Compliance Testing of Phthalates in Toys - Analytical Chemical Control of Chemical Substances and Products

8/8/2019 Compliance Testing of Phthalates in Toys - Analytical Chemical Control of Chemical Substances and Products

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National Environmental Research Institute

Ministry of the Environment.Denmark

Compliance testingof phthalates in toysAnalytical chemical control

of chemical substances and products

NERI Research Notes No. 185


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[Blank page]


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National Environmental Research InstituteMinistry of the Environment

Compliance testingof phthalates in toysAnalytical chemical control

of chemical substances and products

NERI Research Notes No. 185

2003

Suresh C. Rastogi

Gitte H. Jensen

Inge M. Worse


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Data sheet

Title: Compliance testing of phthalates in toys.Subtitle: Analytical chemical control of chemical substances and products

Author(s): Suresh C. Rastogi, Gitte H. Jensen, and Inge M. WorseDepartment(s): Department of Atmospheric Environment

Serial title and no.: Research Notes from NERI No. 185

Publisher: National Environmental Research Institute Ministry of the Environmen t

Date of publication: August 2003

Financial support: No external financial support

Please cite as: Rastog i, S.C., Jen sen , G.H . & Wor se, I.M. (2003) Com plian ce testin g of p hth alates intoys. Analytical chemical control of chemical substances and pr odu cts. NationalEnvironm ental Research Institute, Denmark . 26pp . Research N otes from NERI No.185. http:/ / research-notes.dmu.dk/

Reprod uction is permitted, prov ided th e source is explicitly acknow ledged.

Abstract: The content of ph thalates in toys and other articles for childr en up to three years ofage is regulated by the Statutory Ord er of Danish Ministry of Environ ment an dEnergy, No. 151 of 15th March 1999. In the p resent investigation, 15 prod ucts (toysand other articles for children up to 3 years of age) were analysed for the content ofph thalates on the requ est of Danish Environm ental Protection Agen cy (DEPA). Thepro du cts received from DEPA were analysed for the contents of dimethyl-, diethyl-,dibu tyl-, diisobutyl-, butylbenzy l-, dicyclohexyl-, diethy lhexyl-, d i-n-octyl-, di-n-nonyl-, di-iso-nonyl- and di-iso-decyl ph thalate. The subsamp les of the produ cts weresoxhlet extracted in dichloromethan e, followed by analysis of the extracts by gaschromatogr aph y and m ass spectrometry . The content of one or more ph thalates inseven of the investigated prod ucts/ part(s) of the produ cts was found to be higherthan th e maximum auth orised concentration , 0.05%.

Keyword s: Toys, phthalates, gas chromatography, mass spectrometry, Statu tory OrderLayout: Majbritt UlrichReferee(s): Asger B. Hansen

ISSN (electronic): 1399-9346

Number of pages: 26

In tern et-version : Th e rep ort is available on ly in electron ic form at from NERIs h om ep agehttp:/ / www .dmu.dk/ 1_viden/ 2_Publikationer/ 3_Arbrapporter/ rapporter/ AR185.pdf

For sale at: Ministry of the EnvironmentFrontlinienStrandgade 29DK-1401 Kbenhavn KTel. +45 32 66 02 [email protected]


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Contents

Summary 5

Resu m 71 Introduction 9

2 Products 11

3 Analysis 133.1 Experimental 133.2 Chromatograph ic cond it ions for phthala te analysis 14

3.2.1 GC-MS 143.2.2 GC-FID 14

4 Results and Discussion 155 References 23

National Environmental Research Institu te 25

NERI Technical Reports 26


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Summary

The content of ph thalates in toys and other articles for children u p tothree years of age is regulated by the Statutory Order of Danish

Ministry of Environment and Energy, No. 151 of 15th March 1999. Inthe present investigation, 15 products (toys and other articles forchildren up to three years of age) were analysed for the content ofphthalates on the request of Danish Environmental ProtectionAgency (DEPA). The products received from DEPA were analysedfor the contents of dimethyl-, diethyl-, dibutyl-, diisobutyl-,butylbenzyl-, dicyclohexyl-, diethylhexyl-, di-n-octyl-, di-n-nonyl-,d i-iso-nonyl- and di-iso-decyl phthalate. The subsamples of theproducts were soxhlet extracted in dichloromethane, followed byanalysis of the extracts by gas chromatography and massspectrometry.

The content of one or more phthalates in seven of the investigatedprod ucts/ part(s) of the produ cts was found to be higher than themaximu m auth orised concentration, 0.05%.

Present work has been performed as technical sup port to DEPA


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Resum

I flge Milj- og Energiministeriets bekendtgrelse nr. 151 af 15.marts 1999 m legetj og and re artikler til brn i aldersgrupp e 0-3 r

ikke indeholde mere end 0,05% phthalater. I nrvrendeundersgelse er indholdet af phthalater bestemt i 15 produkter(legetj og and re artikler til brn i aldersgrupp en 0-3 r) efter enanmodning fra Miljstyrelsen. Produkterne blev modtaget fraMiljstyrelsen og analyseret for indholdet af dimethyl-, diethyl-,dibutyl-, diisobutyl-, dicyclohexyl-, butylbenzyl-, diethylhexyl-, di-n-octyl-, di-n-nonyl-, di-iso-nonyl- og di-iso-decyl ph thalat. Delprver afprodukterne blev soxhlet ekstraheret i dichlormethan, efterfulgt afanalyse af ekstrakter ved gaskrom atografi og massespektrom etri.

Indholdet af en eller flere phthalater i syv af de undersgteprod ukter/ delprodu kter var hjere end 0,05%, den hjest tilladtekoncentration.

Arbejdet er ud frt som bistand sopgave for Miljstyrelsen.


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1 Introduction

The Statutory Order of Danish Ministry of Environment and EnergyNo. 151 of 15th March 1999 regulates the content of phthalates in toys

and other children articles for the age grou p 0-3 years (1). The toys aswell as other articles, which children may put in the mouth, shouldnot contain > 0.05% ph thalate accord ing to th e Statu tory Order. In theStatutory Order, all diesters of o-phthalic acid have been consideredas ph thalates. This mean s that most of the common ly usedphthalates in children's products are covered by the Danishregulation. The European Commision (EC) has also implemented arestriction on phthalate content in toys and other articles for childrenin the age group 0-3 years (2). The EC regulation is, however,temporary and that concerns only six phthalates: dibutyl phthalate(DBP), butylbenzyl phthalate (BBP), di-n-octyl phthalate (DnOP),

diethylhexyl phthalate (DEHP), diisononyl phthalate (DINP) anddiisodecyl phthalate (DIDP). Furthermore, according to the ECregulation, the maximum authorised concentration of thesephthalates (total phthalate content) in toys and other articles forchildren in the age group 0-3 years is 0.1% (w/ w).

The Danish Environmental Protection Agency (DEPA) requested theNational Environmental Research Institute (NERI) to determinecontents of ph thalates in toys and other articles for children in the agegroup 0-3 years, to check the compliance of these products with theDanish Statutory Order. In the present investigation, contents ofsome commonly used phthalates in consumer products, includingthose regulated by EU (in toys), have been determ ined in 15 produ ctsprovided by DEPA.

Present work has been performed as technical sup port to DEPA.


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2 Products

DEPA provided 15 produ cts for the analysis of ph thalate content(Table 1). The p rod ucts w ere collected in December 2002 from Danish

retail outlets. DEPA specified the p art(s) of each p roduct tha t shou ldbe analysed for the content of phthalates.

Table 1. Toys and other ar ticles analysedNERI

Reg.No.

MST No. Product identification Product description

3-0001 675 Build ing blocks Soft Build ing blocks3-0002 676 Santa Claus Inflatable figure, to be blown up3-0003 677 Book Laminated cardboard book3-0004 678 book Laminated cardboard book3-0005 679 Hippopotamus + 3

pu ps + 2 bathing rings

Hipp opotamu s shaped as a bath tub, pups and

inflatable rings3-0006 680 Tooth brush Yellow shaft covered with soft blue material3-0007 681 Tooth brush Blue shaft covered with soft yellow material3-0008 682 Book Laminated cardboard book3-0009 683 Book Laminated cardboard book3-0010 684 Book Laminated cardboard book3-0011 688 Bib Cotton bib with soft plastic lining3-0012 689 Bib Cotton bib with soft plastic lining3-0039 674 Cash register A cash register with keyboard , calculator, etc.3-0040 704 Bull A solid figure made of p lastic material3-0041 705 A chicken on a boat A soft chicken melted on a soft boat


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3 Analysis

The products were analysed for the content of following phthalates:dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl

phthalate, dibutyl phthalate (DBP), dicyclohexyl phthalate (DCHP),d i-n-octyl phthalate (DnOP), diethylhexyl phthalate (DEHP), di-n-nonyl phthalate (DNP), diisononylphthalate (DINP), diisodecylphthalate (DIDP) and butylbenzyl phthalate (BBP). Duplicatesubsamples of each product were soxhlet extracted indichloromethane followed by analysis using gas chromatography -mass spectrometry (GC-MS) and GC-flame ionisation detection (GC-FID), as described previouly (3, 4).

3.1 Experimental

For qualitative analysis, 1 g sample was soxhlet extracted in 100 mldichloromethane for 16 h at 66C. 90 ml of the extract wereconcentrated to 10 ml using a rotary evaporator. 1l of theconcentrated as well as non-concentrated extract was analysed byGC-MS as described in 3.2.1. For quantification, fresh extracts of thesamples were prepared so that concentration/ dilution of the extractswas avoided, and subsequently analysed by GC-FID as described in3.2.2. All samples were an alysed in du plicate, both for qu alitative andfor quan titative analysis.

The recoveries of all phthalates at two concentration levels (600 mg/ L

and 6000 mg/ L for DINP and DIDP, and 60 mg/ L and 600 mg/ L forall other phthalates) were determined by the extraction of knownamoun ts of phthalates un der th e same conditions as the samples.

Calibration curves of all phthalates, except DINP and DIDP, wereprepared by analysing solutions of respective standard chemicals atseven concentra tions (40 mg/ L-2000 mg/ L). The DIN P calibrationcurve was prepared by analysing 200 mg/ L-10000 mg/ L solutions ofthis chemical. DIDP was determined as DINP because some of theGC peaks of isomers of these substances overlapped . Thu s, it w as notnecessary to prepare calibration curve of DIDP. In each GC run, 3

calibration standard solutions of the phthalates concerned wereanalysed after every 2-3 samples (4-6 extracts). These calibrationcurves were used for the quantification. Each standard solution aswell as sample extract was analysed two times by GC-FID. Thecontents of phthalates in a sample extract was calculated using thecalibration stand ard s analysed closest (in GC-sequen ce) to the samp leextract.

Repeatability of the determination (precision) was calculated by 10consecutive GC analysis of phthalate standard solutions at twoconcentration levels: 2000 mg/ L and 6000 mg/ L for DINP; 4000mg/ L and 10000 mg/ L for DIDP; and 200 mg/ L and 1000 mg/ L forall other phtha lates.


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The identification of phthalates was performed by comparing the GCretention times and mass spectra of the sample peaks with theretention times and mass spectra of phthalate standards. Moreover,the chromatographic pattern of isomeric DINP and DIDP wasconsidered for the id entification of these phth alates. From th e resultsof qualitative analysis, approximate concentrations of the phthalates

present in the respective samples were calculated. On the basis ofthese results, fresh extracts of the samples were prepared, where theamount of the sample and the volume of extraction solvent wereadjusted so that no concentration/ dilution of the extract w asnecessary for the quantification (in most cases). In every second set ofsoxhlet extraction (eight extractions p er set), a blank w as included .

3.2 Chromatographic conditions for phthalate

analysis

3.2.1 GC-MS

Intstrument: Perkin Elmer Turbomass mass spectrometer coupledto AutoSystem XL gas chrom atograph w ithsplit/ splitless injector

Transfer line: Direct to ion source, 310C

GC column : Chrompack fused silica column CP-Sil-5CB, 50 m x 32mm , d f 0.12 m

Temperature

program: Start temp erature 150C, 5C to 280C, 5 min at280C

Carrier gas: He, 55 ml/ min, column head pressure 19.5 psi

Injector: Split, 300C, injection volum e 1 l

Ion source: 7 eV, 175C, +ve ion mod e, scan m/ z 33-300 in 1 sec

MS Library: NBS and Wiley

3.2.2 GC-FID

Instrum ent: Hewlett Packard (HP) gas chromatogr aph 5890A

with split/ splitless injector, flame ionisation d etector,HP autosamp ler 7673A and HP Chemstation.

GC column : Chrompack fused silica column CP-Sil-5CB, 50 m x0.32 mm, d f 0.12 m

Temperatureprogram: Start temp erature 150C, 5C to 280C, 5 min at

280C

Carrier gas: He, 55 ml/ min, column head pressure 19.5 psi

Injector: Split, 300C, injection volum e 1 l

Detector: Flame ionisation, 300C, make-up gas N 2 30 ml/ min


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4 Results and Discussion

The analyses of ph thalate contents in the produ cts were performed intwo steps. In the first step, a screening analysis for the identification

of phthalates as well as an estimation of their concentration in thesamp le extracts was performed. This was followed by quan titativedetermination of the identified phthalates in fresh sample extracts,wh ere relevant calibration standard s were an alysed together w ith theextracts. The qualitative analysis of phthalates was performed usingGC-MS. GC-FID was used for the quantification of the identifiedphthalates. The GC-MS method used in the present investigation isan extension of the GC-FID method (3, 4), that has previously beenproved to be suitable for the identification and determination ofphthalates in toys. As described below, the important characteristicsof the method (stability of the GC-retention time, calibration range,

recovery, repeatability of determination, etc.) were checked in thepresent investigation, and they were found satisfactory for theanalysis of ph thalate content in toys.

The GC retention times (tR) of the investigated p htha lates were stablethrough out the study, with a maximum variation


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phthalates. The relative standard deviation (RSD) for thedeterm ination of all ph thalates was within 5%.

For the determination of the phthalate content in the products, freshsample extracts were prepared so that concentration/ dilution of theextracts before GC analyses was avoided in most cases. Thedetermination was performed in duplicate samples using 3-pointcalibration curves prepared by the analysis of the relevant standardsolutions run in the same sequence as the samples. The GC-sequencewas designed so that appropriate standard solutions were analysedbefore and after each set of 2-3 samples (in duplicate). The calibrationstandards were selected to match the estimated concentrations ofphthalates in the sample extract. The regression line equation wasused for the quantification. The determ ination revealed that thecontent of phthalates in a product was similar or very close to theestimated concentrations derived from the screening analysis. Whena product contained DINP as well as DIDP, GC chromatograms ofwhich overlap partly (Figure 1), the content of both of these

phth alates in the produ ct was determined together as DINP.

The results of the analysis of phthalate contents in the investigatedprod ucts/ par t(s) of the produ cts are described in Table 2. Of the 15products (toys and other articles for children) investigated in thepresent study, one or more of the phthalates were found in 10products. Among the investigated phthalates, BBP (


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investigated p rodu cts was higher than the m aximu m allowedconcentration.

Table 2: Phthalate content in the investigated toys.

NERIReg. No.

DEPANo. The part/p iece of the toy analysed

Phthalate contentPhthalate Content

(% w/w)

3-0001 675 Build ing blocksGreenYellowBlue

---

---

3-0002 676 Plastic material from thehead

- -

3-0003 677 Book, subsamples of page 3/ 4 DBPBBP

0.1530.010

3-0004 678 Book, subsamples of pages 7/ 8 and9/ 10

DBPDIBP

0.0040.226

3-0005 679 Bathing ring

Hippopotamu s tub

DEHPDINP+DIDP

-

28.9761.666

-

3-0006 680 Blue material on the shaft - -3-0007 681 Yellow material on the shaft - -3-0008 682 Book, subsamples of pages 3/ 4 DBP

BBP0.4630.019

3-0009 683 Book, subsamples of pages 3/ 4 DBP < 0.0053-0010 684 Book, subsam ples of back pages DBP

DIBP< 0.0050.032

3-0011 688 Soft lining material DBPDEHP

< 0.0050.189

3-0012 689 Soft lining material BBPDEHPDINP

< 0.00514.8001.202

3-0039 674 Keys 0 and 1 of the keyboard DIBPDEHP

< 0.0050.0365

3-0040 704 Solid material from the back sid e of the figure

- -

3-0041 705 Boat material DINP 37.290


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Figure1:GC-separationofinvestigatedphthalates.DINPandDIDPap

proximately0.6%andotherph

thalatesapproximately0.04%.


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Figure 2: GC chrom atogram of the extracts of laminated cardboard books 3-0003 (A) 3-0004 (B).

A

B


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Figure 3: GC chrom atogram of the extracts of bathing ring 3-0005 (A) and laminated cardboard book 3-

0008 (B).

A

B


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Figure 4: GC-chrom atogram of the extracts of bib samples. 3-0011 (A) and 3-0012 (B).

A

B


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Figure 5: GC-chromatogram of the extract of chicken on the boat (3-0041)


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5 References

1. Milj- og Energiministeriets bekendtgrelse nr. 151 af 15. mar ts1999Bekendtgrelse om forbud mod ph thalater i legetj til brn i

alderen 0-3 r samt i visse smbrnsar tikler m.v.2. Forslag til Europa-Parlamen tets og Rdets Direktiv om toogty-

vende n dring af Direktiv 76/ 769/ EF om indbyrd es tilnrmelseaf med lemstaternes adm inistrativt eller ved lov fastsattebestemm elser om begrnsning af markedsfring og anvend else afvisse farlige stoffer og pr parater (phthalater) og om nd ring afRdets direktiv 88/ 378/ om ind byrdes tilnrm else afmed lemsstaternes lovgivning om sikkerhed skrav til legetj.1999/ 0238 (COD).

3. Rastogi S. C. (1998) Gas chrom atograp hic analysis of ph thalate es-

ters in plastic toys. Chromatograp hia 47: 724-726.

4. Rastogi S.C., Worse I.M., Kpp en B., Hansen A.B. and AvnskjoldJ. (1997) Ind hold af organiske op lsningsmidler og ph thalater ilegetj. Danmarks Miljundersgelser, 34 s- Faglig rapport fraDMU, nr. 217.


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Documents

Compliance Testing of Phthalates in Toys - Analytical Chemical Control of Chemical Substances and Products