organized group. “Some
companies have their own private lists because they started on
this path a long time ago and have had their list a long time,” notes
Eapen. “Other companies have their own list because they have a
broad range of products in addition to apparel and footwear.”
Some RSLs also include a “best practices” list, which catalogs
chemicals that might be banned in the future. AFIRM has a best
practices list and AAFA is also planning to include one in a separate
section of its RSL says Eapen.
So far it all sounds very cut and dry. Keep an RSL, or borrow the
AAFA’s industry-wide one, and require all your vendors to comply
with it. So why do government groups or the media report incidents
of formaldehyde in dress shirts or lead in children’s clothing? “Part
of the problem is some of the smaller companies haven’t caught
up yet,” says Roaldi. “They don’t have the money or resources to
manage an RSL, so they just focus on an individual country’s local
requirements.” She also notes that sometimes these issues occur
because the supplier changes the raw materials used without
informing the brand, or ensuring that the new raw material is
compliant. Supply chain controls are crucial.
PRACTICAL CONSIDERATIONS
Testing for possibly-harmful substances and certifications of safe
manufacturing practices certainly help protect consumers—and
brand reputations. But there are some practical considerations.
You can’t test for everything—it doesn’t make sense and it makes
products too expensive to manufacture. Somebody has to pay for
the testing. “Every retailer wants testing, but they don’t always
want to pay for it,” says Wentz.
“The practical problem to finding out whether a fabric is safe
or not is the cost; it really costs too much to execute those tests,”
says Gery Emonds, sourcing & purchasing manager at Crossline
(China) Ltd. “Can we make the testing a bit cheaper, please?”
Pacheco agrees that the cost of testing is high. “Regulations should
focus on areas of highest concern rather than blanket regulations
on all items,” he says.
“I’m not opposed to testing, but you have to be intelligent about
what is required,” says Eapen. “There are more than 100 chemi-
cals on the AAFA RSL. You don’t need to test for most of them in
every instance. It depends on the specific chemicals used in the
process and on the end use of the product.” For example, lead is
not often found in fabrics, but is sometimes found in plastic and
metal buttons and zippers says Eapen. “Some RSL’s have a matrix
for testing. This is a very practical approach to reduce testing
costs and assure RSL compliance,” he says. A testing matrix would
provide the conditions under which the presence of a chemical
might be expected, and whether to test for it. if a certain chemical
substance is never used in processing synthetic fabrics, testing for
that substance in a shipment of acrylic blankets would make no
sense, for example.
Testing and certification may add to the costs of producing and
selling textile products, but those costs are small compared to the
value of protecting a brand’s reputation. And the protection of
human health and the environmental health of the planet are worth
far more. “We see environmental challenges all over the world. It’s
capital intensive to solve these problems, but the chemicals we put
into the water and atmosphere stay around for a long, long time,
even 50 years later,” says Jesseph. “Let’s make an investment now
and make sure we’re minimizing our environmental impact, for us
and for our children.”

LINKS:
AAFA (American Apparel & Footwear Association):
www.apparelandfootwear.org

AFIRM Group (Apparel & Footwear International RSL

Management Working Group):
www.afirm-group.com

For more information about safe textile certifications, watch

for the July issue of AATCC News in your email inbox. Get your
free subscription at www.aatcc.org/media/news.

28 AATCC R e v i e w www.aatcc.org June 2009

  
Flammability of Construction and Building Textiles
By Dwayne Sloan, Underwriters Laboratories Inc.

There are more than 200 test methods published by AATCC • Fabric horizontal shades or blinds
for the testing and quality control of textile products. However, • Fabric vertical shades or blinds
there are additional test methods and standards relating to the • Horizontal folding shades
flammability characteristics of textiles. For fabrics and films • Hospital privacy curtains
used within a building or as part of the construction, the major • Roll-type window shades
flammability codes throughout the US refer to National Fire • Stage or theater curtains
Protection Association (NFPA) 701, Standard Methods of Fire • Swags
Tests for Flame Propagation of Textiles and Films. The method • Vertical folding shades
evaluates a material’s ignition resistance and its potential to • Window curtains
propagate flame beyond the area exposed to a specified • Window draperies
ignition source.
It should be noted that for those materials applied to building
surfaces or as backing for interior finishes (e.g., fabric wall cov-
erings) should be evaluated in accordance with UL723 or ASTM
E84, Standard Method of Test of Surface Burning Characteristics
of Building Materials, or NFPA 265, Standard Methods of Fire
Tests for Evaluating Room Fire Growth Contribution of Textile
Coverings on Full Height Panels and Walls. The authority having
jurisdiction should be consulted in these instances.

Code References to NFPA 701

Both the International Code Council (ICC) and NFPA model codes
include numerous references to NFPA 701. The International
Building Code (IBC) even defines “flame resistance” as a mate-
rial or combination of materials that restricts flame spread in
accordance with NFPA 701. Table I is an overview of some of
the model code requirements that specify NFPA 701.

NFPA 701, Test Method 1

NFPA 701 is divided into two sections. Test Method 1 applies to
single-layer fabrics or multilayer curtain and drapery assemblies
in which the layers are fastened together by sewing or other
means. For the purpose of the standard, curtains include:

JUne 2009 AATCC Rev i e w 29

App lied Tech

Test Method 1 also applies to table skirts, table linens, display

booth separators, and textile wall hangings. Materials with an
area density greater than 700 g/m2 would be examined using
Test Method 2.
A general summary of Test Method 1 is that a weighed textile
or fabric specimen, 15.8 in. long, is suspended vertically in an
open-faced test chamber. An approximately four-in.-high flame
with a specified gas flow rate is applied to the specimen for 45
seconds and then withdrawn (Fig. 1). The specimen is allowed to
burn until the flame self-extinguishes and no further specimen
damage occurs. The specimen is removed and weighed again.
The percent weight loss is used as a measure of total flame
propagation and damage. The average weight loss of the 10
specimens shall be 40% or less in order to meet the requirement
of the standard. In addition, dripping residue falling to the floor
shall not burn for more than two seconds.

NFPA 701, Test Method 2

Test Method 2 applies to fabrics, including multilayered
fabrics, films, and plastic blinds, with or without reinforcement
or backing. This method is used for testing vinyl-coated fabric
blackout linings, draperies with such linings, decorative or other
plastic films used inside a building, and plastic films used to
enclose buildings under construction. Test Method 2 also applies
to fabrics used in the assembly of awnings, tents, tarps, similar
architectural fabric structures, and banners.
For Test Method 2, a 47-in. specimen is exposed to an
11.0-in. flame for two minutes inside a four-sided test cabinet.
The specimen is allowed to burn until the flame self-extinguish-
es and no further specimen damage occurs (Fig. 2). Specimens
that flame after the exposure flame is removed, or drip residue
that flames for more than two seconds, are considered non-
compliant with the standard. Criteria also exist for length of char.
Fig. 1. Close-up of NFPA 701 Test Method 1.

30 AATCC R e v i e w www.aatcc.org June 2009

 App lied Tech
Other Criteria
For both test methods in NFPA 701, when durability to cleaning
or weathering is claimed, the textile or material must be tested for
flame propagation as produced, and after being subjected to the
applicable cleaning or exposure procedures. For example, if the
fabric is intended to be refurbished by dry cleaning or laundering,
the fabric would be subjected to a specific number of cycles of
the dry cleaning or laundering recommended by the manufacturer.
If the material is expected to be used outdoors, the material
must be subjected to an accelerated water leaching procedure.
Products certified to NFPA 701 requirements by Underwriters
Laboratories are covered under product category “Fabrics
(category code GPIX).”

Author
Dwayne Sloan is the Principal Engineer for Building Materials
and Building Contents at Underwriters Laboratories. He is
a member of NFPA Fire Test Committee responsible for the
Standard NFPA 701.

Dwayne Sloan, Underwriters Laboratories Inc., 12 Laboratory Dr.,

Research Triangle Park, NC 27709, USA; phone +1 919 549
1676; fax +1 919 547 6287; Dwayne.E.Sloan@us.ul.com.

Fig. 2. NFPA 701 Text Method 2.

TABLE I.
Codes Referencing NFPA 701
Products or Materials Codea
• Textile or fabric films used in children’s playground structures International Building Code
• Textiles and films used in sets and scenery
• Decorative materials
• Curtains, draperies, hangings for certain occupancies
• Membranes and interior linings used for noncombustible membrane structures
• Canopy materials
• Motion picture screens International Fire Code
• Curtains, draperies, hangings, other decorative materials
• Tents, canopies, membrane structures, sidewalls, tarpaulins, floor coverings, bunting
• Textiles and films for kiosks and similar structures NFPA 5000 Building Construction & Safety Code
• Membrane structure fabrics
• Tent fabrics, coverings for awnings and canopies
• Combustible scenery NFPA 1 Uniform Fire Code
• Curtains, draperies, hangings membrane structure fabrics
• Exhibit booths
• Synthetic fabrics permitted in Class A and Class B chambers NFPA 99, Standard for Health Care Facilities
a Code references as of October 2008.

JUne 2009 AATCC Rev i e w 31

Pee r Reviewed

Low Pressure, Nonequilibrium-Plasma-Assisted

Generation of Flame Retardant Cotton
By Vladimir Totolin, Majid Sarmadi, Sorin O. Manolache, and Ferencz S. Denes,
University of Wisconsin-Madison

ABSTRACT

The objective of this project was to generate a durable flame retardant (FR) treatment on cotton fabrics. Sodium silicate
(SS) layers were pre-deposited onto clean cotton substrates and crosslinked using low pressure, nonequilibrium
oxygen (O2) plasma. Prior to deposition, cotton samples were Soxhlet extracted in acetone for 6 h to ensure a clean
surface. A statistical design of experiments was used to optimize plasma parameters. Cotton samples were tested
for flammability with an automatic 45°-angle flammability chamber. Thermogravimetric analyses (TGA) indicated
a low quantity of coating material. Durability to laundering studies were also conducted to determine the coating’s
resistance to the accelerated laundry technique. Control (untreated) and treated sample surfaces were characterized
by X-ray photoelectron spectroscopy (XPS), attenuated Fourier transform infrared spectroscopy (ATR/FTIR), and
scanning electron microscopy (SEM).
Key Terms: Coatings, Cotton, Flame Retardant, FR, Plasma, Silicate

Introduction or by inhibiting oxidation in the gas phase.3 The simplest

FR and FR textiles are prevalent in all aspects of our
daily lives. They are present in upholstered furniture,
curtaining, home furnishings, car seats, in the workplace,
and in all public areas, including trains and passenger
aircraft. FRs are chemicals added to polymeric materials,
both natural and synthetic, to enhance FR properties.
FR chemicals are most often used to improve the fire
performance of low-to-moderate cost commodity poly-
mers. FRs may be physically blended with or chemically
bonded to the host polymer. They generally either lower
ignition susceptibility or lower flame spread once ignition
has occurred.
Some polymers are inherently less flammable due
to more stable polymeric structures; these are usually
higher-priced engineering plastics such as polyimides,
polybenzimidazoles and polyetherketones.1 In more flam-
mable natural or synthetic polymers, the most significant
step in the burning process is the fuel production stage,
where thermal energy induces bond scission mechanisms
that result in volatile molecular fragment formation.
These low molecular weight compounds diffuse into the
surrounding environment and generate flammable gases
which initiate combustion. Modifications can be made
to alter a material’s flammability at various stages of the
burning process, which include heating, degradation and
decomposition, volatilization, and oxidation.2 Most FRs
decrease flammability by increasing char formation or
reducing formation of volatiles in the condensed phase,
modification methods involve addition of water-soluble
acid ammonium phosphates and borates. More sophis-
ticated and durable finishes use phosphorus compounds
in conjunction with urea and melamine resins to create
a crosslinked finish with cellulose.4 This type of finish is
applied via a pad-dry-cure method.5 Problems with these
finishes include yellowing from heat curing and acid
damage, alteration of fabric hand, and degradation, or
total loss of mechanical properties.1-5
There has been an increasing demand to replace
both antimony-halogen systems in textile back coatings
and formaldehyde-free treatments in durable finishes.
Therefore, the number of new articles, patents, and prod-
ucts associated with silicon-based FR systems is evidence
of renewed interest in FR approaches that do not rely
completely on halogens or phosphorus. It is believed that
silicon-based FRs for synthetic or organic polymers act
in two basic ways: by thermal quenching (endothermic
decomposition of the FR) and by forming a protective
coating (liquid or char barrier).6-16
Due to increased requirements on textile fabric
finishing, as well as the market and societal demand for
textiles that have been processed by environmentally-
friendly methods, new, innovative production techniques
are needed. These concerns and limitations have led
to further development of alternative physicochemical
processing methods. In this field, plasma technology
shows distinct advantages because it is environmentally
friendly, and surface properties of inert materials can be

32 AATCC R e v i e w www.aatcc.org June 2009

 Pee r Reviewed
easily modified. On this basis, this paper discusses FR conditions. Samples were mounted in a frame and held
improvements of cotton fabrics using SS and low-pressure at an angle of 45°. A standardized flame was applied
O2-plasma treatments. to the surface near the lower end for specified amount
of time (5 s). The flame traveled up the length of the
Experimental fabric to a trigger string, which stopped the timer when
burned through. The time required for the flame to
Materials travel the length of the fabric and break the trigger string
Bleached desized cotton print cloth (78 × 76), weight = was recorded, as well as the fabric’s physical reaction
102 g/m2 was purchased from Testfabrics Inc. and cut at the ignition point. Five samples for each treatment
in 2- × 6-in. samples. Acetone and SS solution (27 wt% were tested and the tests were duplicated. It should be
SiO2) were purchased from Sigma Aldrich Chemicals. mentioned that even though the standard test requires a
1-s ignition time, for these experiments, the ignition time
Procedure used was 5 s because the plasma-treated samples did not
Cotton samples were Soxhlet extracted with acetone catch fire in the first place.
for 6 h to remove impurities from the fibers, then dried
overnight in a vacuum oven at 30 Torr, at room tem- Thermogravimetric Analysis (TGA)
perature (RT). Samples were soaked in SS solution at the TGA measures weight changes in a material as a function
desired SiO2 concentrations for 2 h. Concentrations were of temperature under a controlled atmosphere and was
chosen according to a statistical design of the experiments performed to aid treatment analysis in correlation with
(Design Expert 7 software). After soaking, samples were spectroscopic data. A TGA Q500 (TA Instruments)
dried in the vacuum oven at RT overnight and then recorded the thermal stability and decomposition of
exposed to O2 plasma in a 13.56-MHz parallel plate reac- samples using
tor.17 Samples were washed for 30 min in de-ionized (DI) a heating rate
of 10C/min up Table I.
water using an ultrasound bath after plasma treatment.
Experimental Treatment Parameters
Three washings for each batch were performed. The fol- to 700C. The and Burning Spread Time
lowing O2-plasma parameters were used: 50W-150W RF purge gas used
was nitrogen. Run # Cold Plasma Treatment Parameters Burning
(radio frequency) power, 2-8 min, 200-mTorr pressure
Time (s)
in absence of plasma, and 60-mTorr base pressure. Table SS Concentration Power Time
I shows the optimization of the plasma parameters and Durability to (%) (W) (min)
their corresponding results for the burning time spread of Laundering
1 5.00 100.00 5.00 27.87
the untreated (control) and treated cotton samples. To evaluate
2 7.00 70.27 3.22 24.40
the durability
45° Angle Flammability Test of the coating 3 5.00 50.00 5.00 27.50
Laundered samples were dried in vacuum oven at 80C during washing, 4 5.00 100.00 5.00 27.30
overnight and then tested for flammability with a 45° the treated
angle Auto-Flame chamber. This test is used to measure samples were 5 7.00 129.73 3.22 14.60
and describe the properties of natural or synthetic fabrics exposed to an 6 8.40 100.00 5.00 13.40
in response to heat and flame under controlled lab accelerated laun-
dering method 7 5.00 100.00 5.00 26.57
Design-Expert® Software
150 00
Burning time
0.0976673
proposed by 8 5.00 150.00 5.00 13.63
Burning time
Design Points McSherry, et
9 5.00 100.00 2.00 25.53
5.97182
30.3
11.8 6 al.18 The stan-
11.47 125 00
17 7201
dard is known 10 7.00 70.27 6.78 25.03
23.59 3
to correlate very
X1 = A: Concentration
11 3.00 129.73 6.78 26.40
closely with 50
B: Power

X2 = B: Power

cycles of domes-
100 00 3
Actual Factor 12 3.00 70.27 3.22 26.33
C: Time = 5.00
tic laundering. 13 3.00 129.73 3.22 27.55
75 00 An approximate
40-to-1 liquid 14 5.00 100.00 8.00 28.27
23.59 3 (DI water) to 15 7.00 129.73 6.78 11.47
50 00

1.6 3.32 5 00 6 68 8.36

fabric ratio was
used with a 16 1.60 100.00 5.00 27.30
A: Concentration 0.5% solution of 17 3.00 70.27 6.78 30.30
tribasic sodium
Fig. 1. Burning time response surface versus power (W) and SS
concentration (%). phosphate

JUne 2009 AATCC Rev i e w 33

Pee r Reviewed

(Na3PO4 × 12 H2O) and 0.1% of Bt = −25.47164 + 8.71527 ⋅ C + 0.68792 ⋅ P + 2.95907 ⋅ t − 0.043474 ⋅ C ⋅ P − 0.1864 ⋅ C ⋅ t
Triton X-100. Samples were boiled − 0.02093 ⋅ P ⋅ t − 0.5576 ⋅ C 2 − 2.43743 ⋅10 −3 ⋅ P 2 + 0.026825 ⋅ t 2
for 4 h, rinsed thoroughly using five
changes of distilled water, and dried in
a vacuum oven at 80C overnight.
Surface Characterization
XPS
A Perkin Elmer Physical Electronics Phi 5400 Small Area
Spectrometer (Mg source; 15 kV; 300W; pass energy =
89.45 eV) was used for the XPS analysis. A 45° take-off
angle was used between the sample and the detector.
Survey and high-resolution (HR) scans for core levels
were done on the samples. The curve fitting of the HR
peaks were done using a Gaussian algorithm.
ATR/ FTIR
ATR/FTIR analyses were performed to get more
information about the chemical linkages and to substanti-
ate the findings from XPS measurements. An Equinox
55 (Bruker) was used for sample surface characterization.
Data were collected in the 500-4000 cm-1 wavenumber
region with 300 scans for each sample at a resolution of
0.5 cm-1. The samples were placed on a
germanium crystal.
SEM
To characterize surface morphology as well as coating
uniformity, the samples were analyzed with a LEO DSM
1530 FE SEM. The magnification used was 20,000×.
Results and Discussions
45°-Angle Flammability Test the substrate was completely consumed at 700C. Weight
The experimental parameters and the results from burn-
ing time spread of the samples are presented in Table I
and Fig. 1. SS concentrations in the 3% to 4% range
and RF-power values of 75W to 90W in the middle of
the time domain (5 min treatment time) led to the best
burning time spread data based on data in Fig. 1. The
quadratic model (0.9999 probability that it is measuring
Eq. 1
Bt is burning time (s), C is the SS concentration (%), t is
the treatment time (min), and P is the dissipated power
(W). The model predicts burning time as high as 31.9 s
for samples using SS concentration of 3% treated for 7.8
min at 76W.
Durability to Laundering
To evaluate the durability of the coating during washing,
treated samples were exposed to the accelerated launder-
ing method proposed by McSherry, et al., as described
earlier. Based on the results obtained from the experi-
mental design, the following O2-plasma parameters were
selected to determine FR behavior: RF power was 100W
and gas pressure in the absence of plasma was 200 mTorr,
with a plasma exposure time of 8 min. Varying just the
SS concentration, the samples were tested for flammabil-
ity both before and after laundering (Table II). Five
samples for each treatment were tested and the tests were
duplicated. The samples tested before laundering showed
very high FR behavior. Furthermore, it was shown that
even after 50 laundry cycles, a dramatic increase in the
combustion time (about three times higher for 2 and
3 wt% and twice for 5 wt%) was observed. Results
obtained for the laundered samples are similar to those
reported by Konda, et al.19 and Ramachandran, et al.20
Thermogravimetric Analysis (TGA)
Typical TGA curves of untreated and 2 wt% SS
solution-treated samples are shown in Fig. 2. Weight loss
of the unmodified cellulose sample started at 330C and
residuals at 700C of silicate-coated and plasma-treated
substrates gave a less significant weight loss (63.6%,
63.2%, and 58.7% for 2 wt%, 3 wt%, and 5 wt% SS
concentrations, respectively) for the samples that were not
exposed to the accelerated laundering technique.
TGA Analysis for 2% Flame Retardant
Control

Treated, before laundering

a systematic 100
Treated, after 50 laundry cycles

effect, not 90

experimen- 80

Table II.
Flammability Results for Different Concentrations of SS
tal noise; 70

ANOVA
Weight residual (%)

60

SS Concentration Burning Time (s) analysis) is 50

(%)
Before Laundering After 50 Laundry expressed 40 b

Cycles by Eq. 1. 30

20
c
0 9.00 9.00
10
a
2 277 29.70 0
0 100 200 300 400 500 600 700

3 290 25.00
Temperature ( C)

5 Did not ignite (DNI) 19.30 Fig. 2. TGA diagrams of (a) untreated cotton, (b) cotton immersed into 2% SS
and plasma treated, and (c) plasma treated cotton after 50 laundry cycles.

34 AATCC R e v i e w www.aatcc.org June 2009

 Pee r Reviewed
(285 eV), C-O (286.5 eV), O-C-O/C=O
(a) (b) (c) (d) (288 eV) and O-C=O (289.2 eV).21
Survey XPS data from non-extracted
cotton gave 67.1% C and 32.9% O for
the relative surface atomic concentrations
(Table III). This is significantly different in
comparison to the atomic concentrations of
the theoretical cellulose structure (C: 54.5%
and O: 45.5%). An explanation is that
cotton fibers are composed of a secondary
wall (typically 90% by weight) and an outer
Fig. 3. Burning behavior of (a) untreated cotton, and (b) 5% silicate, (c) 3% silicate, (d) 2% silicate primary wall.22 The secondary wall is essen-
deposited and plasma-treated cotton. tially cellulosic in nature, whereas the outer
primary wall consists of ~55% cellulose, the
rest attributed to proteins, pectins, and wax; thus the
Table III.
Relative Surface Concentrations of Virgin, Extracted,
presence of hydrocarbon impurities can be observed.
and Plasma-treated Cotton The HR C1s diagram (Fig. 4a) of non-extracted cotton
confirms that high carbon content was present in the
Sample Carbon Oxygen Silicon Ratios
(%) (%) (%)
surface layers of the substrate. The presence of an intense,
C/O C/Si high relative-surface area C-C peak (57.2%) compared to
Virgin Cotton 67.1 32.9 - 2.0 - the C-O peak (35.7%) surface area indicated the presence
Extracted Cotton 50.9 49.1 - 1.0 -
of carbon-based impurities (Table IV).
Survey and HR XPS results collected from the
Plasma treated cotton 43.4 50.2 6.4 0.8 6.8 Soxhlet extracted cotton samples (Fig. 4b) clearly show
the existence of a lower relative surface carbon atomic
Substrates that went through a 50-cycle laundering concentration (51%) and a significantly decreased relative
process gave weight losses of 87%, 89%, and 88%, surface area of the C-C peak (32.4%) after extraction
respectively, regardless of the silicate solution concentra- (Tables III and IV). It was concluded that, to simplify
tion used during the coating process. It can be concluded surface analysis of this complex system, Soxhlet extraction
that most of the pre-deposited and plasma-treated silicate
layer was removed during the laundering process. Weight
loss that began at lower temperatures for the treated Table IV.
samples was related to the chemically-bound water (pres- Relative Percentage of Carbon Functionalities for Virgin,
Extracted, and Plasma-treated Cotton
ent in SS) released through an endothermic reaction.
Sample C-C C-O O-C-O C-Si O-C=O
Burning Behavior
The photograph in Fig. 3 shows the behavior of treated Virgin Cotton 57.2 35.7 5.3 - 1.8
samples (b, c, and d) compared to the untreated one (a) Extracted Cotton 32.4 52.2 12.8 - 2.6
during the burning test. Virgin cotton burns completely
while most of the burned material is retained as a char Plasma treated cotton 31.0 50.0 10.8 6.4 1.8
in the case of silicate/plasma treated samples. This is
characteristic of a homogeneous silicate coating on the
treated samples. a b c

XPS Analysis C-
C C-O
Pure cellulose consist of C-O and C=O/O-C-O link- C-O
C-
ages. However, even high purity filter paper or cotton O-C-
C/
C-
structures incorporate small amounts of O-C=O groups C-O
O C-
C
O-C- Si
O-C- O
originating from uronic acid and C-C aliphatic bonds O
O-
related to the presence of carbon-containing surface O-
C=O
C=
O-
C=
O
impurities. This is why, prior to the deposition of the O

silicate layers, cotton samples were Soxhlet extracted in

acetone for 6 h. The high resolution (HR) C1s peak is 290 288 286 284 290 288 286 284 290 288 286 284

fitted in four distinct peaks including: C-C/C-H Fig. 4. High resolution C1s spectrum of (a) virgin, (b) acetone extracted, and (c)
plasma-assisted silicate-covered cotton samples.

JUne 2009 AATCC Rev i e w 35

Pee r Reviewed

in acetone should precede the coating and plasma-treat- (a)

ment steps to remove the impurities that might interfere
with the deposition processes and could also influence the
adhesion characteristics of the plasma layers to
the substrate.
The decrease in the relative surface atomic carbon
content and the presence of silicon atoms (6.4 %) incor-
porated into the silicate-coated and O2-plasma-exposed,
as well as results for the consecutively extracted samples,
are shown in Fig. 5 and Table III. It is suggested that part
of the pre-deposited silicate structure had been cross-
linked and converted into a non-water soluble network.
The presence of a larger relative surface area 285 eV
peak (Fig. 4c) in the HR C1s diagram indicates that, in (b)
addition to C-C linkages, C-Si bonds also are part of the
plasma-modified layers.
ATR/FTIR
Infrared (IR) waves penetrate substrate surfaces to a
depth of 2-5 µm, while plasma species penetrate only a
couple of nanometers into the surface layer. ATR/FTIR
measurements were performed on cellulose samples and
on plasma-treated samples to find out if, during the
plasma treatment, unmodified silicate molecules were
encapsulated below the top crosslinked structure. All cel-

(c)

O 1s
50.2 %

C
43.4 %

Si 2p
6.4 %

1000 900 800 700 600 500 400 300 200 100 0
Binding Energy

Fig. 5. XPS survey spectrum of O2-plasma assisted SS (2%) covered

cotton sample. Fig. 7. SEM images of (a) control cotton, (b) plasma-treated
cotton exposed to 50 laundry cycles, and (c) plasma-treated cotton
1.5
Plasma treated
non-laundered.
0.9

0.7
lulose IR absorptions were assigned:23 663-670 cm-1
(OH wagging); 893-900 cm-1 (C1-O-C4 ring stretch);
1000-1030 cm-1 (C-O stretching); 1050-1100 cm-1
Transmittance (normalized)

1.0 0.5
Control

0.3
(C-O-C asymmetric bridge stretching); 1315-1370 cm-1
(CH wagging, CH bending); 1428 cm-1 (in-plane OH
0.1 bending); 2893-2950 cm-1 (C-H stretching); and 3300-
0.5
3400 cm-1 (H-bonded OH stretch). ATR-FTIR diagrams
-0.1
of cellulose, and silicate-coated and plasma-treated
-0.3 cellulose (Fig. 6), did not show significant differences.
This indicates that non-plasma-modified silicate was not
0.0
3500 3000 2500 2000 1500 1000 incorporated under the thin crosslinked surface layer. The
Wavenumber (cm-1)
presence of a weak bimodal absorption in the
Fig. 6. ATR/FTIR spectrum of control and plasma treated cotton.
1920-2200 cm-1 wavenumber zone of the non-treated
cellulose substrate is related to remnant unsaturated

36 AATCC R e v i e w www.aatcc.org June 2009


hydrocarbon contamination due to handling after
extraction. Due to silicate coating of the substrates and
subsequent plasma treatment, these absorptions were
not evident in the ATR/FTIR diagram of SS/O2-plasma
modified samples.
SEM
Comparative SEM images of cellulose and modified
cellulose samples (Fig. 7) indicate the presence of
silicate-based coating on treated fiber surfaces. A less
clear image of the fibers’ features due to the coating and
plasma-treatment in comparison to the unmodified cel-
lulose fibers can be noted. It can be concluded that even
after the accelerated laundry procedure, the silicate-based
structure is still on the fiber surfaces.
Conclusions
A complete statistical design of experiments was
conducted to predict FR proprieties of SS-O2 plasma-
exposed cotton, based on the SS concentration used.
Combustion time of the treated cotton samples (after
laundering) dramatically increased to about three times
greater than the control sample. According to both the
statistical model and the experiments conducted, better
results were obtained when both low SS concentrations
and power dissipated to electrodes were used at higher
O2-plasma exposure times. An explanation is that higher
concentrations of SS resulted in thick SiO2 layers that
cannot be polymerized uniformly and completely by O2
plasma. It is important to note that plasma treatment
increased the ignition time from 1 s to 5 s. Therefore,
all treated samples were tested with a 5 s ignition time
(instead of 1 s). TGA results showed that silica layer
acts as a thermal insulator, allowing the coated cotton
to decompose at lower rates compared to the untreated
sample. Surface characterization of the substrates with
XPS, ATR/FTIR, and SEM confirmed the presence of
silicate-like structures on the surface of the fabrics even
after 50 laundry cycles. It was concluded that the
low-pressure plasma technique used to crosslink the pre-
deposited silicate layers onto the cotton has the potential
to generate flame retardant fabrics.
Acknowledgements
The authors would like to address their appreciation
to the US Department of Agriculture (Research Grant
S-1026) and the graduate school of University of
Wisconsin-Madison for the financial support of
this research.
References
1. Gann, R. G., Kirk-Othmer Encyclopedia of Chemical Technology,
4th edition, Vol. 10, John Wiley & Sons, New York, N.Y.,
USA, 1993, pp930-936.
JUne 2009 AATCC Rev i e w 37
Pee r Reviewed
2. Lyons, John W., The Chemistry and Uses of Fire Retardants,
Wiley Interscience, New York, N.Y., USA, 1970.
3. Handbook of Fiber Chemistry, edited by Manachen Lewin and
Eli M. Pearce, Marcel Dekker, New York, N.Y., USA, 1998.
4. Carty, Peter and M. S. Byrne, The Chemical and Mechanical
Finishing of Textile Materials, Newcastle upon Tyne Polytechnic
Products Ltd., Newcastle, UK, 1987.
5. Horrocks, A. R., Flame Retardant Finishing of Textiles, Vol. 16,
1986, pp62-101.
6. Quede, A., et al., Surface & Coatings Technology, Vol. 180-181,
2004, pp265-270.
7. Takao, A. and N. Kazunori, JP Patent No. 49023278, 1970.
8. Yamaguchi, H., Mokuzai Gakkaishi, Vol. 40, 1994, pp830-837.
9. Paren, et al., US Patent No. 5,417,752, 1995.
10. Gutek, US Patent No. 4,419,402, 1983.
11. Mitsuo, I. and T. Hashimoto, JP Patent Nos. 52063496 and
54004440, 1975.
12. Kuechler, William L., US Patent No. 3,666,544, 1972.
13. Junichi, K., JP Patent No. 49120999, 1973.
14. Hideaki, N., I. Toshiyuki, and Y. Shigeki, JP Patent
No. 48091396, 1972.
15. Park, B. K., WO Patent No. 2004062815, 2004.
16. Terrance, K. M., GB Patent No. 2290989, 1996.
17. Totolin, Vladimir, Masters Thesis, University of Wisconsin-
Madison, 2006.
18. McSherry, W. F., et al., American Dyestuff Reporter, Vol. 63,
No. 7, 1974, pp52-67.
19. Konda, A., et al., Journal of the Textile Machinery Society of
Japan, Vol. 28, No. 8, 1975, pp100-107.
20. Ramachandran, T., et al., IE (I) Journal, Vol. 85, 2005,
pp29-32.
21. Johansson, L. S., et al., Surface and Interface Analysis, Vol. 36,
2004, pp706-710.
22. Mitchell, R., et al., Cellulose, Vol. 12, 2005, pp629-639.
23. Tasker, S., et al., Polymer, Vol. 35, No. 22, 1994, pp4717-4720.
Author
Majid Sarmadi is a Rothermel Bascom Professor of
Textile Science and Materials Science at the University of
Wisconsin-Madison. For the past 23 years, his research
has focused on plasma treatment of textiles and other
polymeric materials. He is the author and co-author
of more than 60 papers and four patents. Sarmadi has
received many awards, including the Harold DeWitt
Smith Memorial Medal, presented jointly by ASTM
International, Committee D13 on Textiles and Albany
International Research Company. His work on the
Sustainable Carpet Project for the State of California,
USA received more than 16 awards.
Majid Sarmadi, Department of Design Studies,
University of Wisconsin-Madison, 1300 Linden Dr.,
Madison, WI 53706, USA; phone +1 608 262 7492;
fax +1 608 265 5099; majidsar@wisc.edu.
Pee r Reviewed

Hydrophilicity and Cell Affinity of

Atmospheric-Pressure Plasma Jet-Treated Nerve
Regeneration Conduit
By Lin Lou, Zhejiang Sci-Tech University & Donghua University; Jia Zhou, Zhejiang Provincial
People’s Hospital & Shanghai Jiao Tong University Affiliated First People’s Hospital; and Nanliang Chen,
Donghua University

ABSTRACT

Nerve conduits made of biodegradable materials will become important in repairing nerve injuries. To improve
hydrophilicity and cell affinity of braided, biodegradable, peripheral-nerve regeneration conduits and to promote
regeneration of an injured nerve, a poly(glycolide-co-L-lactide) (PGLA) nerve regeneration conduit was treated with an
atmospheric-pressure plasma jet (APPJ). Surface modification of the material was achieved. Using a wicking property
survey, X-ray photoelectron spectroscopic (XPS) analysis, in vitro cell culture experiments, methylthiazolyl tetrazolium
(MTT) cell proliferation assays, and field emission scanning electron microscopic (FESEM) analysis, the influence of
APPJ treatment on hydrophilicity and cell affinity of three different nerve regeneration conduits was determined.
Key Terms: APPJ, Biodegradation, Braiding, Cell Affinity, Hydrophilicity, Nerve Regeneration Conduit, PGLA, Plasma

Introduction healing effects in in vivo assays.1,6 However, there is still a

The nervous system performs important functions in
the human body. Nerve injury is usually followed by
failure of normal organ functions. Many strategies have
been attempted to stimulate the regeneration of injured
nerves. The most successful approach to date is to bridge
the defect with a peripheral nerve graft. Autografting,
taking a nerve segment from another part of the body
and placing it at the needed site of the same individual,
is a common and effective clinical practice, although
drawbacks include donor site morbidity, the need for a
secondary surgical site, inadequate functional recovery,
and the difficulty of finding a matchable donor source.1,2
Use of a peripheral nerve regeneration conduit is an
alternative solution to overcome these drawbacks. The
conduit is a kind of prefabricated tube, made of bioma-
terials or non-biomaterials, used as a bridge to guide the
axons to grow from proximal stump to the distal stump
by implanting the conduit, placing the proximal and
distal stumps into respective ends of the conduit, and
by suturing the epineurium to the wall of the conduit.3
Among different kinds of peripheral nerve regenera-
tion conduits, biodegradable PGLA nerve regeneration
conduits with a braided structure have good mechanical
properties, suitable degradation properties, and fine
biocompatibility.2,4,5 This specially-made conduit is an
advanced technology that has demonstrated fairly good
long way to go before the conduit can be used in clinical
application. Some research shows that the healing effect
of autografting is slightly better than that when braided-
PGLA nerve regeneration conduit was used.7 Researchers
are still looking for the optimum conduit material. Based
on the fairly good behavior of the braided-PGLA nerve
regeneration conduit, improving its surface properties was
crucial for success, to replace autografts, and to become
the best solution for the future.
Better surface medical properties of the conduit can
be achieved by surface modification. APPJ treatment is
an environmental-friendly technique that can modify
the surface layer of ~10 nm in depth with no harm
to material’s general properties. The technique is also
convenient, efficient, gentle, and cheap, which is not the
case for other plasma treatments, such as low-pressure
glow discharge, dielectric barrier discharge, corona
discharge, transferred arc, or plasma torch.8,9 Little has
been reported about APPJ treatment on braided-structure
materials or on PGLA biomaterials.
Hydrophilicity and cell affinity are important factors
when braided-PGLA nerve regeneration conduit, a
biodegradable polymeric material, is used and evaluated
as a cell scaffold in tissue engineering.10 The purpose of
this study is to improve hydrophilicity and cell affinity
of braided-PGLA nerve regeneration conduit by surface
modification using APPJ treatment, and thus make
clinical application of the conduit more feasible.

38 AATCC R e v i e w www.aatcc.org June 2009

 Pee r Reviewed
Fig. 1. Triaxial braiding structure.

Fig. 3. Schematic diagram of atmospheric pressure plasma jet apparatus.

Plasma Treatment
Plasma treatment of the conduits was carried out on an
APPJ apparatus manufactured by Surfix Technologies.
The schematic diagram is shown in Fig. 3. This device
Fig. 2. Schematic of braided nerve conduit. generates a stream of reactive atoms at a low temperature
and at atmospheric pressure using a 13.56MHz radio
Experimental frequency. Treatment was carried out using a rectangular
nozzle that covered an active area of 2 ×10 mm2 and was
Materials mounted vertically above the substrate conveyor belt,11
A conduit of triaxial-braided PGLA structure was used. which moves at a constant speed of 2.5 mm/s. Helium
The PGLA material had a co-monomer ratio of 90% and oxygen were used as carrier and reactive gases respec-
glycolide (GA) to 10% lactide (LA), suitable for nerve tively. Processing parameters are listed in Table II.
regeneration.4,5 Studies show that a conduit with a
braided structure, especially a triaxial-braided structure, Wicking Property Test
have good mechanical and degradation properties. 2,5,10 Wicking rate was tested using a wicking property testing
Conduit parameters in this study are shown in Table I. device. One end of the conduit was fixed on a frame
The braiding structure and a schematic of the conduit are while the other end dipped vertically into a 27C ±2C
given in Figs. 1 and 2 respectively. 0.5% potassium dichromate solution. The wicking height
Before plasma treatment and testing, the conduit was immediately recorded. For the first minute of each
samples were scoured with absolute ethanol for 30 min test, the interval between every two recordings was
to remove possible impurities (e.g., finishing oil from 10 s. After the first minute, the interval was prolonged to
braiding process and dust), dried in a freeze dryer (FD- 1 min. Five conduits were tested per sample group.
ID-50), and then conditioned in a standard atmospheric
environment (20C ±2C, RH 65% ±3%). Some samples XPS Analysis
were coated with 3.0% chitosan. Biocompatible, bio- Surface chemical compositions and bonds of the PGLA
degradable, and bioactive, chitosan promotes nerve cell conduit were studied by XPS (X-ray Photoelectron
10
adhesion, migration, and differentiation. Similar to the Spectroscopic, Thermo ESCALAB 250) analysis using a
matrix of composite material, chitosan coat-
ing also provides mechanical support to the TABLE I.
braided structure. Processing Parameters of Braided Conduit
Three groups of different conduits were
Inner Braiding Linear Linear Wall Axial Yarn Length Absorption
used in this study:
Diameter Angle α Density of Density of Thickness Density (cm) Period
A. Triaxial-braided PGLA conduit (mm) Braiding Yarn Axial Yarn (mm) (yarn/cm) (day)
(°)
B. Triaxial-braided PGLA conduit treated (tex) (tex)
with plasma jet 1.80 60 36.32 18.16 0.25 19.18 15 90
C. Triaxial-braided PGLA conduit with chito-
san coating and treated with plasma jet
Table II.
Pretreated conduit samples of B and C were Processing Parameters of Atmospheric Pressure Plasma Jet Treatment
mounted on a rectangular wooden frame, which
was placed on the conveyor belt vertically under Helium Oxygen Gas Output Jet-to- Substrate Upside Underside
Flow Flow Temperature Power substrate Speed Treatment Treatment
the plasma jet nozzle before plasma treatment. Rate Rate (C) (W) Distance (mm/s) Times Times
(L/min) (L/min) (mm) (time) (time)
10 0.1 100 30 3 2.5 5 5

JUne 2009 AATCC Rev i e w 39

Pee r Reviewed

dual anode Mg Kα excitation source (hν=1253.6 eV), Results and Discussion

a power of 300W, and an energy analyzer with a fixed
transmission energy of 20 eV. The data were rectified by Wicking Ability Improvement
C 1s of the C-C bond and the bonding energy was The wicking effects of different conduits are shown in
284.8 eV. Fig. 4. The three curves show similar tendencies. Wicking
heights of B and C were greater than that of A, indicat-
Microscopic Cell Culture Observation ing much better wicking ability and hydrophilicity after
Bone marrow tissue was extracted from the thighs of plasma jet treatment. This is due to the reduction of
male SD rats (60~90 g), cultured to the second genera- contact angles on the fiber surface or coating surface
tion and purified into a 1 × 105/mL Bone Marrow Stem caused by newly-created roughness (i.e., an increase of
Cells (BMSCs) suspension. Fluid extractions of materials specific surface area) and by some hydrophilic chemical
of A, B, and C were obtained by putting 3 cm2/mL of A, groups after the plasma treatments.
B, or C into Dulbecco’s Modified Eagle’s Medium/F12 The wicking speed of C was not as fast as that of B
(DMEM/F12, cell culture medium) that also included because part of the openings on PGLA fiber and spaces
10% Fetal Bovine Serum (FBS, providing protein for the in PGLA yarn and conduit were covered by a non-
cells) according to Biological Evaluation of Biomaterials water soluble chitosan coating, which had a very good
and Medical Devices (GB/T 16886.12-2005). The fluid film-forming ability. The number of capillary tubes was
extractions were used for toxicity testing and biocom- reduced, weakening the capillary effect. However, the
patibility evaluation of the conduit. These extractions wicking ability of C was still better than that of A, espe-
partially imitate an in vivo environment and BMSCs cially at the beginning. Research12 shows that the average
were cultured in them. wicking height of triaxial-braided PGLA conduits, with
The conduit segments were exposed to BMSCs in the chitosan coating but no plasma treatment, can only
fluid extractions. In addition, Group D was a negative- achieve 4.03 cm by the seventh minute, while that of
control group culture fluid of DMEM and Group E Group A reached 9.30 cm. The wicking ability of that
was a positive-control group culture fluid of 2% phenol conduit was far worse than B, C, and even A were in the
DMEM. A blank control group was used for a zero set- present study. Despite its advantages, the chitosan coating
ting, culturing no cells. BMSCs growth were observed covered fiber surface spaces and blocked water passage.
under an inverted microscope (Olympus CKX31) every Plasma jet treatment can greatly improve the wicking
day. In each group of materials, six samples ability of the chitosan-coated conduit.
were observed.
MTT Assay of Relative Cell Growth Rate Fig. 4.
On the 5th and 7th day of BMSCs culture in fluid Wicking rate
comparison
extraction, a MTT (methylthiazolyl tetrazolium) assay among
was used to test relative cell growth rates of different conduits of
groups according to Eq. 1. MTT (10 µL) was added to Group A, B
and C.
every 0.1 mL BMSCs suspension whose concentration
was 5 × 104/mL, and the optical density (OD) was mea-
sured at 570 nm.
In each group, six samples were tested. The OD was
presented in the form of mean value ±standard deviation
(n = 6, x ±s). All the data were processed by SPSS 13.0
statistics software. One-way ANOVA was used to com-
pare different groups and t-test for independent samples
Table III.
was used to compare mean values between every two Surface Chemical Changes Determined by XPS
groups. Statistical significance was observed when the P
value was less than 0.05. Sample Atomic Concentration Atomic Carbon Bonds (%)
Group (%) Ratio (%)
MTT value of experiment al group Eq. 1
Relative growth rate =
MTT value of negative control group C O N O/C C–C C–O C=O
A 51.56 48.44 - 94 20.36 46.63 33.01
FESEM Analysis
B 48.63 51.37 - 106 13.70 39.91 46.39
Cell morphology and growth adhering to the material
surface were examined by FESEM (Sirion 200). BMSCs C 43.09 52.35 4.56 121 9.77 39.94 50.29
were cultured with A, B and C materials for 12 days and F: Inner 48.58 47.45 3.97 98 11.79 53.46 34.75
then observed by FESEM at magnifications of 1000× Surface of
and 5000×. C Conduit

40 AATCC R e v i e w www.aatcc.org June 2009

 Pee r Reviewed
Chemical Analysis occurred after 5 to 7 days. Their growth aspects were
The difference of surface chemical compositions and the same as conventionally-cultured BMSCs. Cell lysis
bonds for each group shown by XPS analysis (Table III). occurred in the culture dishes of E and no cells were seen
The atomic ratio of oxygen/carbon increased (13% for adhering to the dishes. These phenomena indicate that
B, 29% for C, and 4% for F) after APPJ treatment on the A, B, C, and D environments were not cytotoxic and
the surface of the conduit material. The percentage of BMSCs were able to live and reproduce in these environ-
C–O and C=O bonds increased (8% for B, 13% for C, ments. The materials of A, B, and C are biocompatible
and 11% for F) with a large growth of C=O bonds. The and can be used for nerve regeneration.
plasma jet can generate free radicals that can oxidize O
and N from reactive gas and the atmosphere. The results
showed a decrease in C–C
bonds and an increase in
a) b)
more oxidized polar groups
with C=O bonds, such as
–COOH and –CONH, that
are much more hydrophilic.
Comparing these groups,
chitosan-coated and plasma-
treated conduit may have the
best hydrophilicity.
Comparing F (the inner
surface of the C conduit) to
C, when plasma treatment
was carried out on the outer Fig. 5. FESEM micrographs of BMSCs on Sample A (triaxial braided PGLA conduit). a) 1000× and b) 5000×.
surface of the conduit, the
effect received by the inner
a) b)
surface was not as good as
that of the outer surface.
However, the porous struc-
ture of the braided conduit
can ensure a certain amount
of jet-stream penetration. A
better solution might be to
place one or more plasma-
treated PGLA fibers in the
chamber of the conduit on
the basis of C.12
Fig. 6. FESEM micrographs of BMSCs on Sample B (triaxial braided PGLA conduit treated with plasma jet).
Cell Culture Observation a) 1000× and b) 5000×.
Observed under the inverted
microscope, round or
a) b)
elliptic cells were found
to sediment at the bottom
of culture dish 24 h after
seeding BMSCs into fluid
extractions of A, B, C and
culture fluid of D. The cells
gradually turned into a shape
of bipolarity or a triangle
with comparatively longer
cell tuber and semi-visible
oval or round nucleus after
48 h. Accumulation phenom- Fig. 7. FESEM micrographs of BMSCs on Sample C (triaxial braided PGLA conduit with chitosan coating and treated with plasma
enon and exuberant growth jet). a) 1000× and b) 5000×.
with a swirl-shaped center

JUne 2009 AATCC Rev i e w 41

Pee r Reviewed
Table IV.
MTT Results of Different Groups (n = 6, ±s)a
Sample Cultured for 5 Days Cultured for 7 Days
Group
A570 nm Relative A570 nm
Growth Rate
A 0.271 ±0.014 97.1% 0.330 ±0.015
B 0.275 ±0.017 98.6% 0.334 ±0.018
C 0.277 ±0.019 99.3% 0.337 ±0.020
D 0.279 ±0.012 100% 0.340 ±0.014
E 0 0 0
aGrowth rate relative to D, P > 0.05.
MTT Assay
Every OD result of an experimental group was adjusted
against a blank control group to remove background
influences before comparisons were made. The MTT
results are shown in Table IV. Comparing every two
groups, P > 0.05 and there were no statistical differences.
These materials showed no restraint to cell growth ability.
Morphological Examination
In Figs. 5-7, round or elliptic BMSCs with obvious
tubers can be seen adhering onto PGLA fibers of each
group. The three-dimensional braiding structure forms
3D longitudinal spaces and brackets for the cells to grow
freely in with 3D shape. As a result, this kind of structure
is very favorable for the regeneration of nerve axons.
From micrographs with 1000× magnification, cells and
the cell matrix were more likely to be found and adhering
more tightly on plasma-treated fibers than on non-treated
fibers. PGLA fibers with chitosan coating and plasma
treatment attracted the largest amount of cells and cell
matrix.
Micrographs with 5000× magnification clearly show
cell morphology and fiber surface. In Fig. 5, the fiber
surface is even and smooth before plasma treatment. Figs.
6 and 7 show the rough surface of the fiber and greater
adhesion of the cells and cell matrix after plasma treat-
ment, which produced etchings and gaps on the surface.
The latter surface provided much greater hydrophilicity
and a more favorable place for the cells to adhere, grow,
and reproduce than other surfaces tested. This should
lead to a better regeneration result if conduit C is used to
repair injured peripheral nerve.
Conclusions
Treating a braided, biodegradable, peripheral
nerve-regeneration conduit with APPJ can successfully
achieve surface modification, greatly increase hydrophilic
groups on the material’s surface, and greatly speed up the
wicking of conduit. None of the three different groups
of PGLA conduit materials tested showed any restraint
42 AATCC R e v i e w www.aatcc.org
or cytotoxicity to cell growth and proliferation. No cell
morphological alternation appeared. PGLA conduit
materials showed good cell affinity. Among the three dif-
ferent groups, the PGLA conduit material with chitosan
Relative coating and plasma treatment was the most favorable
Growth Rate
for BMSCs to adhere, grow, and reproduce on. Triaxial-
97.9% braided PGLA conduit with chitosan coating and treated
98.2% by APPJ can provide a comparatively better growth
99.1% environment and therefore should be a good solution for
peripheral nerve injury.
100%
These results show a promising prospect for a triaxial-
0
braided PGLA nerve regeneration conduit with chitosan
coating and plasma treatment. In vivo investigations are
being conducted and clinical trials are needed to demon-
strate the healing effect of this conduit.
Acknowledgement
The authors would like to address their appreciation to
the “Dawn” Program of Shanghai Education Commission
of China (Grant No. 02SG29) for the sponsorship.
References
1. Xu, G., et al., NeuroReport, Vol. 15, No. 14, 2004, pp1-6.
2. Liu, G., P. Zhang, and W. Wang, Proceedings of The Textile
Institute 83rd World Conference, Shanghai, China, 2004,
pp1021-1024.
3. Lou, L., et al., Book of Papers, AUTEX World Conference,
Raleigh, U.S.A., 2006.
4. Liu, G., et al., Journal of Donghua University (Eng. Ed.), Vol.
21, No. 9, December 2004, pp66-70.
5. Liu, G., et al., Proceedings of 2005 International Conference on
Advanced Fibers and Polymer Materials, Shanghai, China, 2005,
pp979-982.
6. Bini, T. B., et al., Peripheral Nerve Regeneration, July 2003,
pp287-295.
7. Liu, G., PhD Thesis, Donghua University, Shanghai, China,
May 2006.
8. Schütze, Andreas, et al., IEEE Transactions on Plasma Science,
Vol. 26, No. 6, December 1998, pp1685-1694.
9. Qiu, Y., et al., Journal of Adhesion Science and Technology, Vol.
16, No. 4, 2002, pp449-457.
10. Wang, A., et al., Tsinghua Science and Technology, Vol. 11, No.
4, August 2006, pp415-420.
11. Wang, C. and Y., Qiu, Surface & Coatings Technology, Vol. 201,
2007, pp6273-6277.
12. Lou, L., Masters Thesis, Donghua University, Shanghai, China,
January 2007.
Author’s Address
Lin Lou, Fashion Institute, Zhejiang Sci-Tech University,
No. 5 2nd St., Hangzhou Xiasha Higher Educational
Zone, Zhejiang Province 310018, China; phone
+86 571 8684 3480; fax +86 571 8684 3481;
loulin@zstu.edu.cn.
June 2009
 Stu dent Paper
Colorfastness to Light:
Finding an L4 Equivalent
By Chelsea D’Andrea, University of Rhode Island

ABSTRACT

When testing for colorfastness to light, AATCC requires the use of a blue wool standard. This standard is colored
through the use of varied concentrations of two different dyes rated on a scale of L2-L9, L2 being the least colorfast
and L9 the most. One of the two dyes used to color the blue wool is now unattainable, but while L2 can be used,
a substitute for L4 (which fades to step 4 on the gray scale after 20 AFUs of exposure) would be advantageous if
discovered. This study will examine a wide range of acid dyes applied to wool as readily available dye candidates,
having fading characteristics comparable to the L4 standard after lightfastness testing, which are suitable for
further investigation.
Key Terms: AATCC Test Method 16, Blue Wool, Colorfastness, Dyes, L4 Standard, Lightfastness

This paper was the second-place winner in the Herman and Myrtle Goldstein Student Paper Competition,
held March 2009 at AATCC’s International Conference in Myrtle Beach, S.C., USA.

Introduction are used to calibrate testing instruments. Today, fastness

The American Association of Textile Chemists and
Colorists (AATCC) defines colorfastness as “The
resistance of a material to any chance in any of its color
characteristics, to transfer of its colorant(s) to adjacent
materials, or both, as a result of exposure of the material
to any environment that might be encountered during
the processing, testing, storage, or use of the material.”1
One such exposure is that of light. AATCC defines
lightfastness as “the property of a material, usually an
assigned number, depicting a ranked change in its color
characteristic as a result of exposure of the material to
sunlight or an artificial light source.”1
Colorfastness to agencies such as light, water, or
perspiration can be measured via a standard test. AATCC
has, as a major part of its mission, the development of
such standard tests. For lightfastness, the quantity and
quality of light impinging on a specimen has been dif-
ficult to assess, and the use of dyed fabrics as “control”
materials in light exposure has been part of the AATCC
lightfastness test method since the 1940s. AATCC’s
standard materials consist of 8 blue wool fabrics (L2 to
L9) dyed with varying ratios of two dyes, C.I. Mordant
Blue 1 and C.I. Solubilized Vat Blue 8.2
The former is fugitive in light and the later has
excellent fastness. Each succeeding standard requires
approximately twice the exposure to fade to the same
degree. These standard fabrics are still used today despite
better control and measurement of light exposure, and
is evaluated on the basis of standard fading hours and
standard fading units.3 In AATCC’s Test Method 16,
exposure is continued until fading to a gray scale change
of 4 is reached and the number of fading units that
produced that change is quoted as the colorfastness.
In addition to the AATCC blue wool standards, ISO
or International Organization for Standardization Blue
Wool also exists. However, they are used to determine a
category for the lightfastness properties of a concurrently
exposed material. Thus, after exposure to fade the test
specimen to step 4, the test material is compared to the
Blue Wool standards and a judgment is made based on
which level of ISO Blue Wool matched the material best
based on fading results.4
One particular AATCC standard is the most widely
used. Standard L4 fades to an extent that corresponds to
the required standard for a wide range of textile materials:
it fades to gray scale step 4 (defined for this color as a
change of 1.7 ±0.3 ∆E CIELAB) after 20 “fading units”
of exposure. The production of this color change on
standard L4 defines 20 AFUs for a given machine. The
problem facing AATCC and other standards institutions
is that C.I. Solubilized Vat Blue 8 is no longer manu-
factured, and thus future supplies of this long-standing
standard are unlikely once existing stocks run out.
Standard L2, dyed only with C.I. Mordant Blue 1, is
likely to remain available, and has been accepted as an
alternative calibration standard, but a replacement for L4
is still desirable.

JUne 2009 AATCC Rev i e w 43

 Table III.
Stu dent Paper

Round Two Candidates and Lightfastness Results

TABLE I. Dye Commercial Methoda
Auxiliary Composition Results Round 2
(% owf) Name
Method Components pH ∆ECIELAB ∆ECMC GS Manual
1 – Neutral 20 g/L ammonium acetate (2:1) Values Eval.
5 g/L Albegal B and should weigh 5 Acid Resorcine 2,3 3.93 1.62 3.90 4
1000 g with water (deionized) Orange 24 Brown G
2 – Acid Milling 5 g/L acetic acid (0.25) Conc
50 g/L sodium sulfate and should weigh 4 Acid Nylosan 1,2 4.69 1.90 3.62 4
1000 g with water (deionized) Orange Orange SL
3 – Acid 14 g/L 70% sulfuric acid 116 (0.25)
Leveling 50 g/L sodium sulfate and should weigh 3 Acid 3.07 1.23 4.19 5
1000 g with water (deionized) Orange
116 (2.0)
This study set out to examine a range of acid dyes Acid Red 4 1.46 0.61 4.68 4
applied to wool, to see if any readily available dye has (0.25)
fading characteristics comparable to the L4 standard. Acid Red 4 Atlantic Acid 3 0.99 0.40 4.30 4
Wool fibers require acid dyes. Acid dyes are divided into (0.75) Eosine G
Conc
acid leveling, acid milling, or neutral dyeing types.
They are generally dyed at the boil with pH carefully Acid Red 4 1.65 0.56 4.45 5
(2.0)
controlled to ensure a balance between good
exhaustion and level dyeing.5,6 Acid Red 1.77 0.71 4.52 4
73 (0.25)

Experimental Procedures Acid Red

73 (0.75)
Croceine
Scarlet Moo
2,3 0.92 0.35 4.76 4-5

Acid Red 1.06 0.42 4.66 5

The dyes for this project were chosen from our labora-
73 (2.0)
tory’s dye library. Initial choice was based on dyes that
had generic names, were well established and were sold Acid Red 2.78 1.26 3.83 3-4
131 (0.25)
by three or more manufacturers. Yellow dyes were omit-
ted. Published fastness information from the Colour Index Acid Red Polar 1,2 1.36 0.58 4.52 4
131 (0.75) Brilliant Red
was used to eliminate dyes of obviously high or 3 BN
low lightfastness.
Acid Red 0.78 0.39 4.72 5
Fifty-five dyes were identified that fit these criteria. For 131 (2.0)
each candidate dye, a 0.2% solution was prepared. 2 g
Acid Red 3.50 2.03 3.47 3
samples of plain weave, worsted wool fabric were labeled
151 (0.25)
and wetted out in 1 g/L nonionic detergent. Auxiliary
Acid Red Nylosan Red 1,2 3.12 2.09 3.74 3
solutions (Table I) were prepared and matched with the
151 (0.75) F-2R
dyeing method of the dye given in the Colour Index.
Dyeings of 0.25%, 0.75%, and 2% owf were performed Acid Red 1.10 0.74 4.61 4
151 (2.0)
at 50:1 liquor ratio with 4 mL of the appropriate auxil-
iary. Dyeings were heated at 4F per minute to 210F and Acid Red 3.74 1.72 2.93 3
243 (0.25)
dyed at that temperature for 1 h before cooling to 140F.
After dyeing, the samples were removed from the Acid Red Sulfonine 1,2 7.19 3.48 4.38 3
243 (0.75) Brilliant
machine, rinsed well, and air-dried. Half of each dyed Red B
specimen was stapled into a black card sleeve and loaded
Acid Red 1.50 0.78 4.24 4
into an Atlas
243 (2.0)
Table II. Ci-35 Weather-
Acid Violet Xylene Violet 3 4.11 2.20 3.60 2-3
Final Dyeings Ometer: this
1 (0.25) RL Conc
Dye Name % owf
machine uses a
3500W water- Acid Violet 2.38 1.48 3.85 4
1 (0.75)
Acid Blue 45 0.25, 0.5, 0.75, 1.0, 1.5, 2.0 cooled xenon arc
lamp to simulate Acid Violet Anthralan 2,3 4.93 0.04 3.86 4
Acid Violet 43 0.5, 0.75, 1.0, 1.5, 2.0 2.5 43 (0.75) Violet 3B
the effects of
sunlight on Acid Violet 5.26 2.28 3.76 4
Acid Orange 116 0.75, 1.0, 1.5, 2.0 2.5, 3.0
43 (2.0)
colored materials.
Acid Blue Nylosan Blue 3 1.99 0.87 4.52 4
25 (0.75) 2AL

44 AATCC R e v i e w www.aatcc.org June 2009

 Stu dent Paper
Acid Blue 1.44 0.76 4.42 4 Acid Red 1 Azo Rhodine 3 1.22 0.39 4.46 5
25 (2.0) (7.5) 2G Extra
Conc
Acid Blue 1.05 0.60 4.50 4
40 (0.25) Acid Red 1 0.68 4.00 4.77 5
(2.0)
Acid Blue Nylosan Blue 3 1.80 0.93 4.32 4
40 (0.75) E-2GL Acid Violet 3.59 1.74 3.30 2
7 (0.25)
Acid Blue 0.77 0.39 4.64 4-5
40 (2.0) Acid Violet Azo Rhodine 3 3.82 1.85 3.85 2-3
7 (0.75) 6B
Acid Blue 2.73 1.28 3.91 3-4
45 (0.25) Acid Violet 1.50 0.78 4.11 4
7 (2.0)
Acid Blue Alizarine 3 2.19 1.12 4.14 4
45 (0.75) Light Blue B Acid Violet 2.37 1.34 3.48 3-4
Conc 90 (0.25)
Acid Blue 3.45 1.80 4.18 5 Acid Violet Orcolan Neut 1,2 1.88 1.01 4.32 4
45 (2.0) 90 (0.75) Bordeaux
BSB
Acid Blue 1.03 0.56 4.42 4
62 (0.25) Acid Violet 0.89 0.61 4.70 4-5
90 (2.0)
Acid Blue Brill.Alizarine 2,3 1.81 0.72 4.55 4
62 (0.75) Light Blue Acid Blue Nylomine 3 1.72 0.93 4.65 4
3FR 41 (0.25) Blue BB
Acid Blue 3.16 1.20 4.31 5 Acid Blue 3.01 1.41 4.73 4
62 (2.0) 41 (0.75)
Acid Blue 0.94 0.47 4.61 4 Acid Blue 2.93 1.51 4.44 4
78 (0.25) 92 (0.25)
Acid Blue Alizarine 2 2.22 1.01 4.54 4 Acid Blue Atlantic Fast 2 1.15 0.76 4.32 5
78 (0.75) Light Blue 92 (0.75) Wool Blue R
AR Acid Blue 0.91 0.64 4.12 5
Acid Blue 3.61 2.42 4.09 5 92 (2.0)
78 (2.0) Acid Black Neutrichrome 1 0.23 0.16 4.59 4-5
Acid Blue 1.42 0.73 4.47 4 194 (7.5) Black M-R
129 (0.25) a 1 = Neutral Dyeing

Acid Blue Sandolan 2 1.55 0.75 4.46 4 2 = Acid Milling

129 (0.75) Fast Blue R 3 = Acid Leveling
Conc
Acid Blue 1.75 0.97 4.42 4
129 (2.0)
A sample of the current L4 standard was also loaded for
later comparison, and the samples then received 20 h
Acid Green Napthol 2,3 1.95 1.95 3.51 4
20 (7.5) Green
of exposure.
Black B The change in color of each sample was measured
Acid 0.85 0.77 4.02 3-4
using a portable spectrophotometer (Datacolor
Brown 14 Microflash). The data were collected in terms of CIELAB
(0.25) color difference (the scale that is currently used to
Acid Resorcine 2 3.48 2.56 4.30 4 measure the change in L4), CMC (2:1) color difference
Brown 14 Brown R (a scale that corresponds more closely to visual color
(0.75) difference) and grey scale rating (a subjective version of
Acid 2.20 1.85 4.31 5 the scale used in visual evaluation). As a check, the color
Brown 14 change was also evaluated visually against a grayscale
(2.0) using the procedure outlined in AATCC Evaluation
Acid 5.11 1.83 3.79 4 Procedure 1.
Orange 7 Of the 55 candidates, 24 were identified with fading
(0.25) characteristics close to L4 (in some cases only one or
Acid AAKASH 2,3 3.01 1.04 4.70 4 two of the depths of shade faded appropriately). These
Orange 7 #151- 24 were re-dyed using the same depths of shade in a test
(0.75) 9505015
of reproducibility. These dyes were also examined using
Acid 1.08 0.39 4.59 5 thin layer chromatography to determine their purity.
Orange 7
(2.0)
Dyes consisting of several components might vary (along
with their lightfastness) when prepared by different
Acid Red 1 1.82 0.88 4.25 4
manufacturers. Chromatography was carried out on
(0.25)

JUne 2009 AATCC Rev i e w 45

Stu dent Paper

Table IV. TABLE V.

Criteria Judgment Results (Nine Dyes from Round Two) Final Three Dye Candidates and Their Lightfastness Results

Dye Name % ∆ECIELAB ∆ECMC Manual GS

Criteria Dye (% owf) Lighfastness Testing # owf (2:1) Evaluation Value
Meta Manufact.
Acid Blue 45 0.25 3.58 1.88 3 3.10
∆ECIELAB ∆ECMC GS
Acid Blue 45 0.5 2.00 0.97 3-4 4.23
(2:1) Value
Acid Blue 45 0.75 2.12 1.01 3-4 4.35
1, 2, 3, 4 Acid Orange 24 (0.25) 3.22 1.50 3.90 7
Acid Blue 45 1 2.21 1.09 3-4 4.21
5 Acid Orange 116 (0.25) 3.42 1.42 3.62 12
Acid Blue 45 1.5 2.90 1.78 3-4 3.56
1, 2, 3, 4, 5 Acid Orange 116 (2.0) 3.08 1.13 4.19
Acid Blue 45 2 1.76 0.92 4 4.36
1, 3 Acid Red 131 (0.25) 2.88 1.21 3.83
Acid Violet 43 0.5 4.72 2.09 3 3.67
2, 3 Acid Red 131 (0.75) 1.10 0.50 4.52 6
Acid Violet 43 0.75 4.76 2.11 3-4 3.76
2, 3 Acid Red 131 (2.0) 0.98 0.38 4.72
Acid Violet 43 1 4.50 1.94 3-4 3.78
4, 5 Acid Red 249 (0.25) 5.50 2.28 2.93
Acid Violet 43 1.5 4.43 1.92 3-4 3.86
3, 4, 5 Acid Red 249 (0.75) 3.27 1.29 4.38 8
Acid Violet 43 2 4.50 1.79 4 3.93
1, 2, 4, 5 Acid Red 249 (2.0) 2.42 0.99 4.24
Acid Violet 43 2.5 4.08 1.87 4 3.83
1, 2, 3, 4, 5 Acid Violet 43 (0.75) 4.56 1.93 3.86 8
Acid Orange 116 0.75 2.03 0.77 4 4.39
1, 2, 3, 4, 5 Acid Violet 43 (2.0) 4.72 2.08 3.76
Acid Orange 116 1 1.13 0.51 4 4.21
1, 2, 3, 4, 5 Acid Blue 45 (0.25) 2.52 1.30 3.91
Acid Orange 116 1.5 1.12 0.41 5 4.75
1, 2, 3, 4, 5 Acid Blue 45 (0.75) 2.45 1.15 4.14 12
Acid Orange 116 2 1.32 0.58 4 4.60
1, 2, 3, 4, 5 Acid Blue 45 (2.0) 2.31 1.16 4.18
Acid Orange 116 2.5 1.09 0.42 4-5 4.69
1, 3, 4, 5 Acid Brown 14 (0.25) 2.26 1.11 4.02
2, 3, 4, 5 Acid Brown 14 (0.75) 1.27 0.87 4.30 8
The wool fabric dyed with the 24 dyes of round two
2, 3, 4, 5 Acid Brown 14 (2.0) 1.49 0.81 4.31 were then exposed to 20 AFU and measured following
3, 4, 5 Acid Violet 7 (0.25) 4.01 1.78 3.30 the same procedures. From the round two candidates,
1, 3, 4, 5 Acid Violet 7 (0.75) 2.56 1.21 3.85 12 the final selection for round three of dyeing was based
1, 3, 4, 5 Acid Violet 7 (2.0) 2.08 0.99 4.11 on five important criteria: their spectrophotometric GS
(grayscale) rating was 3.9-4.1, their depth after fading
4 Acid Blue 92 (0.25) 1.60 0.79 4.44
in comparison to the L4 standard (samples which faded
2, 3, 4 Acid Blue 92 (0.75) 1.74 1.10 4.32 6 differently at different depths were noted), their relative
1, 2, 3, 4 Acid Blue 92 (2.0) 1.55 1.47 4.12 brightness, and easy availability (defined in this case by
a 1 - 3.8-4.2 GS Value their being offered by at least eight manufactures). Dyes
2 - Approximate Depth of L4 not meeting these criteria were eliminated from the study
3 - Not very Bright at this stage. A summary of the results can be viewed in
4 - More than 2 gradations fading to 4
5 - Manufacturers Number 8 or More
Table IV. Based on published chemical structures, those
that would be easiest to prepare with least isomeric varia-
polyester plates pre-coated with cellulose powder, using tion were emphasized.
n-butanol:ethanol: water (4:2:1) and n-butanol:methanol: Nine dyes that passed all of the criteria after the
ammonia: water: pyridine (5:2:3:3:3) as eluents. An second round of dyeing and testing might be worthy of
example is shown in Fig. 1. further examination. This project focused on three (Acid
Blue 45, Acid Violet 45, and Acid Orange 116) which
were dyed at a range of concentrations (shown in Table
II) to find the closest match to the L4 standard at these
levels, and also to examine the degree to which fading
varied with depth of shade. For this stage of the project
the weight of wool dyed was doubled to 4 g.

Results and Discussion

The 55 dyes are listed (together with small colored
Fig. 1. Thin layer chromatography. swatches) in Fig. 2. The 24 dyes that faded to approxi-

46 AATCC R e v i e w www.aatcc.org June 2009

 Stu dent Paper
Table VI.
Final Dyeing GS Value Relationships

Dye Name % ∆ECIELAB ∆ECMC AATCC Manual

owf (2:1) Fastness Evaluation
Proc. 1
Acid Blue 45 0.25 3.58 1.88 3 3
Acid Blue 45 0.5 2.00 0.97 4 3-4
Acid Blue 45 0.75 2.12 1.01 4-5 3-4
Acid Blue 45 1 2.21 1.09 4 3-4
Acid Blue 45 1.5 2.90 1.78 3-4 3-4
Acid Blue 45 2 1.76 0.92 4-5 4

ducible in different labs and in different apparatus.

Fig. 2. Original 55 acid dyes in light, medium, and dark gradations.
mately the correct level after round two of the dyeing
process are listed in Table III, together with the color
change data after 20 AFUs of exposure.
The nine dyes (and depths) that met the more
stringent criteria were 0.25% owf Acid Orange 24; 2.0%
Acid Orange 116; 0.25% Acid Red 131; 2.0% Acid Red
249; 0.75% and 2.0% Acid Violet 43; 0.25%, 0.75%,
and 2.0% Acid Blue 45; 0.25% Acid Brown 14; 0.75%
and 2.0% Acid Violet 7; and 2.0% Acid Blue 92. The
color changes on exposure to 20 AFUs for these dyes are
listed in Table IV. It was felt that any of these might be
worthy of further examination in more detail. The light
fading of the three dyes that were examined in greater
detail is shown in Table V. The effect of depth of shade
on fading is small, suggesting that a standard based on
any of them would be robust to shade variation.
Simply finding a dye that fades to the right level under
standard conditions does not give a full answer to the
need for an L4 replacement. The fading must be repro-
Reaction to Lightfastness - Final Dyeing
5 4. Brochure, Atlas Weathering Testing Guidebook, Atlas Material
4.5
4
3.5
GS Value
More importantly, the fading must match that of
L4 under inevitable variations of temperature and
humidity that occur in practice, and interlaboratory
testing would need to include such variations to
determine if the fading matches that of L4 under
those varying conditions. The relationships of the final
three dyes chosen are outlined in graphical form below in
Fig. 3.
Of the three dyes selected for the final round
of dyeing, Acid Blue 45 dyed at 0.5 or 1% owf showed
great promise in its relation to the L4 standard with a GS
Value of 4.23 and 4.21 respectively, whose lightfastness
results can be examined below in Table VI.
Conclusion
This project has taken the first steps in identifying
candidate dyes that in self-shade might provide a replace-
ment for AATCC standard L4. Several dyes are worthy
of investigation. Of those examined in depth here, Acid
Blue 45 would seem most promising.
References
1. AATCC Technical Manual, Vol. 83, AATCC, Research Triangle
Park, N.C., USA, 2008, pp23-34.
2. Pugh, Samantha L. and James T. Guthrie, Review of Progress in
Coloration, Vol. 31, 2001, pp41-55.
3. Collier, Billie J. and Helen H. Epps, Textile and Testing Analysis,
Prentice Hall, Upper Saddle River, N.J., USA, 1999.
Testing Technology LLC., 2003.
5. AATCC Buyer’s Guide, Textile Chemist and Colorist, Vol. 24,

3 No. 7, 1992, pp77-84.

2.5 Acid Blue 45
2 6. Colour Index, Third Edition, AATCC/SDC, 1971.
1.5 Acid Violet 43
1
0.5
Acid Orange 16 Author’s Address
0 Chelsea D’Andrea, University of Rhode Island,
0 0.5 1 15 2 2.5 3 35
46 N. Hull St., East Providence, RI, 02914, USA;
% owf
+1 401 527 4167; cvd3584@hotmail.com.

Fig. 3. Final dyeing GS value relationships

JUne 2009 AATCC Rev i e w 47

40 Years Ago...
In 1969, AATCC launched its first journal. We’ve been celebrating
this momentous event all year, but it wasn’t the only “first” that
year. Test your knowledge of history with the questions below. Send

40
an email to wymand@aatcc.org or visit www.aatcc.org/media
to submit your answers by June 30. Everyone with all five correct
answers receives a 40th-anniversary pen—and congratulations in
the August issue.

In 1969, skirts:

l eb r at i n
a) went from very long to very short.
e b) were knee-length.
c) went from very short to very long.
g
C

Years
d) stayed short.
1969 2009
ce
Publ

en

 On November 19, 1969, Pelé scored his 1000th football

is

h ®
l

in e
Exc
(soccer) goal in a match against Vasco da Gama. What
g
was Pelé’s career total for goals scored?

 On April 4, 1969, Dr. Denton A. Cooley performed the

first artificial heart implant. The artificial heart was lined
with fabric designed to promote formation of a smooth
cellular surface. Who developed the implant?

 In November 1969, the AATCC council was informed that

membership was nearly 9,600, up from 9,200 at the same
time in 1968. How much were the annual dues for a senior
member in 1969?

 On July 20, 1969,

Neil Armstrong took
his famous “one small
step for man, one giant
leap for mankind.”What Get Your Own
Piece of History
was the designation
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2009 Editorial Calendar
AATCC Review
In our upcoming issues…
JULY September
Swimwear The Denim Issue
Additional distribution at Outdoor Retailer, Utah, USA A look at eco-denim.
Design challenges, fit, performance, colormatching,
October
printing, quality control. Fabric must stand up to
Quality: Who Cares?
chlorinated water, sea water, high UV exposure, and
How do you maintain the same quality standards
frequent laundering.
throughout the world? Why is standardized
AUGUST testing important?
Fibers That Perform NOVEMBER
Performance and industrial fibers—a primer.
Intimates
What are the fibers and their applications?
How do the colors match? What are the design, fit,
merchandising, and performance challenges? How do
you maintain quality?

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