rohs_ test methods
DESCRIPTION
RoHSTRANSCRIPT
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RoHSTest Methods
Presented by:Bruce Peterson
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Motivation for Presentation
The EU RoHS directive takes effect July 1, 2006Customer confusion about -
Scope of directiveHow much testing needs to be performedAnalytical Testing Techniques AvailableExpected Costs
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Scope of RoHS Directive
What is included:Applies to any product which is dependent on electric current orelectromagnetic fields in order to work properly. Includes all non-electronic parts of the product.Voltage rating of product is less than 1000VAC or 1500VDC
What is NOT included:Spare parts for the repair , or the reuse, of electrical and electronic equipment put on the market prior to July 1, 2006Military EquipmentMedical EquipmentMeasurement and Control EquipmentLarge scale stationary industrial tools
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Specific Exemptions from RoHS
Mercury in compact fluorescent lamps (with restrictions)Lead in cathode ray tubes, light bulbs and fluorescent tubesLead as an alloying element in steel (< 0.35%), Aluminum (< 0.40%), Copper Alloy (< 4%)Lead in high melting temperature soldersLead in solders for servers, storage and storage array systemsLead in solders for network infrastructure equipment for switching, signaling, transmission and network managementLead in ceramic partsCadmium platingHexavalent chromium as an anti-corrosion of the carbon steel cooling system in absorption refrigerators
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Definitions
Unit –The smallest part of an electrical or electronic equipment that can be separated from the equipment by using ordinary tools, without destroying the function of the part when it is removed.
Mechanically Disjointed –Dismantling of a unit by simple processes (such as screwing, disconnecting and/or desoldering) using ordinary tools (i.e. not applying chemicals, cutting, grinding and/or polishing) without destroying the function of the unit.
Homogeneous Material –A homogeneous material cannot be “mechanically disjointed” into different materials. ”Mechanically disjointed” means that the materials cannot in principal be separated into other materials by mechanical methods such as unscrewing, cutting, crushing, grinding or abrasive processes
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RoHS Enforcement
RoHS is EU directiveEach member state will use the directive as model for local legislationEach member state will be responsible for enforcement testing
Enforcement testing will be regional and therefore may vary
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How Do I Comply with RoHS?
It is up to each company to:Assess riskBuild risk mitigation policyEstablish “due diligence” defense in case of litigation
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RoHS Concentration Limits
0.1 (1000ppm)Polybrominated diphenyl ethers (PBDE)
0.1 (1000ppm)Polybrominated biphenyls (PBB)
0.1 (1000ppm)Hexavalent Chromium (Cr6+)
0.01 (100ppm)Cadmium (Cd)
0.1 (1000ppm)Mercury(Hg)
0.1 (1000ppm)Lead (Pb)
Allowed Limit (% by weight)Substance
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Other RoHS Green Initiatives
RPCEP (Regulation for Pollution Control of Electronic Products –July 1, 2006JGPSSI (Japan Green Procurement Survey Standardization Initiative – July 1, 2006SB20 (Electronic Waste Recycling Act of 2003 – California, Jan 1, 2007“China RoHS” – March 1, 2007Also adopting EU RoHS directive: Australia, Canada, Korea, Taiwan
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RoHS Testing Decision Flowchart
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RoHS Analytical Method Flowchart
Sampleshomogenous materials
-plastics-metals
-PCB/components
EDXRFICP-OES
ICP, AASEDXRF
EDXRFICP-OES
Pb, Cr, Hg, = <700ppmBr = < 300ppmCd = <70ppm
High performance applicationEDXRF
screening for compliance Diphenyl-
Carbazide/HPLC
PASSRoHS compliant
GC-MS,FTIR, HPLC
Pb
Cd
Cr(VI)
Hg
PBB,PBDE
Pb, Hg >1300ppmCd = >130ppm
FAIL non-compliant
INCONCLUSIVE
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Energy Dispersive X-Ray Fluorescence
Nucleus
Valence electrons
Atom
Primary X-ray
Ejected electron
0
5
10
15
20
25
0 10 20 30 40 50 60 70 80 90Atomic number
Ene
rgy
(keV
)
Kα
Lα
Mα
Characteristic X-ray Energy
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Energy Dispersive X-Ray Fluorescence
X-ray Guide tube
Detector CCD Camera
Sample
Primary X-ray
Fluorescent X-ray
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Energy Dispersive X-Ray Fluorescence
X-ray Intensity (cps)
X-ray Energy (keV)
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Energy Dispersive X-Ray Fluorescence
More expensiveLN2 required
Best resolution (150eV)Best limit of detection for all RoHS elements
Si, Si(Li)
Resolution may not be good enough for some samplesSn Lα = 3.440KeV, Cd Lα = 3.134KeV (Δ = 306eV) Limit of quantification for Cd close to RoHS limit
Good resolution (275eV)Does not need LN2Can be used for portable systems
PIN diode
Won’t analyze all RoHS elementsHigh limit of detectionGood for Pb only
Fast Pb only screeningInexpensiveMeasure plating composition
Proportional Counter
LimitationAdvantageDetector Technology
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Energy Dispersive X-Ray Fluorescence
Other desired characteristics for XRFSmall X-ray spot sizeCapillary optics in favor of collimatorsEvacuated X-ray detector path for light element detection
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Fourier Transform Infra-Red Spectrometer (FTIR)
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Fourier Transform Infra-Red Spectrometer (FTIR)
Many sampling techniquesAttenuated total reflectance (ATR)Diffuse reflectance KBr pelletsTransmission or Reflectance using FTIR microscope
Detection limits are 30,000ppm Materials containing PBBs and PBDEs will generally have concentrations exceeding 5% (50,000ppm)
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FTIR Spectrum of PBBs and PBDEs
“Fingerprint region” for PPBs and PBDEs are in the 1000cm-1 to 1500cm-1 range
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Cr6 determination using “spot test”Based on ISO-3613Uses test solution with 1,5-diphenylcarbazideTest solution must be prepared not more than 8 hours prior to usePlace 1 to 5 drops on clean sampleA red/violet color will appear in a few minutes if Cr6 is present – ignore any color that appears much laterNegative result concludes Cr6 testing, positive result requires more testing for Cr6 quantification
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Atomic Spectrometry Equipment
Detection limits µg/liter
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Atomic Spectrometry Equipment
Orders of Magnitude of Signal Intensity
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Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES)
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Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES)
Used for quantifying Pb, Cd, Hg and Cr when XRF results are in the “uncertain range”Lowest detection limits (ppb to ppt range) No matrix interferencesAnalytical range good for over 5 orders of magnitude (less need for dilution) Requires sample digestion (turn into liquid) with strong acids –use microwave digestion system to accelerate processInstrument requires calibration against reference samples –good linearity in analytical range (fewer calibration points)Sensitivity of instrument may require sample dilution to prevent detector overload
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High Pressure Liquid Chromatography (HPLC)
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High Pressure Liquid Chromatography (HPLC)
Used for determination and quantification of PBBs, PBDEs when XRF total Bromine concentration is above limitsNeed extraction of PBBs and PBDEs from sample matrix –use FTIR first to identify matrix material for solvent determinationRequires calibration against reference standardsUsed for quantification of Cr6 when XRF total Chrome concentration (Cr6 + Cr3) is above limits - use reference standards or XRF results for quantificationNeed extraction of Cr from matrixUse photodiode array detector for best results
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Gas Chromatograph – Mass Spectrometer (GCMS)
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Gas Chromatograph – Mass Spectrometer (GCMS)
Use for quantification and identification of PBBs and PBDEs when XRF total Bromine concentration is above limitsMost accurate analytical technique for quantification of PBBs and PDBEsNeed extraction of PBBs and PBDEs from sample matrix – use FTIR first to identify matrix material for solvent determination Requires calibration against reference standards
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Analytical Testing Techniques
HighNeeds sample digestionDestructive testSingle element test
No matrix interferencesLow detection limitsHigh resolution
AA/AAS
HighNeeds sample extractionDestructive test
Low detection limitsHigh resolution
GCMS
HighNeeds sample digestionDestructive testMay need to dilute sample
No matrix interferencesLow detection limitsHigh resolution
ICP-OES/ ICP-MS
HighNeeds sample extractionDestructive test
Better detection limits than FTIRHPLC for PPBs and PPDEs
MedRequires Cr ion extractionBest for Cr6 quantificationCan be used with XRF results
HPLC for Cr6
LowNo quantificationFast go/no go test of Cr6 Diphenylcarbazide Test
LowHigh detection limits (≥ 30,000ppm)
Little sample prepNo reference samples
FTIR
LowMatrix interferencesSample absorption
No sample preparationNon-destructiveCan use FP mode
ED XRF
CostLimitationsAdvantagesAnalytical Technique
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Thank You!
Bruce PetersonAccolade Engineering Solutions949-597-8378www.AccoladeEng.com