Chairmanrsquo s message

Welcome to the Fall edition of your CAD News newsletter published byJamie Przybylski As I sit here writing this message the leaves are changingcolors there is a noticeable crispness in the air the World Series is on TV andit is a reminder that summer has ended It is also the time of year when we gettogether in some city conduct our annual CAD RETECreg technical confer-ence This year was quite special because we celebrated our 50th anniversaryand that is quite special

Congratulations to Sandra Davis and her committee for organizing this very special RETECreg inLouisville KY The conference was a tremendous success with approximately 480 attendeeswhich makes it one of the best-attended conferences in our 50 year history The conference wasanchored by a strong technical program an interesting panel discussion and it featured over 60tabletop exhibitors and plenty of professional and social interactions The conference organizersread the surveys that you fill out and submit and they try and listen to you and this is evident inthe cities that are chosen the length and format of the conference and some of both the traditionaland new features of the RETECreg Finally I want to say thank you to everyone who attended andfinancially supported the conference The proceeds from our RETECreg support scholarships and

continuing education for the professionals in ourindustry We are insuring the future success ofour industry by developing the people who willlead the next generation of color scientists

Our next technical forum will be at theANTECreg in Cincinnati Ohio on April 22-24Scott Heitzman is chairing this event and he isbusy putting together a full palette of technicalpapers for you Please visit specadorg for moreinformation and you can find a link to register toattend as well

Our group continues to grow and evolve andthere are a couple of changes Id like to sharewith you First George Rangos has taken overthe Endowment Committee from JohnnySuthers George has served on the board forquite a long time and he has served in virtuallyevery capacity including the five year rotationthroughout the chair positions He is very capa-ble of managing this very important function ofour Division We would like to thank Johnny forhis years of leadership during which time he notonly managed the funds but he worked directly

continued on page 2

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fall issue

20122012

Table of ConTenTs

CliCk on arTiCle or page number

To go To page

Chairmanrsquos Message 12Mission Statement 2BOD Election Nominee Request 2Sponsorships 3Councilorrsquos Report 4Minutes of Board Link 4Sponsorships 5Color Mischief 7 6RETECreg 2012 Wrap-up 7Invitation to Attend our Board Meetings 7Scholarship Endowment Program 8Your Company Our Division 8Call for Papers RETECreg2013 9Social Media- LinkedIn 9Plastic Courses at Terra Community College 10Sponsorships 11Technical Article 12-19Sponsorships 15CAD BOD Directors Listing 20Other Contact Info 20

with the students that CAD was nurturing Secondly Id like to welcome Mark Freshwater as the newest member toyour Board of Directors Mark received the highest number of votes in the spring election and he will fill an openingthat was created recently We look forward to working with Mark and we are confident that he will bring new energyand ideas to the CAD

Please check the website often and look for emails from SPE about ongoing events in general I look forward to seeingeveryone in Cincinnati in April

Best Regards

Jim FiganiakCAD Chairperson

Chairmanrsquo s message - ConTinued

SPE CAD NEWS Fall 2012 page 2 wwwspecadorg

DisclaimerThe information submitted in this publication is based on current knowledge and experience In view of the many factors that may affect processibil-ity and application this datainformation does not relieve processors from the responsibility of carrying out their own tests and experiments neitherdo they imply any legally binding assurance of certain properties or of suitability for a specific purpose It is the responsibility of those to whom thisinformation is supplied to ensure that any proprietary rights and existing laws and legislation are observed

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spe Color amp appearanCe division

mission sTaTemenT

The Color and Appearance Division of SPE

strives to educate train inform and to pro-

vide professional interaction opportunities

to the global community involved in visual

performance and aesthetics of plastics

annual board eleCTions

of Color amp appearanCe

divisionDeadline for Nomination Submissions

December 15 2012

The Color amp Appearance Division of the SPE will beconducting its annual board elections in February 2013The election is open to SPE members with CAD astheir primary division Time commitment is four meet-ings per year including those held at ANTECreg andRETECreg and participation in CAD activities and ini-tiatives If you are interested or would like to nominatea colleague please contact Ann Smeltzer at the notedemail address or phone before December 15th Nominate a Colleague by emailing Ann Smeltzer atannsmeltzerclariantcom or calling 412-298-4373

Submit you nomination now

with the students that CAD was nurturing Secondly Id like to welcome Mark Freshwater as the newest member toyour Board of Directors Mark received the highest number of votes in the spring election and he will fill an openingthat was created recently We look forward to working with Mark and we are confident that he will bring new energyand ideas to the CAD

Please check the website often and look for emails from SPE about ongoing events in general I look forward to seeingeveryone in Cincinnati in April

Best Regards

Jim FiganiakCAD Chairperson

Chairmanrsquo s message - ConTinued

SPE CAD NEWS Fall 2012 page 2 wwwspecadorg

DisclaimerThe information submitted in this publication is based on current knowledge and experience In view of the many factors that may affect processibil-ity and application this datainformation does not relieve processors from the responsibility of carrying out their own tests and experiments neitherdo they imply any legally binding assurance of certain properties or of suitability for a specific purpose It is the responsibility of those to whom thisinformation is supplied to ensure that any proprietary rights and existing laws and legislation are observed

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spe Color amp appearanCe division

mission sTaTemenT

The Color and Appearance Division of SPE

strives to educate train inform and to pro-

vide professional interaction opportunities

to the global community involved in visual

performance and aesthetics of plastics

annual board eleCTions

of Color amp appearanCe

divisionDeadline for Nomination Submissions

December 15 2012

The Color amp Appearance Division of the SPE will beconducting its annual board elections in February 2013The election is open to SPE members with CAD astheir primary division Time commitment is four meet-ings per year including those held at ANTECreg andRETECreg and participation in CAD activities and ini-tiatives If you are interested or would like to nominatea colleague please contact Ann Smeltzer at the notedemail address or phone before December 15th Nominate a Colleague by emailing Ann Smeltzer atannsmeltzerclariantcom or calling 412-298-4373

Submit you nomination now

ech haintL and PsrrsoloCou Y

he tsech hastgmeni and P

Needou

cetLinwww

Ad

tcatnCo Ch336

moclanoitanretnIh

stgmeniPampvesitidAd

nruChselraCh336-255-6673 nLinruChselraCh

moclanoitanretnIhcetn

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Prompt deliveries from our warehouses across the county

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Brea CA 92821P 714-990-4300F 714-990-4302

wwwspectradyescom

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Pigments and Additives for the Plastics Industry

Clariant Corporation4000 Monroe Road Charlotte NC 28205Phone 8004414414wwwclariantcom

Leading Manufacturer of Complex Inorganic Color Pigments (CICP) bull Pigment Brown 24 Yellow 53 Blue 28 Green 50 Black 28 etcbull Environmentally Friendly Pigments Brown 48 etcbull Laser Marking Pigmentsbull Pigments for Biodegradable Plastics

Contact in Americas

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HIGH PERFORMANCE PIGMENTS FOR PLASTICS

Ferros Geodereg Complex Inorganic Color Pigments offer unsurpassed color quality and stability

The complete Geodereg line includes

Chrome Titanates l Cobalt Blues amp Greens l Nickel Titanates

Heat stable Blacks l Iron Free Browns l IR Reflecting Blacks

Ferro Corporation Performance Pigments amp Colors

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Phone 724-223-5900

Fax 724 223-2700 wwwferrocom

wwwshepherdcolorcom

Lintech has theColors and Pigments

You Need

SPE CAD NEWS Fall 2012 page 3 wwwspecadorg

The Color and Appearance Division (CAD) commits to the pub-lishing of at least three newsletters a year (four if there is sufficientmaterial to justify the extra issue) Each newsletter is electronical-ly distributed to our membership of nearly 1000) Each sponsorrsquosart directly links to the companyrsquos website

In addition we print one of these newsletters on 80gloss coatedstock All electronic versions are also posted on the SPE websitewhere it available for anyone to download

For the small donation of $300 per year we offer a business cardsized (2 x 35 inches) mention in our newsletter

We currently have the following slots available for sponsorship

(2) 2 x 35 inch or (1) 4 x 35 inch

If interested in learning more please contact

SHARYL REID Phone 8649682426

Email Sharyl_Reidusaschulmancom

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SPE CAD NEWS Fall 2012 page 4 wwwspecadorg

CounCilorrsquo s reporT

The Fall Council meeting was held on September 15 2012 in Dearborn MI The day before the Councilmeeting there were various committee meetings including Divisions Committee and ConferenceOversight Committee The Fall meeting is the election meeting at which time the next leaders of SPEare selected by the Councilors

MEMBERSHIP While membership has shown slow growth over the past couple years in the first halfof 2012 there has been 2 decrease in membership This has been attributed to reduced retention rates

and the scheduling of ANTECreg It is felt that the retention rates have been negatively impacted due to the difficulties asso-ciated with membership renewal using the website which are directly related to the management software being used bythe organization The scheduling of ANTECreg adversely impacted membership numbers because there were less than 12months between ANTECreg 2011 and ANTECreg 2012 therefore members who joined in order to attend ANTECreg 2011 atthe member rate were able to register for ANTECreg 2012 as a member without renewing their membership

FINANCIAL Despite budgeting more tightly for 2012 than 2011 the mid-year financial review has shown a $52000shortfall The second half is typically lower in revenue for the organization so there is little expectation of making up thisshortfall Additionally the impact of ANTECreg Mumbai is unknown The worst case scenario has a year-end shortfall of$350000 for the organization A revised budget is being prepared to minimize the shortfall

ELECTION Vijay Boolani was elected by the Councilors as the President-Elect Additionally Raed Al-Zubiwas elected as Senior Vice-President and Dick Cameron was elected Vice-President

Sincerely

Sandra DavisCAD Councilor

ediTorrsquo s noTe

Hopefully many of you had a chance to attend the past CAD RETECreg in Louisville this fall Itwas a historic event the 50th anniversary conference conducted by the Color and AppearanceDivision of the SPE Sandra Davis and her team should be commended for making it success-ful and memorable One thing that made it memorable for me was the attendance of one specialperson Robert Charvat Not only has Bob been a good friend and mentor to many of us on theboard he has the distinction of being one of the founding members of the CAD and not onlyattended the very first conference but also helped finance it Bob was recognized at the awardsreception and given a plaque listing all of the conferences to commemorate his involvement

throughout the years I have included a picture of Bob and his plaque Bob is no longer a board member but hestays involved and is always in our hearts One other thing I would like to mention is that I am the professor in TerraState Community Collegersquos Coloring of Plastics program which Bob was also instrumental in starting and nurturingFor those of you that might have not seen it in Plastics News in August there was a nice article about our programAs always I ask you to spread the word about Terra to your colleagues and contacts that may be in the need of colortraining If you have not had a chance to see the article click here to the linkHave a save and happy Holiday season

Jamie PrzybylskiCAD Editor

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Organic Pigments Inorganic Pigments

Pigment Preparations

Heucotech Ltd 99 Newbold Road Fairless Hills PA 19030

wwwheubachcolorcom 215-736-0712

Organic amp InorganicPigments and Preparations

(416) 253-4297 hkennedydominioncolourcomwwwdominioncolourcom

DOM 653 ProgramAd_retec09_v2_ 72209 217 PM Page 1

Quality Formulation oF

Color amp additive ConCentrates

wwwtechmerpmcom

18420 laurel Park road 1 Quality Circle

rancho dominguez Ca 90220 Clinton Tn 37716

(310) 632-9211

(865) 457-6700

ISHIHARA CORPORATION (USA)l TiO2 l Ultra-fine TiO2

l Nickel Titanates l Chrome Titanatesl Conductive Pigments

600 Montgomery Street Tel (415) 421shy8207

San Francisco California 94111 Fax (415) 397shy5403wwwishiharacom

page 5

SPE CAD NEWS Fall 2012 page 5 wwwspecadorg

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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg

Color misChief 7Can sTorage of samples or sTandards

be a problem

The answer to the title question is ldquoOh my yes it canrdquo

Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong

However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure

Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers

Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability

If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations

A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature

One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples

This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle

Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon

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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg

The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry

In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly

The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)

Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years

reTeCreg 2012 Wrap-up

inviTaTion To aTTend our Cad board

meeTings

The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg

The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg

Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information

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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg

soCieTy of plasTiCs engineers

endoWmenT sCholarship program

for The 2013 ndash 2014 sChool year

The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships

Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school

scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools

scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the

Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships

application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry

Dear Members

Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website

We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January

Click here for the link to view httpwwwspecadorgindexphpnavid=28

BOARD MINUTES

SPE CAD NEWS Fall 2012 page 9 wwwspecadorg

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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics

Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom

Venue Baltimore Marriott WaterfrontBaltimore MD

Call for papers

ConneCt With sPe Cad via soCial media

Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements

Group Name SPE Color amp Appearance Division Group ID 152108

wwwlinkedincomgroupsgid=152108

September 22-24 2013 Society of Plastics Engineers

Color andAppearance

Division

Abstract Deadline February 2013 Event September 22-24 2013

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a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics

its ability to provide eature of the Te fy distinctiverA v

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(online) coursesra plastics program is

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Click here

Plastics News Article

highlighting Terra

SPE CAD NEWS Fall 2012 page 10 wwwspecadorg

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page 11

DuPonttrade TishyPurereg titanium dioxide

duPont titanium technologies8004419485

wwwtitaniumdupontcom

The DuPont Oval DuPont trade The miracles of sciencereg and TishyPurereg

are trademarks or registered trademarks of EI du Pont de Nemours and Company

PoLYmers Light amp sCieNCe

Polymers Light and the Science of TiO2

Color Concentrates and

single Pigment dispersions

for all Thermoplastic Polymers

A World of Color Perfection since 1964

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Operations amp

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(215) 997-2221

wwwpenncolorcom

BTitanium dioxide

Brutile amp anatase

Bhigh Performance organic Pigments

B dPP reds hP yellowsB PvC additives

B lubricants amp stabilizers

364 Johnny Mercer blvd b-7 294 - savannah ga 31410

Tel (912)507-8972 - lwaltersagrofertinccom

wwwagrofertinccom

World leader in effect

Pigments

one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275

wwwemdchemicalscom

A Complete Line of DyestuffsInorganic Pigments and

Organic Pigments forPlastics amp Fibers

lanXeSS corporation

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Since 1986

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SPE CAD NEWS Fall 2012 page 11 wwwspecadorg

SPE CAD NEWS Fall 2012 page 12 wwwspecadorg

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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions

author roger reinicker basf Corporation newport de 19804

Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered

introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix

For example some plastic constructions may be pressurized others need to have good impact strength

In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test

pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional

table 1 Some details of ASTM D3218 section 17 filter test

reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)

melt or metering pump optional shy any type

screens composition 304 or 316 stainless steel

screens diameter 2235 inches (567 mm)

screens mesh in order 32550 32550 200X1200 DTW50 32550

breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles

volume of material 025 x ratehr plus 30 pounds

temperature 2 65˚C

throughput not specified

max pressure 5000 psig or 345Mpa

procedure purge 15 minutes then run 30 pounds

measure of rate of filter increase megapascals per kg or psi per pound

SPE CAD NEWS Fall 2012 page 13 wwwspecadorg

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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab

screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness

Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400

Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters

continued from page 12

1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html

TyPE 1 35 ndash 38 25

screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm

screen 2 square mesh plain weave 063 mm 04 mm

TyPE 2 23 ndash 26 20

screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm

screen 2 square mesh plain weave 063 mm 04 mm

TyPE 3 16 ndash 18 10

screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm

screen 2 square mesh plain weave 025 mm 016 mm

screen 3 square mesh plain weave 063 mm 040 mm

estimates

TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2

AbSOLuTE

RETENTION

mICRONS

NOmINAL

RETENTION

mICRONS

TAbLE 2

continued on page 14

SPE CAD NEWS Fall 2012 page 14 wwwspecadorg

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TAbLE 3

continued from page 13

PARAmETER TEST STANdARd ENGLISH uNIT

single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil

The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute

extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling

breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided

Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our

laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation

continued on page 15

SPE CAD NEWS Fall 2012 page 15 wwwspecadorg

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Under the standard the pure pigment content and total throughput weight is set for two different mixtures

Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments

Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations

The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations

Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams

interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles

Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow

The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result

Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters

continued from page 14

continued on page 16

SPE CAD NEWS Fall 2012 page 16 wwwspecadorg

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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests

The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing

with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt

pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined

industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications

Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware

For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged

US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased

Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition

continued from page 15

continued on page 17

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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg

Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The

test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test

The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications

Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen

What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature

2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high

pressures

Table 4 Correlation between local test and the DINEN test using commercialdispersions

In-house Pressure Rise Test

Pigment inthe conc

PressureRise in

psigTimemin

165X1400psimin

325 meshpsimin

PFStatus

Type 125

Type 180

Type 225

Type 325

corre-lation

Fail ifgt267 Fail if gt25 barg barg barg barg

1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG

10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG

ISODIN EN13900-5

some decomposition noted during local test

Table 4Local test and the DINEN test as locally adapted

local test EN13900-5screw diameter

screw rpmscrew LD

screw amp barrel wearfeed rate

developed pressure variable bar

polymer

12 MFI PP

(unstabilized)40MFI PP pellettemperature

Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment

Table 4 Correlation between local test and the DINEN test using commercial dispersions

continued from page 15

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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg

Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment

Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard

ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH

ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors

The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates

Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo

The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test

TAbLE 4 Local test and the DINEN test as locally adapted

LOCAL TEST EN13900-5

screw diameter 1 (254mm) 20 mm

screw rpm 75 102shy105

screw LD 25 25

screw amp barrel wear unknown (old) new condition

feed rate 44gmin (varies) 40 gmin

developed pressure variable constant at 435 bar

polymer 12 MFI PP homopolymer flake 40MFI PP pellet

(unstabilized)

temperature 5100F (2650C) 4460F (2300C)

3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004

continued from page 17

continued on page 19

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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg

FIGuRE 1 Filter Value Apparatus

FIGuRE 2 Fiber Value Pressure Trace

FIGuRE 3

Test screen with

pigment particles

PigmentConcentrate

BreakerPlate

meltPump

screen Pack

Feedback Loopto extruder

Drive

extruder

to

recorder

Pre

ssu

re

bar

Time

Pmax

Pmax - P

Ps

Ts Tp

PT

PE

Color amp appearanCe division board of direCTors

OFFICERSChairman

James Figaniak 215shy736shy1126

LTL Color CompoundersInc

jimfiganiakxxxltlcolorcom

Chair-Elect

Ann Smeltzer 412shy298shy4373

Clariant Corporation

annsmeltzerxxxclariantcom

Finance Chair

Betty Puckerin 812shy466shy9828

Ampacet Corporation

Bettypuckerinxxxampacetcom

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Sun Chemical Corporation

scottheitzmanxxxsunchemicalcom

Councilor

Sandra Davis 302shy999shy2540

DuPont

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Treasurer

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brucemulhollandxxxticonacom

Secretary

Jeff Drusda 570shy668shy8321

Silberline Manufacturing Co Inc

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dIRECTORS until 2014Sharon Ehr 616shy494shy7577

Uniform Color

sehrxxxuniformcolorcom

Steve Esker 614shy679shy4677

Paramount Colors Inc

steveeskerxxxhotmailcom

Mark Freshwater

Lansco Colors

markxxxpigmentscom

Steve Goldstein 508shy829shy6321

Clariant Corp

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Larry Nitardy 423shy312shy3439

ComAssist

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Jamie Przybylski 419shy559shy2459

Terra Community College

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Austin Reid 228shy255shy2362

DuPont

Austinhreidshyjrxxxusadupontcom

Mark Tyler 859shy372shy3221

Ticona

marktylerxxxticonacom

dIRECTORS until 2015Earl Balthazar 817shy719shy0224

SpectroTechs Color Solutions

ebalthazarxxxtxrrcom

Alan Bodi 419shy356shy7308

PolyOne

AlanBodixxxPolyonecom

Hal Button 330shy535shy2100

Akrochem

halbuttonxxxakrochemcom

Jack Ladson 215shy369shy5005

Color Science Consultancy

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Frank Lavieri 401shy461shy4100

Lansco Colors

FrankxxxPigmentscom

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George Rangos 724shy229shy5371

Ferro Corporation

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A Schulman Inc

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EMD Chemicals

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Tracy Phillips 770shy995shy0887

Uniform Color

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Tom Rachal 405shy775shy5014

Tronox LLC

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Roger Reinicker 302shy992shy1252

BASF Corporation

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Johnny Suthers 423shy229shy4258

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Brian West 865shy457shy6700

Techmer PM LLC

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Please note The email addresses above contain xxx which should be ignored when actually emailing

The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless

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CDs PerfectBinding

OmniPress

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ACE Chair Roberto Todesco

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National Plastics Center

Museum amp Collections Director

Marianne Chalifoux

210 Lancaster Street

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SPE Headquarters

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CAD Newsletter Publication

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WebSite HostDesigner

Becky and Jeremy Hodge

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OTHER USEFUL CONTACTS