PBB and PBDE Analysis Under RoHS with Py-GCMS

Analysis of PBB and PBDE under RoHS Scope Using Py-GCMS Analysis of PBB and PBDE using Py-GCMS in accordance with the Restriction of Hazardous Substances (RoHS) directive.

Objective of the Study

RoHS; is a directive published by the European Union in 2003 that restricts the use of hazardous substances such as mercury (Hg), lead (Pb), and cadmium (Cd) in electrical and electronic equipment. The RoHS Directive aims to protect the environment and human health. The directive limits the quantities of hazardous substances as follows. • Lead (1000 ppm) • Mercury (1000 ppm) • Cadmium (100 ppm) • Chromium (1000 ppm) • Polybrominated Biphenyl (PBB) • Polybrominated Diphenyl Ether (PBDE) (1000 ppm) As of July 2019, phthalate compounds have been added to the scope of the RoHS Directive. Banned phthalates and their limits are specified as follows. • DEHP (Bis (2-ethylhexyl) Phthalate) (1000 ppm) • DBP (Dibutyl Phthalate) (1000 ppm) • BBP (Butyl Benzyl Phthalate) (1000 ppm) • DIBP (Diisobutyl Phthalate) (1000 ppm) This directive applies to manufacturers, authorized representatives, importers and distributors of the following products. • Large and small household appliances, • Information technology and telecommunications equipment, • Lighting, • Electrical tools, • Toys and entertainment equipment, • Sports equipment, • ATMs and vending machines, • Medical devices, • Monitoring and control instruments.

Method and Materials

Our study was conducted using a Shimadzu GCMS-QP2020 NX model GCMS. GCMS-QP2020 NX EGA/PY-3030D Multi-Shot Pyrolyzer

Analytical Conditions

Instrument: GCMS-QP2020 NX EGA/PY-3030D Column: Ultra Alloy PBDE (0.05 μm x 0.025 mm x 15 mm) Measurement Mode: Heart-cut method Pyrolysis Unit Furnace Temperature Program: 340°C 3 min Pyrolysis Interface Temperature: 300°C Injection Temperature: 300°C Linear Velocity: 52.6 cm/s Interface Temperature: 320°C Ion Source Temperature: 230°C Split Ratio: 50 Mode: SCAN Mode / SIM Mode Duration: 16 min

Equipment & Chemicals Used

1. GCMS with pyrolysis unit 2. Analytical balance (0.00001 g precision) 3. ERM EC591 4. Sample preparation kit 5. Sampling container (phthalate-free) 6. Glass wool

Assessment

For inspection of products containing 750 ppm PBB or PBDE, the liquid method is applied.

References

• "Ant Teknik Analysis of PBB and PBDE under RoHS Scope Using Py-GCMS Application Note" • Shimadzu Application Data Sheet No:45 • Analysis of Brominated Flame Retardants and Phthalate Esters In Polymers Under the Same Conditions Using a Pyrolysis GC-MS System (2) - Phthalate Esters • EN 62321-6:2015 Determination of certain substances in electrotechnical products Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry (GC-MS)   Prepared by Ömer Halit Turmuş Chemist Application Team Leader Ant Teknik