Method Validation for 16 Trace

Element Determinations in
Polypropylene and High Density
Polyethylene by ICP-MS

Application Note

Authors Abstract
Elisabete S. Saron, Plastic materials used in food packaging may be contaminated with substances
Marcelo A. Morgano, hazardous to human and environmental health, among them, potentially toxic
Paulo H. M. Kiyataka, and elements that can migrate into the food. The analysis of plastic materials for
Sílvia T. Dantas elemental determination presents challenges from the assurance of sample
Institute of Food Technology homogeneity/representativity, through digestion and quantification. The Agilent
Campinas, SP, Brazil 7700 Series ICP-MS System is a powerful tool for quantification of potentially toxic
elements, capable of detecting trace level concentrations even in a complex matrix,
Fabio F. Silva
such as digested polymers, by the unique High Matrix Introduction (HMI) system.
Agilent Technologies Brasil
This application note presents the method validation for 16 element determinations
São Paulo, SP, Brazil
in samples of polymers used in food packaging.
Gabrielle F. Santos and Solange Cadore
University of Campinas
Campinas, SP, Brazil
Introduction Experimental
In 2011, Brazil produced 6.502 million tons of processed plas- All the solutions in this work were prepared using reagents
tics, and 16 % of the total (1,040 tons) was used to produce with analytical grade and ultra-purified water 18.2 MW cm
packaging for food and beverages, of which 25 % was from a Milli-Q system (Millipore Merck, Darmstadt, Germany).
polypropylene (PP) and 21 % was high density polyethylene The solutions used as standards for calibration curves were
(HDPE) [1]. Scientists and authorities are concerned because prepared from individual stock solutions containing 1,000 mg/L
plastic materials can be contaminated with elements that of each these elements: Li, B, Cr, Mn, Fe, Co, Cu, Zn, As, Se,
cause harm to human health and environmental disequilib- Cd, Sn, Sb, Ba, Hg, and Pb (Fluka, Sigma-Aldrich, USA and
rium. Contamination may come from the raw materials used Merck, Darmstadt, Germany). A Ge, In, Sc, and Y solution con-
in plastic production, catalyst residues used in polymerization taining 250 µg/L (Specsol, São Paulo, Brazil) of each element
processes, additives (thermal stabilizers), pigments, and even was used as on line internal standard.
material processing [2]. These potentially toxic elements,
when present in food packaging, can migrate into the product, Before acid digestion, the samples of HDPE and PP were
representing a risk of ingestion by the consumer. The pres- ground using a cryogenic mill. Approximately 4 g of
ence of these elements in polymeric materials may prechopped sample were placed in a 50 mL stainless steel jar
constitute a risk of environmental contamination when this from CryoMill (Retsch, Haan, Germany), together with a
material is disposed improperly. 25 mm stainless steel grinding ball. Then, the sample was
submitted to the grinding program shown in Table 1.
An assessment of contamination magnitude by determining
the concentration of potentially toxic elements in plastic
materials is the first step to contamination control and risk Table 1. Cryogenic Grinding Program Used for Homogenizing Polymeric
Material Samples
evaluation, and the elements of interest in samples can vary
in concentration level from low ppb (µg/kg) to ppm (mg/kg). Step Time (min) Frequency (MHz) Liquid nitrogen
Precooling 10 – X
To achieve the required performance, one needs a sensitive
technique to measure low concentrations of elements in the Milling 1 2 25 –
digested samples, a wide linear working range, method linear- Intermediate cooling 2 – X
ity for more concentrated elements, and a robust system to Milling 2 2 25 –
maintain long-term stability in a large batch of analyses.
Multi-element quantification at low levels and determination
of isotopic ratios capabilities in plastic materials samples
using ICP-MS has been demonstrated by GINÉ-ROSIAS et al.
[3]. The Agilent 7700 Series ICP-MS has all the features
required to perform plastic material analysis for ultra-trace
elemental determination, including the unique HMI
(High Matrix Introduction) system, which increases plasma
robustness even when heavy matrix samples are analyzed by
ICP-MS.

The objective of this study was to develop and validate a

method for the determination of 16 elements chosen to cover
the main legislations on food packaging safety in Brazil [4,5]
and Europe [6] (Li, B, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Cd, Sn,
Sb, Ba, Hg, and Pb) in samples of HDPE and PP used for food
packaging.

2
The ground polymer samples were submitted to acid digestion
in a closed system, assisted by microwave heating.
Approximately 200 mg were weighed in Teflon vessels using
an analytical balance (A-250, Fisher Scientific), with a 10–4 g
resolution. Subsequently, 5 mL of HNO3 65 % m/v and 2 mL of
H2O2 48 % m/v (both from Merck, Darmstadt, Germany) were
added, followed by 1 mL of ultrapure water, then this mixture
was kept standing for 1 hour at room temperature to allow
reaction between the samples and the digestion mixture. All
the vessels were closed and the digestion was run in an
ETHOS 1 microwave system (Milestone, Italy) using a 4-stage
program with a maximum temperature of 220 °C, and total
time of 50 minutes, as shown in Table 2. The digest solutions
were quantitatively transferred to a 50 mL volumetric flask
using ultrapure water.
For elemental quantification, the 7700 Series ICP-MS System
(G3281A) was used, fitted with the Agilent I-AS Autosampler
(G3160B), a standard sample introduction system (MicroMist
glass concentric nebulizer, quartz double pass spray chamber,
connector tube with dilution port for High Matrix Introduction
(HMI), Quartz torch with 2.5-mm id, and standard nickel
cones. The 7700 Series ICP-MS System tuning was based on
Materials Preset Method from ICP-MS MassHunter Software.
He and HEHe (High Energy) modes were used in this method.
Table 3 shows the tuning conditions.
The parameters evaluated for method validation according to
the document DOQCGCRE-008 [7] were calibration curve lin-
earity (R), precision, and accuracy. The limit-of-detection
(LOD) and limit-of-quantification (LOQ) were calculated as 3 s
and 10 s, respectively [8].

Table 2. Heating Program Used to Digest Plastic Materials

Step Ramp time (min) Temperature (°C) Hold time (min) Table 3. Agilent 7700 Series ICP-MS System Operating Conditions
1 5 110 10 Agilent 7700 Series ICP-MS System parameters
2 5 170 10 RF power 1,600 W
3 5 220 30 Plasma gas flow 15 L/min
Auxiliary gas flow 0.9 L/min
Carrier gas flow 0.35 L/min
For the method validation, a certified reference material
Argon flow for aerosol dilution (HMI) 0.6 mL/min
(CRM) of Low Density Polyethylene - ERM-EC680k (acquired
Number of elements/internal standards 16/3
from the Institute for Reference Materials and Measurements,
IRMM, Geel, Belgium) was used, with certified concentration Replicate/peak pattern/sweeps 3/1/100
values for As, Pb, Cd, Hg, Sb, and Zn. To determine the accu- Reading time 2.4 minutes
racy of other elements, a standard addition was made into the Cell tuning modes He/HEHe
CRM. A standard addition of all elements was done in three Sample depth 10 mm
levels (L1, L2, and L3) in HDPE and PP resin samples with Shift time between modes (He/HEHe) 10 seconds
and without additives containing 0.3 % m/m of magnesium He cell flow on HEHe mode 10 mL/min
stearate.
Kinetic energy discrimination on HEHe mode 7V
He cell flow on He mode 5 mL/min
Kinetic energy discrimination on He mode 5V

3
Method development and validation
During the method development, it was observed that, even
after sample digestion, the measurements made in triplicate
of the same solution showed high values of standard devia-
tion. To correct this effect, Ge, In, Sc, and Y were used as
internal standards. Each element from the internal standard
solution was chosen for signal correction for each analyte.
The empirical criteria used to choose the best internal
standard for each analyte was the standard deviation from
the measurements (triplicate) and the certified reference
material/spike recovery. However, internal standardization
was not enough, and the method still presented drift, and the
long term stability was not good. It was necessary increase
the plasma robustness. Therefore, the high matrix tuning was
adopted using preset method conditions when the HMI
system was applied. The HMI system introduced an argon Figure 1. High Matrix Introduction (HMI) System operation.
flow in the connection between the spray chamber and the
torch, perpendicular to the sample aerosol stream, promoting
an aerosol dilution controlled by means of a sophisticated CV values were below 6.5 % for all elements except Sn, which
tuning algorithm. Figure 1 presents a schematic of the showed 10 % for precision. However, all elements had values
system. After HMI application, 140Ce16O+/140Ce+ ratios below the maximum CV (15 %) calculated according to
dropped from approximately 1.5 % to less than 1 %, and Horwitz [9]. Thus, the method can be considered precise.
method precision was improved considerably, allowing
adequate performance for method validation. The recoveries obtained after CRM analysis were between
90% and 110% for all elements, indicating the method is
For method validation, the calibration curve linearity was eval- accurate. The accuracy was also assessed by recovery in
uated by correlation coefficient (R). For all the elements, samples of HDPE and PP (n = 3) with standard addition in
R was more than 0.99 in the following ranges: 0.5–40 µg/kg three concentration levels (low-L1, medium-L2, and high-L3)
for Hg; 2–200 µg/kg for Cd, Sn, Sb, and Pb; 5–60 µg/kg for As in relation to calibration curves, this test was run on two
and Se; 10–300 µg/kg for Cr, Co, and Cu; 300–1,000 µg/kg for days.
B, and 100–1,000 µg/kg for Li, Mn, Fe, Zn, and Ba.
Although the CRM ERM-EC680k has a certified mean value of
After initial calibration, a sequence with 10 analytical blank 20.2 ± 1.1 mg/kg for Cr, depending on the sample intake as
measurements was run to find standard deviation (s) and cal- well as on digestion conditions (acid mix, temperature, pres-
culate detection limits (LOD = 3 x s) and quantification limits sure) obtained by conventional acid digestion, the measured
(LOQ = 10 × s). Precision was calculated using the coefficient values ranged from 2.9 mg/kg up to 16.2 mg/kg [10]. In this
of variation (CV with n = 9), and accuracy was evaluated by study, the mean value obtained for Cr was 4.89 mg/kg.
analyte recovery. In both cases, determination was done Therefore, the recovery for Cr presented in this study was
using certified reference material Low Density Polyethylene- based on the concentration of standard added on CRM.
ERM-EC680k (CRM). The values obtained are given in Table 4.
The average values for samples of HDPE and PP with
standard addition in three levels are given in Tables 5 and 6,
respectively.

4
Table 4. Isotopes Evaluated, Cell Mode, Internal Standard, LOD, LOQ, Precision (CV – Coefficient Variation), and Accuracy for Elements Studied

Accuracy (%)
Internal LOD LOQ Precision Analyte expected
Isotopes standard Cell mode (µg/kg) (µg/kg) CV (%) concentration (mg/kg) CRM Spiked CRM
7Li In115 He 3.1 10.2 2.7 0.40(1) -- 90.9
11B In115 He 64.4 214.5 6.4 0.40(1) -- 94.6
52Cr Sc45 HEHe 0.3 0.9 5.2 0.05(1) -- 99.2
55Mn Ge72 HEHe 0.5 1.6 1.4 0.40(1) -- 103.1
56Fe Y89 He 19.3 64.4 2.5 0.40(1) -- 98.4
59Co Ge72 He 0.2 0.5 4.3 0.05(1) -- 100.7
63Cu Sc45 He 0.2 0.7 6.4 0.05(1) -- 83.6
64 Zn In115 He 9.3 31.0 4.3 137 ± 20(2) 91.7 --
75As Ge74 He 0.1 0.2 4.5 4.1 ± 0.5(2) 83.6 --
78Se In115 HEHe 0.2 0.6 2.7 0.015(1) -- 104.9
111Cd Y89 He 1.6 5.2 1.8 19.6 ± 1.4(2) 83.3 --
116Sn Sc45 HEHe 2.1 7.1 10.0 15.3 ± 2.8(2) 81.8 --
123Sb Ge74 He 0.1 0.3 4.3 10.1 ± 1.6(2) 87.0 --
137Ba In115 He 0.5 1.6 2.6 0.40(1) -- 100.6
202Hg Ge74 He 1.4 4.7 4.3 4.64 ± 0.20(2) 110.1 --
206Pb Ge74 He 1.1 3.6 3.8 13.6 ± 0.5(2) 98.8 --

(1) Concentration of standard addition on CRM

(2) Certified value of analyte concentration in CRM

Table 5. Results Obtained at Recovery Test for HDPE and HDPE Added with Magnesium Stearate, Evaluated at
Three Concentration Levels (Low-L1, Medium-L2, and High-L3)

Spike in HPDE and HPDE with Recovery (%)(1)

magnesium stearate (µg/kg) HPDE HPDE + Mg stearate
Isotope L1 L2 L3 L1 L2 L3 L1 L2 L3
7Li 150 500 900 97.2 95.9 94.7 92.2 100.9 98.0
11B 350 450 900 96.4 104.4 107.9 95.9 106.9 114.1
52Cr 20 80 250 103.1 102.3 103.3 102.3 100.3 103.4
55Mn 150 500 900 102.0 100.7 100.0 100.9 99.1 101.5
56Fe 150 500 900 88.8 101.2 99.2 88.8 102.2 101.7
59Co 20 80 250 97.2 107.9 103.8 101.4 103.5 106.0
63Cu 20 80 250 102.2 100.5 104.3 92.9 105.4 101.6
64Zn 150 500 900 95.8 94.6 92.5 103.2 97.1 95.2
75As 8 20 50 101.9 108.7 103.0 106.2 103.4 105.3
78Se 8 20 50 96.7 99.6 99.1 90.0 99.1 98.2
111Cd 4 40 150 99.2 96.9 95.4 97.6 101.3 96.7
116Sn 4 40 150 115.7 112.3 123.1 114.5 111.9 114.1
123Sb 4 40 150 115.7 128.6 123.4 112.4 114.7 124.3
137Ba 150 500 900 100.3 100.4 98.1 97.9 102.3 101.1
202Hg 8 20 50 104.7 109.5 113.7 111.1 110.6 114.3
206Pb 4 40 150 103.7 109.3 102.8 112.6 107.3 105.4
(1) Average values of three determinations carried out on two different days.

5
Table 6. Results Obtained at Recovery Test for PP and PP Added with Magnesium Stearate, Evaluated at
Three Concentration Levels (Low-L1, Medium-L2, and High-L3)

Recovery (%)(1)
Spike in PP and PP with
magnesium stearate (µg/kg) PP PP + Mg stearate
Isotope L1 L2 L3 L1 L2 L3 L1 L2 L3
7Li 150 500 900 108.1 105.1 107.6 107.0 110.6 108.5
11B 350 450 900 95.8 97.2 100.2 107.2 102.5 101.2
52Cr 20 80 250 92.3 96.5 103.3 103.4 102.7 103.6
55Mn 150 500 900 99.7 100.1 100.9 100.7 100.8 102.2
56Fe 150 500 900 114.3 102.9 103.3 102.5 103.6 104.0
59Co 20 80 250 102.4 103.8 104.0 112.7 105.2 106.7
63Cu 20 80 250 99.00 97.4 102.7 100.8 104.9 105.4
64Zn 150 500 900 81.4 89.0 89.1 87.1 94.2 92.3
75As 8 20 50 91.8 94.4 97.4 95.7 99.6 97.8
78Se 8 20 50 91.0 98.7 100.9 95.4 101.4 102.4
111Cd 4 40 150 105.3 97.8 96.2 103.3 99.6 97.0
116Sn 4 40 150 94.6 118.6 126.1 87.3 126.8 125.0
123Sb 4 40 150 96.0 110.5 112.2 81.8 112.4 111.7
137Ba 150 500 900 99.2 99.4 100.0 103.3 103.3 104.2
202Hg 8 20 50 100.6 106.9 112.5 94.3 103.1 107.4
206Pb 4 40 150 94.2 93.2 93.6 88.9 94.1 91.4

(1) Average values of three determinations carried out on two different days.

The recoveries obtained in this test were between 80 % and
120% for most elements in the three concentration ranges
measured for the two polymer types studied. Only the
elements Sn and Sb show recoveries over 120 %.
The data shown in Table 6 demonstrate satisfactory method
performance and the possibility of their application in real
samples, for which the results are shown next.
HDPE and PP analysis
To evaluate the method performance for plastic samples with
different metal concentrations, samples of HDPE and PP were
specially produced by Multicel Pigmentos Indústria
e Comércio Ltda (São Paulo, Brazil) spiked with known per-
centages of pigments. The samples were analyzed applying
the method proposed in this study as shown on Table 7.
Looking at the data above, it is possible to realize the impor-
tance of some features of this method such as sensitivity,
robustness, and wide linear range. Some samples exhibit very
low levels of very toxic elements such Cd, Hg, and Pb, and in
spite of the 250 times dilution factor from sample digestion it
was possible to quantify these low levels in some samples.
The robust plasma associated with on-line internal standards
keeps the standard deviation at a low level. The wide linear
range allows quantifying elements from µg/kg level to g/kg
levels.

6
Table 7. Results Obtained at CRM for HDPE and PP Samples Produced with Known Percentages of Pigments, mg/kg
HDPE + HDPE
Isotope Result CRM(3) HDPE Mg stearate orange PP PP blue PP black
52Cr A 4.89 ND ND 0.04 0.29(2) 143.25 1001.15
SD 0.72 (4) (4) 0.01 0.07 7.45 82.88
Min 3.36 (4) (4) 0.02 0.24 134.66 942.38
Max 5.64 (4) (4) 0.05 0.33 147.93 1095.95
55Mn A ND ND ND 0.04 ND 0.31 215.21
SD (4) (4) (4) 0.02 (4) 0.02 9.54
Min (4) (4) (4) 0.02 (4) 0.29 207.57
Max (4) (4) (4) 0.05 (4) 0.33 225.90
56Fe A ND ND ND ND 8.55(2) 45.71 14.29
SD (4) (4) (4) (4) 1.36 3.86 0.94
Min (4) (4) (4) (4) 7.59 41.31 13.35
Max (4) (4) (4) (4) 9.51 48.54 15.22
59Co A 0.04 ND ND ND ND 153.17 1.65
SD 0.01 (4) (4) (4) (4) 13.83 0.06
Min 0.03 (4) (4) (4) (4) 137.23 1.59
Max 0.06 (4) (4) (4) (4) 162.24 1.70
63Cu A 14.44 ND ND ND ND 0.36 914.32
SD 0.34 (4) (4) (4) (4) 0.02 76.88
Min 14.05 (4) (4) (4) (4) 0.34 852.43
Max 15.03 (4) (4) (4) (4) 0.39 1000.38
64Zn A 125.56 ND 1.64(3) 127.22 ND 2.08(2) 2.99
SD 5.40 (4) 0.33 0.33 (4) 0.10 0.13
Min 117.21 (4) 1.41 126.91 (4) 2.01 2.84
Max 132.89 (4) 1.87 127.57 (4) 2.15 3.10
75As A 3.43 ND ND ND ND ND ND
SD 0.16 (4) (4) (4) (4) (4) (4)
Min 3.10 (4) (4) (4) (4) (4) (4)
Max 3.59 (4) (4) (4) (4) (4) (4)
78Se A 0.24 ND ND 575.89 ND ND ND
SD 0.05 (4) (4) 5.86 (4) (4) (4)
Min 0.18 (4) (4) 569.25 (4) (4) (4)
Max 0.33 (4) (4) 580.33 (4) (4) (4)
110Cd A 18.38 0.10 0.16 5508.00 ND ND ND
SD 0.47 0.04 0.05 105.18 (4) (4) (4)
Min 17.45 0.06 0.10 5393.06 (4) (4) (4)
Max 18.89 0.14 0.21 5599.46 (4) (4) (4)
116Sn A 12.52 0.26 0.27 5932.58 ND ND ND
SD 1.25 0.03 0.08 88.45 (4) (4) (4)
Min 11.01 0.2 0.21 5844.27 (4) (4) (4)
Max 14.29 0.27 0.36 6021.16 (4) (4) (4)

7
Table 7. Results Obtained at CRM for HDPE and PP Samples Produced with Known Percentages of Pigments, mg/kg (continued)
HDPE + HDPE
Isotope Result CRM(3) HDPE Mg stearate orange PP PP blue PP black
123Sb A 8.78 ND ND ND ND ND ND
SD 0.38 (4) (4) (4) (4) (4) (4)
Min 8.14 (4) (4) (4) (4) (4) (4)
Max 9.24 (4) (4) (4) (4) (4) (4)
137Ba A 7.58 ND ND 29.10 ND ND ND
SD 0.19 (4) (4) 1.10 (4) (4) (4)
Min 7.17 (4) (4) 28.16 (4) (4) (4)
Max 7.85 (4) (4) 30.31 (4) (4) (4)
202Hg A 5.11 0.33 0.16(2) 0.15(2) ND ND ND
SD 0.22 0.11 0.07 0.04 (4) (4) (4)
Min 4.82 0.22 0.12 0.12 (4) (4) (4)
Max 5.45 0.45 0.21 0.18 (4) (4) (4)
206Pb A 13.44 ND ND 0.12 ND ND ND
SD 0.52 (4) (4) 0.03 (4) (4) (4)
Min 12.61 (4) (4) 0.10 (4) (4) (4)
Max 14.01 (4) (4) 0.15 (4) (4) (4)

A/SD/Min/Max: Average/Standard deviation/Minimum value/Maximum value

(1) Three real replicates
(2) Two real replicates
(3) Nine real replicates
(4) Not applicable

ND: Not detected.

Li and B was not detected in any sample

Conclusion
This application note shows a validated method for plastic
materials analysis applied for two kinds of polymers (HDPE
and PP) and how the Agilent 7700 Series ICP-MS System fea-
tures can facilitate method development with tuning condi-
tions from preset methods, HMI for robust conditions with no
sensitivity losses, and wide linear range that allows g/kg
concentration quantification with no need for dilution.
This method can be applied to study plastic materials for food
packaging and support further studies related to migration of
elements from plastic materials to food. This method can help
in complying with current regulations regarding material dis-
posal such as the Coalition of northeaster governors (USA)
[11], European Parliament (Directive 94/62/EC) [12], and
RoHS - Restriction of Certain Hazardous Substances
(Directive 2002/95/EC) [13].

8
References
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Zn in two polyethylene reference materials” Certified
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