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© SPEX CertiPrep, Inc. 2011
1
Patricia AtkinsSPEX CertiPrep
Phthalates & BPA in Consumer Products
© 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!
© SPEX CertiPrep, Inc. 2011
In the News
© 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
© 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
© 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
© 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)
© 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
© 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)
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© 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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
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
© SPEX CertiPrep, Inc. 2011
References
All references available by request
– Call 1-800-LAB-SPEX
– Or email crmsales@spexcsp.com
For more information, see our white paper
‘The Analysis of Laboratory and Consumer Water Sources for the Presence of BPA and Phthalates’
© SPEX CertiPrep, Inc. 2011
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