Analysis of Polymer for EnvironmentalRegulationsThermo Scientific ARL PERFORM’X SeriesAdvanced X-Ray Fluorescence Spectrometers

IntroductionPlastic has become a leading material in the productionand packaging of intermediate and finished goods. Overthe last several decades, plastics have been accumulated,filling vast portions of landfills creating an ecologicaldisaster. The destruction or recycling of plastics and thegoods which contain them has lead to the potential releaseof these heavy metals as toxins into the environment.

In recognition of these effects and of the growing sizeof consumerism and waste sites, Europe and Japan areenforcing new regulations for monitoring the level ofhazardous substances in the manufacture, recycling anddestruction of products that include plastic, to prevent therelease of hazardous toxins into the environment duringincineration or any other treatment methods.

Waste Electrical and Electronic Equipment (WEEE)and Restriction of Hazardous Substances (RoHS)regulations have set rules regarding the highest tolerablelimit for certain metals (particularly Pb, Cd, Hg, Br andCr). For the given ranges specified in these regulations,XRF is the most appropriate solution featuring rapidity,ease of use and reliability.

InstrumentThermo Scientific ARL PERFORM’X series spectrometerused in this analysis was a 4200 watt system. This systemis configured standard with 6 primary beam filters, 4collimators, up to 9 crystals, 2 detectors, helium purge andour 6 GN Rh X-ray tube for ultra light element analysis.

The ARL PERFORM’X spectrometer offers theultimate in performance and sample analysis safety. Withits unique Protec-Ultra-Safe design, the instrument cancompletely protect the entire X-ray system. This feature isequipped with liquid cassettes recognition, insuring thatno liquid cassette will be subjected to vacuum causing thesample to rupture in the system. The ARL PERFORM’Xinstrument is also designed with over exposure technology,which automatically ejects a liquid samples if the X-rayexposure time is too long.

The Secutainer system protects the primary chamberby vacuum collecting any loose powders in a speciallydesigned container, easily removed and cleaned by anyoperator. The X-ray tube-shield provides total protection ofthe X-ray tube from sample breakage and liquid rupture.For the spectral chamber protection, the Protec-Ultra-Safe isfitted with a Be shutter designed for absolute protection ofyour goniometer during helium flush analysis.

CalibrationAnalyzing RoHS/WEEE elements requires the detection ofvery low X-ray intensities at the trace elementalconcentrations. For optimal analytical analysis, theconditions and parameters used in this measurement wereset to excite each element as much as possible whilekeeping the background as low as possible. Once achieved,background positions were determined and measured forevery element allowing for net intensity analysis.

A set of certified polymer standards were used in thecreation of the following regression plots. These plots arelinear regression of the known concentration plottedagainst the measured intensities.

Key Words

• ARL PERFORM’X 4200 W

• Polymer

• XRF

• X-ray fluorescence

• RoHS/WEEE

ApplicationNote: 41662

Regression plots

Figure 1: Hg Regression SEE = 0.0022%

Figure 2: Br Regression SEE = 0.0085%

v

Figure 3: As Regression SEE = 0.00017%

Figure 4: Pb Regression SEE = 0.0005%

Figure 5: Cd Regression SEE = 0.00046%

Figure 6: Cr regression SEE = 0.00034%

Note: SEE (Standard estimate of Error) was achieved using 32 secondcounting time for all elements except Cd which used 60 second.

ResultsFrom the above calibration, table 1 lists detection limitsfor all the elements analyzed using 100 second countingtimes. These limits demonstrate that the ARLPERFORM’X is an excellent instrument for RoHS/WEEE analysis in polymers.

Dynamic St.Dev. LoDElement Range (PPM) (PPM)

As LoD-0.05 0.57 1.7

Cd LoD-0.05 1.17 3.5

Cl LoD-0.08 0.47 1.4

Hg LoD-0.05 0.53 1.6

S LoD-0.06 1.13 3.4

Ti LoD-0.12 0.07 0.2

Pb LoD-0.05 0.43 1.3

Zn LoD-0.05 0.07 0.2

Cr LoD-0.05 0.10 0.3

Cu LoD-0.05 0.07 0.2

Ni LoD-0.05 0.07 0.2

Br LoD-0.05 0.07 0.2

Ba LoD-0.05 0.30 0.9

Table 1 Typical Calibration Range and Analytical Performance

Conclusion The results show that RoHS/WEEE analysis can easily beperformed with the ARL PERFORM’X sequential XRFspectrometer. The precision and accuracy are shown to bevery high in polymers for both routine and R&D analysis.

Furthermore, operation is made easy through thestate-of-the-art Thermo Scientific OXSAS software whichoperates with the latest Microsoft Windows® 7 packages.

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