Hexamoll® DINCH for medical applications

Quick Links

2

Medical Devices & Soft-PVC

Medical Device Market

Medical Device Materials

PVC & Medical Devices

Properties ofPVC-Medical

Devices

Regulatory InformationRegulatory Timeline of DEHP

ToxicologicalProfile

Human Biomonitoring

Approvals (EU, USA, Asia)

Evaluations for usein Med Dev.

Hexamoll® DINCH

Hexamoll® DINCHThe non-phthalate

plasticizer

Value Chain Integration

Capacities

Supply Chain Set-up

In Medical ApplicationsIntraveneous studies

Suitability for critical care

Examples of Applications in Use

Technical Aspects

Technical Information

1 Medical Devices & Soft-PVC

European Medical Device Market Western Europe accounts for ¼ of

global market (Germany 30% ofconsumption)

2.7% p.a. av. growth in Western Europe 2014-2019• Strongest growth in Norway

5.3% & UK 5.1% (reforms extra funding in healthcare sector)

• Slowest growth in Italy 0.8% (low economic growth, budgetrestrictions)

High pressure on margins, particularlyfrom co-operative purchasing andtenders

Medical Device Market

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Global Medical Plastics Market

Annual growth for plastic medical devices market: 7% until 2020

Most commonly used plastic is PVC (Highest growth has PP)

PVC has largest share in medical plastics (40%)

85% of Disposable Medical Devices are made of PVC:

• Annual growth of 12%

• Largest markets: BRIC, US, Japan, + EU: Germany, France, Italy & UK

• Disposability is fundamental to reduce the occurrence oftransfusion-transmitted diseases(pre-sterilized, single-use devices)

• Main applications

– Dialysis treatments– Blood contact applications (stabilizing effect on red

blood cells)– Other: respiratory & incontinence therapies

Sources: Medical Device Business (2015), Markets & Markets (2015), Freedonia (2014)

Medical Device Materials

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PVC & Medical Devices

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Increasing availability of

DEHP-alternatives

Growing public awareness of DEHP health

effects

Benfits of PVC Medical Devices

PVC Material market share 40%(esp. single-use disposables)

OEMs continue to offer PVC- product lines

BASF & PVCMed Alliance believe in the benefits of PVC …

•Long history of use•Stability•Compatibility•Transparency•Flexibility•Durability•Processing properties•Recyclability•Design capabilities•Affordability

… and promote the shift towards non-DEHP plasticizers!

Choice of Plasticizer

The right choice of plasticizer depends on the application

Risk = Hazard x Exposure

Alternatives to DEHP exist for all medicalapplications, but:

• Nutrition: TEHTM is not approved forfood contact, thus artificial nutrition(EU Regulation 10/2011)

• Blood contact: Hexamoll® DINCH is the only plasticizer that fulfills the RBC-stabilizing requirements for blood bags and is in commercial use

• Infusions: Sorption behaviors of TEHTM, DEHTP and Hexamoll® DINCH are equivalent

Properties of PVC Medical Devices

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PVC-Bag Inside Solution

Leaching

Adsorption

Absorption

Effect Interaction in PVC

LeachingThe plasticizer leaches out of the PVC-bag and enters the solution.

Nutrition solution Migration

Blood transfusions Migration Stabilization of RBC

AdsorptionAn active ingredient adheres to the inside of the PVC-bag, e.g. Diazepam

Pharmaceutical solutions Loss of effect

AbsorptionAn active ingredient enters the PVC-bag, e.g. Isosorbiddinitrat

2 Regulatory Update

Regulatory Timeline of DEHP

*Identified High Risk Groups in DEHP Risk Assessments, e.g. neonates, peripubertal males and pregnant females (Hemodialysis) and adults for treatmentslike heart transplantations or massive infusion of blood (trauma patients)

REACHOct 2008Inclusion on SVHC candidate list(Human health)

CLPJun 2009DEHP listing astoxic toreproductionCategory 1B

Medical Device Directive 2007/47/ECMar 2010• Labelling requirements according to CLP:

Hazard Statements H360Df• Justification requirement if used for

children, pregnant or nursing women

REACHDec 2014 (ongoing)DEHP inclusion on candidate list for itseffects to mammalsin the enviroment

REACHFeb 2015Sunset date forDEHP (human health – exempt: Med Device)

France2012Law 2012-1442 bans DEHP-containing tubesfor certainapplications

2001 2006 2007 2008 2009 2010 2011 2012 2013 2014 2015 2016 2017 2018

US FDA*

HealthCanada*

GermanBfArM*

EU SCENIHR*

DanishEPA*

SwedishKEMI*

67/548/EECAug 2001DEHP Repr. Cat.2

Medical Device Regulation (EU) 2017/745May 2017 (Fully enforced in 2020)• 0.1% concentration limit for Cat. 1A and 1B

CMRs and EDCs• Includes justification requirements• SCHEER published preliminary guidelines on

use of phthalates 15.03.2019public hearing: 04.04.2019, deadline for public consultation: 29.04.2019

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REACHReg (EU) 2018/2005:amendment of REACH Annex XVII 51broad restriction (some exemptions) to 0.1%by weight starting 07.07.2020

REACHAug 2013Applicationdeadline forauthorized uses

Notification from Arabian Pensinsula1 towards WTO:Restriction on DEHP, BBP, DBP, DIBP from July 22, 2021 onwards2:- max. permissible concentration (in weight):

0.1%- will apply to medical devices, incl. in vitro,

monitoring and control instruments incl. industrial use

1participating states: Bahrain, Kuwait, Oman, Qatar, Saudi Arabia, United Arab Emirates, Yemen2 will not apply to medical devices placed on the market before July 22, 2021

DINP: Regulatory Status (06/19)

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1999 2005 2008 2009 2013 2014 2015 2017 2018 2019

EU bans DINP for mouthabletoys and childcare articles (interim ban)

US Consumer Product Safety Improvement Act (HR 4040) poses an interim ban on mouthable toys and childcare articles.

ECHA completes re-evaluation of DINP toy-restriction

Danish EPASep 2013 Suspects DINP to be endocrine disruptive at high exposure levels.

Per recommendation of the US CHAP, the interim ban of DINP in mouthable toys is converted into a permanent ban.

ECHA REACH update for DINP: Toy restrictions are maintained Com. Reg. (EU) 2015/326

Danish EPAFeb 2015 Submits dossier to ECHA proposing classification.

Danish EPAApril 2017 Submits reworked dossier proposing classification in:>Cat. 1B Developm.>Cat. 2 Fertility

ECHA opens 45 days of public consultation until May `17 of the Danish CLH Dossier.

RAC agreed not to classify DINP for reproductive toxicity March 7, 2018

European Plasticizers contributed to the public consultation phase by submitting substantial comments based on the available toxicological data, concluding that: a classification of DINP is not warranted.

Permanent restriction in toys and childcare articlesDirective 2005/84/EC

Launch of the re-evaluation of the restriction as set out in REACH Annex XVII (52a)Com. Reg. (EC) No 552/2009

The State of California lists DINP as carcinogenic in Proposition 65 leading to labelling requirements in Cal.

May 2019: American Chemistry Council submitted DINP for risk evaluation under TSCA* to US EPA** (it was identified in the 2014 update to the TSCA work plan)

*Toxic Substance Control Act** US Environmental Protection Agendy

Medical Device Regulation (EU) 2017/745

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Replacing Medical Device Directive 93/42/EEC (amended by 2007/47/EC)

Timeline:

• Published in the Official Journal on May 5th

• Enforcement in a tiered manner

• Completion/ full enforcement in three years (May 2020)

Includes a 0.1% concentration limit for Cat. 1A and 1B CMRs (carcinogenic, mutagenic, reprotoxic) and EDCs (endocrine disrupting chemicals) ( DEHP)

Justification would need to be based on thorough scientific analysis and arguments why any possible substitutes cannot be used

The scientific committee on health, environment and emerging risks (SCHEER) will draft guidelines and conduct risk-benefit assessments on the use of phthalates (beginning September 2017, that shall be ready before March 31, 2019) and subsequently for CMRs and EDCs

Hexamoll® DINCHExcellent toxicological profile

Hexamoll® DINCH does NOT show any of these adverse effects: Environmental hazards Peroxisome proliferation Accumulation within the body Carcinogenicity Reproductive hazards

Testicular toxicity Impairment of fertility Developmental toxicity Teratogenicity Endocrine disruption

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Complete regulatory database regarding phys-chem, eco- and toxicological data available

Study reports have been evaluated worldwide by respective competent authorities/ commissions, e.g. EU (SCENIHR, EFSA) Germany (UBA/ BfR) Switzerland (BAG) Netherlands (RIVM) France (ANSES) USA (NSF) Health Canada Australia (NICNAS) China (CFDA) Japan (PMDA/ MHLW)

Hexamoll® DINCHHuman Biomonitoring (HBM)

Human Biomonitoring

German EPA (UBA)* targeting to monitor plasticizers in human specimen

VCI** members developed Human Biomonitoring methods: Determination of urinary metabolites

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Hexamoll® DINCH Biomonitoring

3 volunteers, swallowed approx. 50 mg Hexamoll® DINCH/ person

Elimination into urine was monitored over 48h (max. elimination after ca. 5 hours)

HBM is based on the metabolites cx- and OH-MINCH

TDI by EFSA1

(µg/kg bw/d)

Average burden

(µg/kg bw/d)

Margin of Exposure

DEHP 50 17* 2.94

Hexamoll®DINCH 1000 0.14** 7140**

*EU RAR DEHP; based on conversion factors by Koch et al.** Schütze et al. 2014, Int J Hyg Environ Health 217(2-3):421-4261 Tolerable Daily Intake by the European Food Safety Agency

Exposure Hexamoll® DINCH metabolites can

be found in urine of 98% of the general public

Conversion of metabolite concentrations in urine to total systemic exposure to parent

Average exposure to Hexamoll®

DINCH: 0.14 µg/ kg bw/ d

*Environmental Protection Agencies (Umweltbundesamt)** Verband der chemischen Industry (i.e. Association of the chemcial industry)

The Risk Management Option Analysis (RMOA, 03/2016) undertaken by French Competent Authority (ANSES) and published by ECHA concludes: “No need to initiate further regulatory risk management action at this time.”

DIN EN ISO 10993Medical devices, based on Hexamoll® DINCH, comply with the requirements, e.g. absence of cytotoxicity, haemolysis, pyrogens, irritation and sensitization

Medical Device Regulation (EU) 2017/745 (formerly Directive 93/42/EEC)

Notified bodies confirm compliance with the new Medical Device Regulation (EU) 2017/745 and audit the medical device producers

No labelling or justification requirements for Hexamoll® DINCH based medical devices

European Pharmacopoeia entry as of January 18, 2018

Hexamoll® DINCHApprovals in Europe

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Hexamoll® DINCH®

Approvals in USA & Asia

USA FDA

● 510(k) process supported by FDA Master Files No. 16323 and 1484 applicable for registering a device based on Hexamoll® DINCH®, e.g. to substitute DEHP

US Pharmacopoeia● Hexamoll® DINCH® based devices comply with the requirements of USP Class VI

Asia In China and Japan medical devices must get approval by a competent authority Chinese FDA and Japan PMDA and MHLW have approved Hexamoll® DINCH® based medical

devices

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Hexamoll® DINCHEvaluations for use in Medical Devices

„Hexamoll® DINCH is one of the most promising alternatives to DEHP for medical devices“

Danish EPA (Environmental project1557, 2014)

Swedish Kemi (Report 4/15)

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3 Hexamoll® DINCH

The trusted non-phthalate plasticizer designed forclose human contact

Excellent toxicological profile with low migrationrates

Meeting technical requirements for broad range ofproducts

Approved & certified worldwide for manyapplications

Classified as “Accelerator“ within BASF‘s Sustainable Solution Steering Program

Trusted by leading brand owners

Hexamoll® DINCH The non-phthalate plasticizer

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OO

O

O

C9H19

C9H19

OO

C9H19

O

O C9H19

cis (90%) trans (10%)

The structural change in the ring makes the difference

3D - chairNon-aromatic

BASF value chain integrationBackward integration is our advantage

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Aldoli-zation

Hydro-formy-lation

Hydro-formy-lation

Dimeri-zation

2-Propyl-heptanol

Isononanol

n-Butene PA

Palatinol® N (DINP)

Palatinol®

10-P (DPHP)

Raffinat II

o-Xylene

Hexamoll® DINCH capacity has continously expanded

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BASF continuously supplies the increasing market demand from two separately operating Hexamoll® DINCH plants in Ludwigshafen

Decision to build a second plant with a capacity of 100 000 mt/a by 2014

2014Expansion to 100 000 mt/a complete

Start up of 25 000 mt/aplant

Pilot production of 200 mt

Start as research project “Sustainable Plasticizers”

Capacity of 200 000 mt/a

Local Tank Farms Ludwigshafen Mannheim Samarate Tarragona

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Well-designed infrastructure to accompany market growth BASF continuously invests in infrastructure to maintain supply security.

Hexamoll® DINCH supply chainProduct availability & supply security are priority

4 Hexamoll® DINCH in Medical Applications

Hazard Hexamoll® DINCH: No substance-related systemic

toxicity, NOAEL* (rat, i.v.) <= 300 mg/ kg body weight (David et al., 2015) • No peroxisome proliferation• No testicular effects• No thyroid effects• No kidney damage• Short elimination half-life (5-12 h)

DEHP: NOAEL* (rat, i.v.) is at 60 mg/ kg body weight (Cammack et al., 2003)

Hexamoll® DINCHIntravenous studies for medical applications

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Risk-Benefit Analysis: Hexamoll® DINCH in IV applications improves patient safety

Exposure Comparing dose level (migration) to NOAEL:

The Margin of Exposure improves by a factor of 10 when DEHP is substituted by Hexamoll® DINCH in IV tubing

Margin of Exposure compares NOAEL to the dose level resulting from plasticizer migration into IV infusion solutions:

• 10 mg for Hexamoll® DINCH (customer data)

• 20 mg for DEHP (Loff et al., 2000)

⇒ reduced exposure⇒ eliminated hazard

*No Observed Adverse Effect Level

No adverse effects of Hexamoll® DINCH regarding toxicity to reproduction identified in relevant animal studies• Prenatal toxicity studies (OECD 414) on rats (NOEL: 1200 mg/kg bw/day)

and rabbits (NOEL: 1000 mg/kg bw/day)

• Two generation reproduction toxicity study (OECD 416) on rats (NOEL: 1000 mg/kg bw/day)

Since more active metabolite is formed via the oral route as compared to the intravenous route (Huber et al., 1996), it is highly unlikely that the plasticizer shows toxicity to reproduction via the intravenous route• 28d repeated dose toxicity study in the rat on the intravenous route: NOAEL 300 mg/kg bw/day

EFSA (2006) and NICNAS (2012) evaluated the thyroid effects after oral administration in animal studies as not relevant to humans (EFSA TDI: 1 mg/kg bw)

Hexamoll® DINCHSuitable for critical care

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Hexamoll® DINCH suitable for medical devices for use in neonatology/ pediatrics

Hexamoll® DINCHSuitable for critical care

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IV Systems Blood Contact Artificial Nutrition Masks Dolls Gloves

• Disposable IV bags & tubings

• Infusion solutions

• RBC and PLT bags*

• Dialysis sets• Blood circuit

tubings• Heart-Lung

machine

• Enteral nutritionbags & tubings

• Respiratorymasks

• Protectivemasks

• Educationalmedical dolls

• Examinationgloves

Hexamoll® DINCHCommercially available medical applications

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All applications suitable for the use in critical care, e.g. neonatology/ pediatrics

More More More More More

* Red blood cells and platelet

Interaction of Nitroglycerin/ Diazepam with PVC tubes (Treleano et al., 2009)• Dose levels of these two active ingredients reaching the patient vary in the range of

+/- 10% when Hexamoll® DINCH -plasticized tubing is compared to DEHP plasticized tubing material Interaction of Diazepam with PVC films (Salloum et al., 2015)

• The drug sorption levels were equivalent for the different plasticizers (DEHP, DEHTP, TEHTM, Hexamoll® DINCH) Interaction with typical IV infusion solutions, such as sodium chloride (0.9% NaCl), 5% Glucose, or Ringer-Lactate, which are all

aqueous• Hexamoll® DINCH is more lipophilic than DEHP⇒ migration is lower as compared to DEHP⇒ reduced exposure• Risk = Hazard x Exposure⇒ reduced hazard: Hexamoll® DINCH is not a hazardous substance⇒ reduced risk, increased benefit

Hexamoll® DINCHSuitable for Infusion Solutions

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Sorption behaviors of Hexamoll® DINCH equivalent to other plasticizers

Hexamoll® DINCHSuitable for blood contact applications

Zhong et al. (2013) ”The migration in the DINCH system was considerably lower than for DEHP, which indicates that DINCH could be a promising alternative plasticizer of DEHP.“

Prowse et al. (2014) confirms that the commercially available blood bags (Macopharma) plasticized with Hexamoll® DINCH meet the stabilization requirements

Bicalho et al. (2015): DEHP and Hexamoll® DINCH bags offer better stabilization capacity on RBC than BTHC bags

Lagerberg et al. (2015) studied the in vitro quality of plasma and RBC collected and stored in a Hexamoll® DINCH collection system developed by Fresenius HemoCare Netherlands BV• Collection systems were stored at 2-6°C for 42 days• During storage in 2nd generation additive solutions (PAGGS-M, AS-3 or PAGGG-M)

hemolysis, potassium leakage and ATP decline were comparable for both, Hexamoll®DINCH and DEHP, bag systems

• Leakage of DINCH blood product during storage was much less pronounced than that of DEHP

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Migration in blood collection systems

(Zhong et al. 2013)DEHP Hexamoll®

DINCH

Concentration of plasticizer inblood (mg/ml) 58 0.67

Migration of plasticizer per unit area (mg/cm2) 56 0.65

Migration of plasticizer of one set of circulation tubing (mg) 250 2.90

Hexamoll® DINCH -based blood bags offer lower migration rates and comparable stabilization capabilities to DEHP

Hexamoll® DINCHSuitable for blood contact applications

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Pediatric platelet bag based on Hexamoll® DINCHproduced by Fresenius has been in use for four years at the Dutch National Blood bank Sanquin.

Achievement:Medical devices without DEHP in blood product applications.

Hexamoll® DINCH - the non-aromatic and non-phthalate plasticizer for whole blood collection systems, platelet pooling sets and pediatric platelet storage bags.

Awarded application: Hexamoll® DINCH -based platelet bags for pediatric use

Hexamoll® DINCHSuitable for blood contact applications

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Fresenius KabiPediatric systems for

RBC/ PLT preparation & storage

MacopharmaBlood bags Toyobo

Blood circuit tubes

Kidney-Dialysis set

Extracorporeal circulation: Heart-lung machine

Hexamoll® DINCHSuitable for enteral feeding

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1) Reg (EU) No. 10/2011 2) Impurity in TEHTM 3) 24h Migration, 1,5kg body weight 4) 50% of TDI from food (EFSA)

Hexamoll® DINCH is the only plasticizer that complies with the TDI threshold.

Nutritional setplasticized with

Plasticizer measured

Total migration [μg]

Dose 3)

[mg/kg bw./day]TDI (EFSA) [mg/kg

bw./day)4) Status

DEHP 1) DEHP 1400 0,93 0,025 37,3

TEHTMTEHTM <5 n.a. n.a.

1,9DEHP 2) 70 0,05 0,025

Hexamoll® DINCH Hexamoll®DINCH 180 0,12 1 0,1

ATBC ATBC 25,000 16,67 1 16,7

Nutrison Nenatal (fat content 4.4%) under realistic application conditions: 24 h @ room temperature, flow rate 5 ml h-1 (Welle et al., 2005)

Note: TEHTM is not approved under EU Regulation 10/2011 for food contact applications, thus not suitable for medical feeding therapies

Enteral nutrition sets by Nutricia

Hexamoll® DINCHSuitable for enteral feeding

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Hexamoll® DINCHSuitable for respiratory masks

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Medical dollsSchossler et al. (2011)

Hexamoll® DINCH, emission chamber setup:Steady state concentration <0.5 µg/m3

at 23°C is reached after approx. 600h

Safety assessment:Concentration x inhaled volume = uptake0.5 µg/m3 x 20 m3 = 10 µgDose: 10 µg/ 60 kg = 0.17 µg/ kg bw/ dayMargin of Exposure: 5882

Respiratory mask

5 Hexamoll® DINCH : Technical Aspects

Hexamoll® DINCHTechnical Aspects

35

OO

O

O

C9H19

C9H19

OO

C9H19

O

O C9H19

cis (90%)

Hexamoll® DINCH

trans (10%)

The structural change in the ring makes the difference

O

R

O

O

O

R

Phthalates

Planar

Aromatic

3D - chair

Non-aromaticTP - Extrusion

Extraction

Stability

Cold Flexibility

Sterilizability

Weldability

TP – Dry Blend Production

Hexamoll® DINCHPlasticizer Extraction

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Plasticizer Extraction by various liquids, weight loss in % DEHTP Hexamoll®

DINCH DEHP

Water, 70°C, 28 days -0.55 -0.02 -0.02

Soapy water, 70°C, 28 days -1.96 -1.11 -6.15

Hexamoll® DINCH shows lower extractability than DEHP, and even much lower extractability than DEHTP

Hexamoll® DINCHStability

Configuration analyzed by 1H-NMR, 90 ±10 % cis- and 10 ±10 % trans-isomer,ratio stable over time (>10 years) as shown in chemical characterization

Stable for several years, proven in chemical characterization

Stable at temperatures higher than processing temperature

Toxicological testing undertaken with representative batches of Hexamoll® DINCH

Stability in food, solutions for gavage or i.v. applications proven by chemical characterizationStability data part of the respective study reports

Stability during processing conditions and during sterilization processes publishedby independent researchers in peer reviewed journals

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Hexamoll® DINCHCold Flexibility

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Hexamoll® DINCH shows the best cold flexibility of all three tested systems

-45

-40

-35

-30

-2545 50 55 60 65 70 75

tem

pera

ture

[oC

]

plasticizer content [phr]

Brittleness Temperature as function of plasticizer content(only completely broken specimens were counted)

DEHPHexamoll® DINCH®DEHTPHexamoll® DINCH

Hexamoll® DINCHSterilizability

39Source: Saint-Gobain

No significant change in tensile elongation for all four formulations

Effect of Sterilization on tensile elongation [%]

0

50

100

150

200

250

300

350

400

450

500

Non-Sterilized ETO Gamma 2.5Mrad

Gamma 5.0Mrad

Steam-121oC Steam-135oC

Hexamoll® DINCH®DEHPTEHTMDEHA

Hexamoll® DINCH

Hexamoll® DINCHSterilizability

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Source: Saint-Gobain

Effect of Sterilization on 100 % Tensile Modulus [MPa]

ETO Sterilization not effecting Modulus significantlyγ− and Steam-sterilization effecting TEHTM, but not effecting other formulations

0

1

2

3

4

5

6

Non-Sterilized ETO Gamma 2.5Mrad

Gamma 5.0Mrad

Steam-121oCSteam-135oC

Hexamoll® DINCH®DEHPTEHTMDEHA

Hexamoll® DINCH

Hexamoll® DINCHSterilizability

41

Source: Saint-Gobain

ETO not changing yellowness for all four formulationsIn γ-sterilization, all formulations turn yellow; The higher the γ-dosage, the higher the yellowness; DEHP showed the highest yellowness, DEHA the

lowestIn Steam sterilization, higher temperatures resulting in higher yellowness

-5

0

5

10

15

20

25

30

35

40

Non-Sterilized ETO Gamma 2.5Mrad

Gamma 5.0Mrad

Steam-121oC Steam-135oC

Influence of Sterilization on Yellowness

Hexamoll® DINCH®DEHPTEHTMDEHA

Hexamoll® DINCH

Hexamoll® DINCHSterilizability

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Source: N. Burgos, A. Jiménez in Polym. Degrad. Stab. 94 (2009) 1473–1478

Surface morphology of PVC/DINP samples: (A) unsterilized; (B) (B) 3 cycles Ethylene Oxide(C) (C) 3 cycles Water Vapor

Surface morphology of PVC/ATBC samples: (A) unsterilized; (B) 3 cycles Ethylene Oxide(C) 3 cycles Water Vapor

Surface morphology of PVC/Hexamoll®DINCH samples: (A) unsterilized(B) 3 cycles Ethylene Oxide(C) 3 cycles Water Vapor

Hexamoll® DINCHSterilizability

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Source: N. Burgos, A. Jiménez in Polym. Degrad. Stab. 94 (2009) 1473–1478

Formulations #1 #2 #3Lacovyl® PB1172 H 100 100 100Palatinol® N (DINP) 70Glyplast® A7C (ATBC) 70Hexamoll® DINCH 70Irganox® 1076 1.7 1.7 1.7

Hexamoll® DINCH additivated sample showed almost no alterations after Ethylen Oxide resp. Water Vapor sterilization

Hexamoll® DINCHWeldability

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Based on the tests, the weldability of all investigated film combinations (A-A, B1-B1, B2-B2 and B3-B3) could be classified as “very good”.

HF-welding trials were made in November 2011 with blood-bag films (DEHP (A) and Hexamoll® DINCH (B1, 2, 3))

Machine type:High frequency machine G 750 SC, Kiefel GmbH Working frequency: 27.12 MHz Power: 800 watts Electrodes dimensions: 200 x 6 mm

Results:

P-PVC performance Three steps in thermoplastic processing

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Dry blend production(mixing)

Compounding(extrusion)

Final forming(molding, extrusion, calandering)

(mouled articles, calandered film and sheets,

Extruded profiles

Target recipe - Status 19.05.

100 phr PVC Vynova S7102

2 phr Reagens SLX/781 as stabilizer

100 and 108 phr Plasticizer: Two high dosages of Hexamoll® DINCH

Optional: in comparison to the analogue recipes with Palatinol® N (DINP) as comparison

Optional: Filler (CaCO3) to be defined

Hexamoll® DINCHThermoplastic processing

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47

Solid blend / Dry Blend

Mixing

higher mixing / processing temperaturecompared to DINP …

Mixing in a fast moving mixer (heating-cooling) 2000-2500Upm Heating Mixer

Dry-Blend in Heating MixerCooling Mixer

Hexamoll® DINCHDry Blend Production

48

Stirrer started at slow rotation speed & preheat PVC up to 50-60°C (opens pores)

Addition of Hexamoll® DINCH (preheated, preferable in several portions …ideally sprayed) and other liquid ingredients so that the temperature does not drop

• 1/3 at the beginning of mixing process

• 1/3 at half of the total mixing time

• 1/3 at ¾ of the total mixing time

Stabilizer preferably added at the end / after Hexamoll® DINCH

Increase mixing speed until dry blend is achieved (at ~90°C)

Add other plasticizer e.g. ESBO (co-stabilizer)

Mixing at high speed until desired temperature is reached (125°C–145°C) assuming there is no problem with the maximum torque being reached

Cooling and storage of dry blend

Hexamoll® DINCHDry Blend Production - optimized approach

49

Stirrer started to preheat PVC (together with solid stabilizer) up to 70°C at 2500 rpm (opens pores)

Addition of 70 phr Hexamoll® DINCH including other liquid ingredients (stabi, ESBO) within 6-7 minutes at 2000 rpm (preferable preheated) and other liquid ingredients so that the temperature does not drop. T at the end of plasticizer dosage at around 90°C.

Addition of second portion (30-40 phr) Hexamoll® DINCH at 100°C at 1600-1800 (in dependence of final plasticizer content) rpm during 3-4 min until 110°C.

Mixing at 1600-1800 until 120°C is reached. (higher T possible..127°C… To be determined in dependence of the mixing geometry)

Add filler, stir to get homogeneous mixture (do not exceed 120°C again)

Cooling and storage of dry blend

* Specific for LU AWETA 10L Henschel Mixer

Hexamoll® DINCHDry Blend Production - optimized approach 01/2016

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Stirrer started to preheat PVC (together with solid stabilizer) up to 70°C at 550-660 U/m (opens pores)

Addition of 100-108 phr Hexamoll® DINCH including other liquid ingredients (stabi, ESBO) within 3-4 minutes at 550-660 U/m (preferable preheated) and other liquid ingredients so that the temperature does not drop. T window 70-85°C (at the end of plasticizer dosage at around 85-90°C.)

Mixing at 550-660 U/m until 120°C is reached.

Add filler, stir to get homogeneous mixture (do not exceed 120°C again)

Cooling at 70-90 l/min (3,5-4,6 m/s) (10-13 min) and storage of dry blend

Hexamoll® DINCHDry Blend Production – optimized approach 03/2016

51

Adding time and speed is crucial

Adding plasticizer is happening too fast:

Mixture gets wet and is not free flowing. Residue will form in the heating mixer and cake. Residue can chip off and cause the mixture to be inhomogeneous and makes the heat transfer difficult.

Redripping of plasticizer:

Vibration of the mixer can cause drops from the plasticizer supply to drip into mixture at end of the process. Moist agglomerates can be formed which cause defects in the material during further processing.

Dry BlendMistakes when processing P-PVC

Hexamoll® DINCHThermoplastic Processing - Extrusion

52

Plasticized PVC with Hexamoll® DINCH shows lower melt viscosity than that with DEHTP, resulting in higher throughput and/or lower energy consumption during processing

0

10

20

30

40

50

60

165 175

MVR

[cm

3 /10m

in]

Temperatur [°C]

MVR - Measurements with granules made with DEHTP or Hexamoll® DINCH

Hexamoll® DINCH®DEHTPHexamoll® DINCH

Hexamoll® DINCHThermoplastic Processing - Extrusion

53

Comparison of Mixing and extrusion of DEHP and Hexamoll® DINCH

PVC with 60 phr DEHP67 phr Hexamoll® DINCH(mixing up to 120°C in high speed mixer)

Dry-blend preparation: Henschel-Type mixer

Extrusion: Krauss Maffei Z 25, co-rotation twin-screw extruder

140 min-1 extruder speed25 kg/h throughput (dosage) 145 – 170°C temperature setting

Torque: -25 %Pressure: -12 %Temperature: -7oCMechanical power: -25 %

Disclaimer

54

WHILE THE DESCRIPTIONS, DESIGNS, DATA AND INFORMATION CONTAINED HEREIN ARE PRESENTED GRATIS, IN GOOD FAITH AND BELIEVED TO BE ACCURATE, THEY ARE PROVIDED FOR GUIDANCE ONLY AND BASF ASSUMES NO OBLIGATION OR LIABILITY FOR ANY RESULTS OBTAINED, ALL SUCH BEING GIVEN AND ACCEPTED AT THE READER’S RISK. BECAUSE MANY FACTORS MAY AFFECT PROCESSING OR APPLICATION/USE OF OUR PRODUCTS, THE READER IS NOT RELIEVED FROM CARRYING OUT ITS OWN INVESTIGATIONS AND MAKING TESTS TO DETERMINE THE SUITABILITY OF A PRODUCT FOR A PARTICULAR PURPOSE PRIOR TO USE. USERS MUST EVALUATE WHAT CLAIMS AND INFORMATION ARE APPROPRIATE AND COMPLY WITH A JURISDICTION’S REGULATORY REQUIREMENTS. NEITHER WARRANTIES OF ANY KIND, EITHER EXPRESSED OR IMPLIED, INCLUDING, BUT NOT LIMITED TO, WARRANTIES OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE, NOR ANY GUARANTEES ARE MADE/GRANTED REGARDING PRODUCTS DESCRIBED, OR THEIR PROPERTIES, DESIGNS, DATA OR INFORMATION SET FORTH, OR THAT THE PRODUCTS, DESCRIPTIONS, DESIGNS, DATA OR INFORMATION MAY BE USED WITHOUT INFRINGING THE INTELLECTUAL PROPERTY RIGHTS OF OTHERS. THEREFORE, THE READER SHALL IN EACH CASE HAVE THE RESPONSIBILITY TO EXAMINE WHETHER ITS USE OF THE BASF PRODUCT(S) OR OF THE BASF INFORMATION FOR THE PRODUCTION, OFFER OR SALE OF ANY FORMULATION OR ARTICLE CONTAINING A BASF PRODUCT MIGHT INFRINGE A THIRD PARTY’S INTELLECTUAL PROPERTY RIGHT. IN NO CASE SHALL THE DESCRIPTIONS, DESIGNS, DATA OR INFORMATION PROVIDED BE CONSIDERED A PART OF ANY SUPPLY AGREEMENT UNLESS THE PARTIES EXPRESSLY AGREE OTHERWISE. (January 2017)

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