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© SPEX CertiPrep, Inc. 2011 1 Patricia Atkins SPEX CertiPrep Phthalates & BPA in Consumer Products
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Page 1: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

1

Patricia AtkinsSPEX CertiPrep

Phthalates & BPA in Consumer Products

Page 2: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Housekeeping

Everyone in attendance will receive a copy of the slides

The webinar is being recorded and will be available for everyone to view on demand

– The recording will be posted about one week after the event

Questions will be answered at the end of the presentation

– Type any questions you may have into the question box and we will answer them during the Q & A portion

Stay tuned after the Q&A session – we’re giving away a free gift!

Page 3: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

In the News

Page 4: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Background• Group of esters of 1,2-

benzenedicarboxylic acid• Produced since late 1800’s• Commercial use in 1920’s

Background• Group of esters of 1,2-

benzenedicarboxylic acid• Produced since late 1800’s• Commercial use in 1920’s

Uses• Plastic compounds

(10-60% by wt)• Binders• Coatings• Fragrances and pigments

Uses• Plastic compounds

(10-60% by wt)• Binders• Coatings• Fragrances and pigments

Health Effects• Residue is widespread• Asthma, reproductive

disorders, diabetes, obesity and genetic effects

• Endocrine disruptor

Health Effects• Residue is widespread• Asthma, reproductive

disorders, diabetes, obesity and genetic effects

• Endocrine disruptor

Response• US ban of DEHP, BBP,

DBP in children’s toys 2009• Mexico, the EU, and Japan

restricted or banned the use of phthalates in children’s toys

Response• US ban of DEHP, BBP,

DBP in children’s toys 2009• Mexico, the EU, and Japan

restricted or banned the use of phthalates in children’s toys

Phthalates

Page 5: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Phthalates in Consumer Products

Water BottlesBottled WaterMedical tubing and devicesCosmeticsPerfumesHealth and Beauty ProductsToysFood PackagingBaby Mattress CoversPlastic FilmsSunscreensBaby Care Ointments & LotionsAir FreshenersVinyl flooring

Page 6: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Common PhthalatesName Acronym Structural formula CAS No.

Dimethyl phthalate DMP C6H4(COOCH3)2 131-11-3Diethyl phthalate DEP C6H4(COOC2H5)2 84-66-2Diallyl phthalate DAP C6H4(COOCH2CH=CH2)2 131-17-9

Di-n-propyl phthalate DPP C6H4[COO(CH2)2CH3]2 131-16-8Di-n-butyl phthalate DBP C6H4[COO(CH2)3CH3]2 84-74-2

Diisobutyl phthalate DIBP C6H4[COOCH2CH(CH3)2]2 84-69-5Butyl cyclohexyl phthalate BCP CH3(CH2)3OOCC6H4COOC6H11 84-64-0

Di-n-pentyl phthalate DNPP C6H4[COO(CH2)4CH3]2 131-18-0Dicyclohexyl phthalate DCP C6H4[COOC6H11]2 84-61-7

Butyl benzyl phthalate BBP CH3(CH2)3OOCC6H4COOCH2C6H5 85-68-7Di-n-hexyl phthalate DNHP C6H4[COO(CH2)5CH3]2 84-75-3Butyl decyl phthalate BDP CH3(CH2)3OOCC6H4COO(CH2)9CH3 89-19-0

Di(2-ethylhexyl) phthalate DEHP C6H4[COOCH2CH(C2H5)(CH2)3CH3]2 117-81-7

Di(n-octyl) phthalate DNOP C6H4[COO(CH2)7CH3]2 117-84-0

Diisodecyl phthalate DIDP C6H4[COO(CH2)7CH(CH3)2]2 26761-40-0

n-Octyl n-decyl phthalate ODP CH3(CH2)7OOCC6H4COO(CH2)9CH3 119-07-3

Diisononyl phthalate DINP C6H4[COO(CH2)6CH(CH3)2]2 28553-12-0

Page 7: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Regulations & Banned Phthalates

DEHP DBP BBP DINP DIDP DNOP

US CPSIA CPSC-CH-C1001-09.03

0.1% individual (All toys & Childcare)

0.1% individual (All toys & Childcare)

0.1% individual (All toys & Childcare)

0.1% individual (Toys &

Childcare w/ Oral Contact)

0.1% individual (Toys &

Childcare w/ Oral Contact)

0.1% individual (Toys &

Childcare w/ Oral Contact)

EU EC Directive 2005/84/EC0.1%

combined (All toys)

0.1% combined (All toys)

0.1% combined (All toys)

0.1% combined (Toys with

Oral Contact)

0.1% combined (Toys with

Oral Contact)

0.1% combined (Toys with

Oral Contact)

Japan ST Standard Part 3 / Food Sanitation Law

0.1% combined (All toys)

0.1% combined (All toys)

0.1% combined (All toys)

0.1% combined (Toys with

Oral Contact)

0.1% combined

(Toys with Oral Contact)

0.1% combined (Toys with

Oral Contact)

Page 8: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Bisphenol A

Background• 2 phenol groups• Produced by condensing

acetone + phenol & acid catalyst

• 3.7 million metric tons/yr• Reported in 1891

Background• 2 phenol groups• Produced by condensing

acetone + phenol & acid catalyst

• 3.7 million metric tons/yr• Reported in 1891

Uses• Polymers• Toys• Medical devices• Coatings and epoxy resins

Uses• Polymers• Toys• Medical devices• Coatings and epoxy resins

Health Effects• Suggested estrogenic

effects the 1930’s• Endocrine disruptor

Health Effects• Suggested estrogenic

effects the 1930’s• Endocrine disruptor

Regulations• The EPA guideline - 50

µg/kg/day• As low as 0.025 µg/kg/day

can have adverse effects

Regulations• The EPA guideline - 50

µg/kg/day• As low as 0.025 µg/kg/day

can have adverse effects

Page 9: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Consumer Products BPA

Water Bottles

Baby Bottles

Dental Filling Material

Toys

Cash Register Receipts

Food can lining (soda, tomatoes, acidic food)

Jar lid linings

Recycled Pizza box lining

Toilet Paper

Plastic water piping

Beer & Wine (fermented in BPA lined vats)

Page 10: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

International Regulations

Area Scope of BPA Ban Requirement Effective Date

EU

Food Packaging migration limit no more than 0.6 mg/kg Limit

TDI 0.05 ppm/per day / per individual Limit

PC baby bottles Banned Mar-11

CanadaPC baby bottles Banned Mar-10

BPA deemed toxic Action Sep-10

Denmark PC baby bottles Temporary Ban Mar-10

Page 11: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

US RegulationsArea Scope of BPA Ban Requirement Effective Date

ConnecticutReusable Food & Beverage Containers, not disposable Banned Oct-11

Prefilled containers containing infant formula or baby food Banned Oct-11

Illinois (Chicago) Empty Beverage Containers (<3 years old) Banned Jan-10

Maryland Empty Food & Beverage Containers (<4 years old) Banned Jan-12

MaineReusable Food & Beverage Containers Banned Jan-11

Manufacturers of baby food products, toy articles, tableware Submit information Jul-11

Minnesota Empty Food & Beverage Containers (<3 years old) Banned 1/1/2010 (Manufacture)2012 (Sale)

New York Empty Beverage Containers, Pacifiers, Childcare Products (<3 years old) Banned Dec-10

New York (Albany Co) Empty Beverage Containers (<3 years old) Banned Feb-10

New York (Schnectady Co) Empty Beverage Containers (<3 years old) Banned 2009

New York (Suffolk Co) Empty Beverage Containers (<3 years old) Banned 2009

New York (Rockland Co) Empty Beverage Containers & Pacifiers (<3 years old) Banned Sep-10

Vermont

Manufacture of formula or baby food in Reusable containers, not disposable Banned Jul-12

Prefilled plastic containers containing infant formula or baby food Banned Jul-12

Prefilled metal cans containing infant formula or baby food Banned Jul-14

WashingtonEmpty Food & Beverage Containers (<3 years old) Banned Jul-11

Sports Water Bottles (<64 oz) Banned Jul-12

Wisconsin Food & Beverage Containers (<3 years old) Banned Jun-10

Page 12: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Testing Methods: Phthalates

CPSC: CPSC-CH-C1001-09.03 Standard Operating Procedure for Determination of Phthalates (Children’s Toys & Childcare Articles) Measurement of 6 Restricted Phthalates

3 Components to Method: Sample Preparation, Extraction & Analysis

Sample Preparation

Toy cut in pieces < 2mm Grind to Powder – SPEX

SamplePrep Freezer Mill Prepare Standards & QC− SPEX CertiPrep Phthalate

Standard 8060-QC− SPEX CertiPrep CRM-PE001

Phthalates in PE QC Standard

Extraction

Many acceptable methods including:− Soxhlet (EPA 3540C, EPA 3541)− Pressurized Fluid Extraction (EPA

3545A)− Ultrasonic Extraction (EPA 3550C)− Microwave (EPA 3546) SPEX CertiPrep Microwave Method

for CRM-PE001 Phthalates in PE Analysis− 1 gm Sample in 25 mL

Acetone:Cyclohexane (70:30)− Temp: 110-140°C− 10 minutes

Page 13: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Testing Methods: Phthalates

CPSC: CPSC-CH-C1001-09.03 Standard Operating Procedure for Determination of Phthalates (Children’s Toys & Childcare Articles)

Analysis

• GC/MS

Page 14: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Testing Methods: Phthalates

EPA Method 606: Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater – Phthalate Ester

Measurement of DEHP, BBP, DBP, DEP, DMP, DNOP

Liquid – Liquid Extraction & Concentration

Analysis by GC/MS

Page 15: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Testing Methods: BPA

ASTM D7065 - 06 Standard Test Method for Determination of Nonylphenol, Bisphenol A, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry

− Solid Phase Extraction

− GC-MS

ASTM D7574 - 09 Standard Test Method for Determination of Bisphenol A in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

− Solid Phase Extraction

− LC/MS

Page 16: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Studies Involving PhthalatesPresence of phthalates in contact lens and cleaning solutions

C. Pérez-Feás, M.C. Barciela-Alonso and P. Bermejo-BarreraMicrochemical Journal

Confirm presence of DMP, DEP, BBP and DBP in contact lens cleaning solutions

DBP and BBP migrated from contact lenses

Determination of phthalates in fruit jellies by dispersive SPE coupled with HPLC-MS

Yuwei Ma, Yuki Hashi, Feng Ji, Jin-Ming LinJournal of Separation Science

DMP, DEP, DPP, BBP, DCHP in fruit jellies BBP and DEP were found in real samples

Page 17: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Studies Involving BPATransfer of bisphenol A from thermal printer paper to the skin

Sandra Biedermann, Patrik Tschudin and Koni GrobFrom the issue entitled "Analytical Chemistry for Drug Discovery and Development / Special review issue (pp. 27-264)“

Thermal paper contained 8–17 g/kg bisphenol A (BPA) Handling for 5 s = 1 μg BPA (0.2–6 μg) 10x more for wet or greasy hands BPA extractable after 2 h on skin Not known if BPA passes through the skin

− (If depth is sufficient, can’t be washed off)

Occurrence of Bisphenol A in Indoor Dust from Two Locations in the Eastern United States and Implications for Human Exposures

Sudan N. Loganathan and Kurunthachalam KannanArchives of Environmental Contamination and Toxicology

BPA was found in 95% of the dust from <0.5 to 10,200 ng/g Median BPA intake (ingestion of dust) 0.35 and 5.63 ng/kg body

weight/day

Page 18: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

SPEX CertiPrep Studies

Laboratory Water

Bottled Water

−Heated & Room Temperature

Consumer Water Sources

Sports Bottles and Reusable Beverage Containers

−Heated & Room Temperature

−Unrinsed & Washed Upcoming – BPA & Phthalates in Small

Toys

Page 19: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Water Quality

US municipal water quality- EPA

− Many guidelines for compounds including phthalates & BPA

Bottle water quality- FDA

− No guidelines currently for phthalates or BPA

Around the world many believe bottled water is a safer alternative to municipal water sources

Page 20: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Bottled Water Industry

$168 billion a year in sales worldwide by 2012

The US consumes 8.8 billion gallons a year

Second largest consumed beverage in the country

Americans drink bottled water:

− Substitute for other beverages

− Concerned over tap water safety

Many sources including tap water

Page 21: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Sources of Contamination

Many potential sources of organic pollutants in water supplies

– Environmental– Manufacturing or Processing– Packaging and/or Transport– Distribution

Does processing of water increase BPA & Phthalates?

Groups raise concern of leaching of chemicals from packaging

– Suggestions include: don’t reuse, no high temperatures, avoid bottled water

Page 22: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Consumer Water Sources & Reusable Bottles

Determine if laboratory and consumer water sources contained phthalates or Bisphenol A

Re-usable beverage/water containers

− BPA-free Sports Bottle

− Traditional Sports Bottle

− Plastic ‘Jug’ Container

− FEP Bottle

− Squeeze-type bottle

Consumer water sources:

− Commercial Bottled Water

− Municipal Tap Water

− Filtered Municipal Water using Point-of-Use (POU) systems

Page 23: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Bottled HPLC grade Water

Bottled HPLC-MS grade Water

DI Water from a HDPE carboy

DI Water from a DDI Water source tap

Laboratory Water Sources

Page 24: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Method & Materials: Reagent Contamination

Widespread laboratory phthalate exposure– Containers, Vessels– Gloves– Dust

Reagent packaging– Even glass containers: plastic caps,

seals or septa– Manufacturing contamination

Difficult to eliminate phthalate contamination from samples All materials must be tested before use Rinse, bake or clean materials when possible

before use

Page 25: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials:Reagent Contamination

Three compounds used:

NaOH, NaCl and Na2SO4

Rinsed with 60 mL aliquots of methylene chloride

Evaporated to 1mL and run by GCMS

Solids then baked at 210°C for 10-30 min

Two more aliquots rinsed and reduced to 1 mL for analysis

Materials pre & post cleaning examined for contamination

Page 26: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials:Reagent Contamination

Reduction of phthalates found from the pre and post cleaned solids

The NaOH did not contain phthalates

0

200

400

600

800

1000

1200

1400

1600

1-Na2SO4

2-Na2SO4

3-Na2SO4

4-Na2SO4

1- NaCl 2- NaCl 3- NaCl 4- NaCl

ppb

Rinses

Page 27: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials: Standards

Phthalate & BPA Standards from SPEX CertiPrep:

S-509 Bisphenol A Standard

8061-X Phthalate Mix

8060-QC Phthalate Mix

CLPS-1 Internal Standards

Page 28: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials: Water Sample Collection

Laboratory & Municipal Water– 500 mL water– DI water system and Point-of-

Use (POU) • Taken from a stationary

system (static for >12 hours)

• Flushed system (> 2 L of water flushed )

– POU-A: dispensing system; no filter or sanitization

– POU-B: UV sanitization & carbon fiber filter

Page 29: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials:Reusable Bottle Testing

500 mL LCMS water Rinsed with LCMS water and retained Cleaned in a dishwasher using hot water

and dish detergent Rinsed several times with DI water and

finally twice with LCMS water 500 mL LCMS water decanted into bottles One set at 60°C for one week Second set room temperature for one week

Page 30: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials: Bottled Water

Two sets of each brandTwo sets of each brand

One set placed at 60°C for one weekOne set placed at 60°C for one week

Second set placed at room temperature for one weekSecond set placed at room temperature for one week

Page 31: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials: Extraction

Liquid – Liquid extraction

15 gm NaCl

Acid extraction: 3-10 drops HCl (pH <3)

Base extraction: 1–5 mL 50% NaOH (pH >9)

30 mL aliquots DCM added to 60 mL

Dried with ‘cleaned’ Na2SO4

Extracts combined & evaporated to 1 mL

Page 32: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Methods & Materials: Instrument Conditions

GC-MS in scan mode

scan range 35-450 m/z

Injection volume 1 µL

CV-5 capillary column (3.0 m x 0.25 mm x 0.25 µm)

Chromatogram of SPEX CertiPrep Phthalate Standard 8061-X & Internal Standard Mix CLPS-I90

Page 33: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Results: Target Compounds

Name Abbreviation RT Ions Structural formula CAS #

Dimethyl phthalate DMP 7.57 163, 77, 164, 76 C10H10O4 131-11-3

Diethyl phthalate DEP 8.43 149, 177, 150, 65, 29 C12H14O4 84-66-2

Diisobutyl phthalate DIBP 10.28 149, 57, 29, 41, 223 C16H22O4 84-69-5

Di-n-butyl phthalate DBP 10.8 149, 150, 29, 41, 57 C16H22O4 84-74-2Di(2-methoxyethyl) phthalate DMEP 10.98 59, 58, 45 C14H18O6 117-82-8

Diisohexyl phthalate DIHxP 11.33 149, 43, 85, 150 C20H30O4 146-50-9

Di-n-pentyl phthalate DNPP 11.66 149, 43, 150, 41, 29 C18H26O4 131-18-0

Bisphenol A BPA 11.83 213, 228, 119, 214, 91 C15H16O2 80-05-7 Di-n-hexyl phthalate DNHP 12.36 149, 43, 41, 29, 150 C20H30O4 84-75-3

Butyl benzyl phthalate BBP 12.42 149, 91, 206, 65, 104 C19H20O4 85-68-7Hexyl 2-ethylhexyl phthalate H2EHP* 12.66 149, 43, 251 C22H34O4 75673-16-4

Di(2-n-butoxyethyl) phthalate DBEP 12.75 149, 57, 56, 101, 85 C20H30O6 117-83-9

Di(2-ethylhexyl) phthalate DEHP 12.95 149, 167, 279, 71 C24H38O4 117-81-7Dicyclohexyl phthalate DCP 12.96 149, 167, 55, 150, 249 C20H26O4 84-61-7

Di(n-octyl) phthalate DNOP 13.53 149, 279, 43, 57 C24H38O4 117-84-0Dinonyl phthalate DINP 14.22 149, 293, 71, 57, 43 C26H42O4 84-76-4

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© SPEX CertiPrep, Inc. 2011

34

Results: Laboratory Water Samples

HPLC LCMSDI Source Flushed

DI Source Stationary DI Bottle

Municipal Tap

DEP 6.28 0.18 0.00 0.30 0.50 0.00DIBP 3.52 0.16 0.88 1.36 0.52 0.00DBP 16.72 0.00 0.00 0.00 0.54 0.00BPA 3.16 0.00 0.00 0.00 0.00 0.00BBP 44.74 0.20 2.32 0.63 0.47 1.29DCP 1.00 0.00 0.00 0.00 0.00 0.00DEHP 15.60 0.63 5.92 26.41 2.44 1.94

Total c (ppb) 91.02 1.17 9.12 28.70 4.47 3.23Total # compounds 7 4 3 4 5 2

0.0010.0020.0030.0040.0050.0060.0070.0080.0090.00

100.00

HPLC LCMS DI SourceFlushed

DI SourceStationary

DI Bottle MunicipalTap

Tota

l c (p

pb)

Total Concentration (ppb)

0

1

2

3

4

5

6

7

8

HPLC LCMS DI SourceFlushed

DI SourceStationary

DI Bottle MunicipalTap

# co

mpo

unds

Total # compounds

Page 35: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Results: Room Temperature Samples

0.00

5.00

10.00

15.00

20.00

25.00

30.00

35.00

40.00

45.00

Brand A RoomTemperature

Brand B RoomTemperature

Brand C RoomTemperature

Municipal Tap Brand A POUFlushed

Brand A POUStationary

Brand B POUFlushed

Brand B POUStationary

Tota

l con

cent

ratio

n (p

pb)

Total Target Compound Concentration (ppb) for Consumer Water Samples at Room Temperature

Page 36: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Results: Exposure to Heat

Heated samples no significant increase (< 2ppb increase)

Number of phthalates increased (largest from 2 to 5) between heated and RT samples

0

1

2

3

4

5

6

7

Brand A Brand B Brand C

# co

mpo

unds

Room TemperatureHeated

0.00

2.00

4.00

6.00

8.00

10.00

12.00

Brand A Brand B Brand C

Tota

l con

c. (p

pb)

Room TemperatureHeated

Page 37: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Results: Bottled Water Comparison

The largest differences between heated and room temperature samples:

− Number of different phthalates slightly increased

− BBP increased after heat in all brands

− DEHP decreased after heating in 2 of 3 brands

Earlier studies found DEHP in water decreased in samples above 20°C –possible breakdown of DEHP

Page 38: Phthalates & BPA in Consumer Products - SPEX CertiPrep · Phthalates & BPA in Consumer Products ... Cosmetics Perfumes Health and Beauty Products ... Manufacture of formula or baby

© SPEX CertiPrep, Inc. 2011

Results: Bottled Water Comparison

0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

Brand A RoomTemperature

Brand A Heated Brand B RoomTemperature

Brand B Heated Brand C RoomTemperature

Brand C Heated

Con

cent

ratio

n (p

pb)

Compounds Found in Bottled Water SamplesDEP DBP BBP DEHP DMP DIBP

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Results: Consumer Water Comparison

Lowest concentration:

– Municipal tap source

– POU after flushing

Highest concentration POU-B (static system)

– Caused by new filter contaminant?

All sources < 10 ppb total concentration except for POU-B static

Bottled water slightly higher concentration than municipal tap

None of the bottled water samples or the municipal tap water sample contained BPA.

The POU-B - small conc. of BPA (static & flushed): 0.04 to 0.09 ppb

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Results: Sports Bottles

Sports Bottle BPA Free Sports Bottle

Unrinsed RT Rinsed RT Rinsed Heated

Unrinsed RT Rinsed RT Rinsed Heated

Old Bottle Rinsed Heated

Dimethyl phthalate 10.74 0.00 0.00 0.00 0.00 0.00 0.00Diethyl phthalate 0.25 0.00 0.00 0.00 0.13 0.00 0.00

Diisobutyl phthalate 0.08 0.00 0.00 4.62 0.13 7.89 2.04Di-n-butyl phthalate 0.35 0.07 0.12 0.00 0.17 0.00 0.00

Bisphenol A 0.17 0.00 0.12 0.00 0.00 0.00 0.00Butyl benzyl phthalate 0.13 0.33 0.00 0.72 0.00 1.06 0.98

Bis(2-ethylhexyl) phthalate 0.34 0.00 0.00 4.00 0.00 4.16 3.53Total Phthalates 12.06 0.40 0.25 9.34 0.43 13.11 6.55# of Phthalates 7 2 2 3 3 3 3

BPA was found in PC Sports Bottle BPA found in Heated PC Bottle No BPA in BPA-Free Bottle Unrinsed bottles had larger amounts of

phthalates All rinsed or heated bottles <15 ppb

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Results: Sports Bottles

Squeeze Reusable Bottle Plastic Jug Type Bottle FEP Bottle

Unrinsed RTRinsed

RTRinsed Heated

Unrinsed RT

Rinsed RT

Rinsed Heated Rinsed RT

Rinsed Heated

Dimethyl phthalate 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00Diethyl phthalate 0.00 0.33 0.37 0.10 0.11 0.28 0.01 0.00

Diisobutyl phthalate 0.00 32.14 0.03 0.09 15.90 0.09 0.04 0.01Di-n-butyl phthalate 0.05 4.15 0.00 0.26 2.38 0.43 0.25 0.21

Bisphenol A 0.00 0.00 0.00 0.18 0.00 0.11 0.00 0.17Di-n-hexyl phthalate 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.09

Butyl benzyl phthalate 0.01 1.41 0.00 0.00 0.95 0.22 0.38 0.03Hexyl 2-ethylhexyl phthalate 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.08Bis(2-ethylhexyl) phthalate 0.00 3.98 0.04 0.00 1.97 0.32 0.00 0.00

Total Phthalates 0.06 42.00 0.44 0.63 21.30 1.44 0.69 0.57# of Phthalates 2 5 3 4 5 6 4 6

BPA was found in Jug type Bottle & FEP BPA found in Heated Bottles not RT No BPA in Squeeze Bottle Less phthalates came from rinse than Sports bottles More phthalates in RT bottles than in Sports bottles Major phthalates at RT from DIBP

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Conclusions: Lab Reagents & Water Phthalate contamination-

widespread in laboratory Many materials may contain

significant phthalates Rinses & baking reduce phthalate

residue Large variability of phthalate in lab

water All laboratory water sources had

contamination– 1 to 91 ppb– Lowest level: LCMS grade

water– Highest level: LC grade water

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Conclusions: Bottled Water

All bottled water < 10 ppb total target compounds

No significant differences in the levels of phthalates in the different brands of water

Heated bottled water samples vs. Room Temp:

– Insignificant increases in phthalate levels

– Slight increases in the number of different phthalates

– DEHP decreased in 2 of 3 brands

– BBP increased slightly in all brands

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Conclusions: Municipal Water Sources

Lowest concentration:

– The municipal tap water

– POU-A filtration system (flushed samples)

Highest concentration:

– POU-B system (static samples)

– Levels were significantly lower after flushed

All static samples higher concentration than flushed samples showing water should be flushed before use

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Conclusions: Sports Bottles

BPA found in PC Sports Bottle

Concentration increased slightly in PC Sports Bottle after heating

Overall concentration of phthalates highest in unwashed bottles

BPA-Free sports bottle did not contain measurable BPA

Heating of BPA-Free sports bottle appeared to increase levels of other phthalates

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Conclusions –Reusable Beverage Containers

Plastic-Jug & soft-squeeze bottle had highest levels of phthalates @ room temp

– Due to isobutyl phthalate and DEHP

– IBP & DEHP not as high in heated bottles

– Similar results to bottled water samples

FEP bottle had consistent levels of overall phthalates in heated & room temp samples

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SPEX CertiPrepCompliance Standards Stock Phthalate Single Standards (1000 µg/mL)

Custom Phthalate Standards (any concentration, matrix or mix)

S-509: BPA Single Standard (1000 µg/mL)

8060-QC: Six Restricted Phthalates (2000 µg/mL) in Isooctane

Phthalates in Polyethylene QC Standards

– CRM-PE001: Phthalates in Polyethylene Matrix

• 8 Phthalates

– 6 Restricted Phthalates 3000 µg/mL

– 2 HMW Phthalates 30,000 µg/mL

– CRM-PEBLK: Polyethylene Blank Matrix

For Metals Analysis

– EMPT-1: Kit of Extractable Metals in Plastic Toys

– EMPT-2: Kit of Extractable Metals in Plastic Toys + Internal Check Standard

– ROHS-25: RoHS/WEEE Check Standard in Polyethylene-based matrix

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References

All references available by request

– Call 1-800-LAB-SPEX

– Or email [email protected]

For more information, see our white paper

‘The Analysis of Laboratory and Consumer Water Sources for the Presence of BPA and Phthalates’

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Questions?

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2011-2012 Catalog

Visit www.spexcertiprep.comto request or download your copy today!

Organic / Inorganic Flip-style Catalog

New Products

Easy to Use Indexes

Lists of Common Testing Methods

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