View Full Version : XRF vs. Spark Test for RoHS Compliance Verification
Eusoof 18th March 2007, 06:59 AM I want to share my experience with my raw material supplier where i have use XRF machine to test if their material are compliance with RoHS requirement or not. From my finding that that raw material (lead substance) are exceed than 3500 ppm and then 3 times repeated test show the same result (note that xrf just for screening propose only). Then i have complaint to supplier that they said their use spark test that more reliable test than our. So my question are bellow :
1.)Although that XRF for screening purpose but show result same result (more than 3500 ppm) that means that material have problem?
2.)Can you share knowledge how to read the mill certtificate figure?
3.)What is spark test?
Thankz
harry 19th March 2007, 05:30 AM The results certainly look bad. In such circumstances, we normally have to ask the following questions:
Is your instrument calibrated?
Are you using the right or approved methods in your analysis? Sorry, but you sound rather green. Do you have recommended testing methods for RoHS?
Is the material homogeneous?
Are there any coating/painting over the tested area which may unduly affect the ray penetration and therefore results.
Have you been trained for this purpose?You should ask your supplier to show their test results or certificates from recognised independent labs and explain them. If you are not satisfied, you can arrange them to be tested at a lab of your choice.
I am not aware of what a spark test means but if XRF results are in doubt, the recommended method is to use inductively coupled plasma atomic adsorption or emission spectrometry (AAS or AES) method for more detail and accurate results.
fireonce 20th March 2007, 03:48 AM I want to share my experience with my raw material supplier where i have use XRF machine to test if their material are compliance with RoHS requirement or not. From my finding that that raw material (lead substance) are exceed than 3500 ppm and then 3 times repeated test show the same result (note that xrf just for screening propose only). Then i have complaint to supplier that they said their use spark test that more reliable test than our. So my question are bellow :
...
Thankz
I think you are right.
As I know, XRF's precision is above 70%,and the result of your company is available,you are supposed to confirm with your supplier again.
The spark-test method specified in this standard is intended for the detection of defects in the insulation or sheathing layers of electric cables. For single core cables with no outer metallic layer, the general process is accepted as being equivalent to subjecting samples of those cables to a voltage test in water. This standard specifies the operational requirements for the spark-test equipment, as well as the principal characteristics, functional parameters and calibration procedures for each type of test equipment
chergh 20th March 2007, 09:53 AM XRF isn't suitable for quantitative measurement, it's semi quantitative at best. The 3,500 ppm figure you have is unlikely to be accurate so you need to send off your material to be analysed using ICPMS. Once you have that you can go to your supplier.
As for spark testing??? I think your supplier must have misunderstood you as how a spark test is going to give information on lead content is beyond me.
harry 20th March 2007, 10:36 AM The OP is referring to the Optical emission spectrometry (OES) using arc and spark excitation method and not the leakage test which has nothing to do with RoHS.
I am not familiar with this method although its being used quite extensively in the metal industry but had not seen it being recommended in any RoHS related documents.
Benjamin28 20th March 2007, 10:42 AM Optical Emission Spectrometry using arc/spark is indeed the preferred method for chemical composition analysis over XRF.
I wonder if your XRF is appropriately calibrated. I suppose if you really wanted to pursue it further you could have an independant lab analyze the sample and compare the results, somewhat like a round robin test.
Interestingly enough, spark testing in the old days used to be performed by operators who needed to quickly identify an alloy type, they would put the metal against a grind wheel and by seeing how long the spark was that it created, it's brightness and color they could determine what alloy they were holding. I'm certain your material supplier is using OES spark/arc and not the old spark method though lol.
What specifically are you asking about as far as interpreting certificate results?
One other thing, as stated in a previous post, XRF is semi-quant, meaning that you can find that XY elements are detectable at approximate levels, so your >3500ppm may well be incorrect as it is an approximation, whereas the spark test will tell you with much greater accuracy what % or ppm of that element is present.
chergh 20th March 2007, 10:56 AM Using oes is certainly better than XRF, just never heard oes methods referred to as a spark test.
XRF should be seen as indicative only and should not be used quantitavley. The official method for determining lead content for RoHS is ICPMS (inductivley coupled plasma mass spectroscopy). This is more sensitive than OES methods but at 1,000 ppm (maximum allowable concentration of lead from RoHS) you are magnitudes above the limit of detection even when using OES methods.
harry 20th March 2007, 12:09 PM Just check the China RoHS documents and OES is also not among the recommended method. To the OP (Eusoof - if he still visits this thread) you can reject your supplier's result and demand that he produce one using RoHS recommended methods or one from an approved lab. (Bear in mind that Sony usually accept only SGS lab. reports over here)
A number of methods are recommended in RoHS documents - each being suitable under different conditions. To clear the confusion, I attached here a document on RoHS testing methods for those who are interested.
Eusoof 9th June 2007, 07:59 AM Thank you, Harry. You send the valuable info regarding this thread. For your info i have send this material and the result bellow 3500ppm but if the all material we test have same result, it's very costly for supplier and my company to bare the cost.
Refer the attachment for SGS RoHS Testing Procedure. I hope you all like it.
harry 9th June 2007, 08:13 AM Thank you, Harry. You send the valuable info regarding this thread. For your info i have send this material and the result bellow 3500ppm but if the all material we test have same result, it's very costly for supplier and my company to bare the cost.
Refer the attachment for SGS RoHS Testing Procedure. I hope you all like it.
Hi Eusoof
I understand the cost factor which is the complaint of most organizations. However, if you qualify as SMI (small medium industry - paid up capital less that RM 2.5 million and employees less than 150), you are entitled to government grants. If successful, the grant will pay for half the approved cost. You may contact SMIDEC for further information.
Thanks for the attachment also.
sfkevin 28th June 2007, 06:42 PM This post has been informative; I have an issue where our XRF test found 2,000 PPM of Lead (Pb) on the leads. The manufacture states there Inductively Coupled Plasma test only came up with 137 PPM.
When I ask for the data from the test along with the other elements I get this;
“This is the average concentration on the parts. I repeat the parts are in compliance with ROHS STD. The Analysis is now complete.”:frust:
I removed of the plating from the parts leads and found the leads passed but the material I removed had 1,500 PPM Pb. Now what, they will not take them back and the parts we feel still cannot be used.
It is frustrating not getting any follow up information from the testing party to use as validation if we used the part and there is an issue for our customer they and we could be in trouble.
harry 29th June 2007, 05:31 AM When I ask for the data from the test along with the other elements I get this; “This is the average concentration on the parts. I repeat the parts are in compliance with ROHS STD. The Analysis is now complete.”
The allowable concentration is express as ppm and is based on the unit weight of the component in question. What they are trying to tell you is that even though you detected a spot with high concentration but overall, the average concentration is much lower - and I think they are right about the method.
Having said that, I would like to investigate and find out why there are spots with such high concentration. You'll sleep better with that knowledge!
sfkevin 29th June 2007, 11:23 AM Having said that, I would like to investigate and find out why there are spots with such high concentration. You'll sleep better with that knowledge!:agree1:
I agree that the method they used was good, but I was hoping for the full report of elements found to compare to my findings to aid in determining why there was a difference.
I sampled ten parts that average the same value range of about 2,000 PPM. I sent them five of the parts I tested and they gave me an average of the five that does not add up.
Just because I stated the Pb value was high I also want to know what the other element values where but they will not give me the information.
I am now looking for the third party to do the test to validate one of the findings. I have been using the XRF for one year and this is the only finding I have not had confirmed by a manufacture.
harry 30th June 2007, 07:50 AM As a matter of interest,
1. Do you carry out the test on the outside surface only? Why not try to reach the inner part by filing or removing some surface material by any method and see what results you get.
2. Do you use certified reference materials (CRM) for reference/calibration of your instrument?
3. Have you ever validated your measurements with analytical testing?
Regards
sfkevin 2nd July 2007, 11:43 AM In response to your questions;
1. Yes, I only can examine the out layer of material with XRF unit, and I did remove the plating to verify the bare leads pass while the plating failed.
2. Yes, I have certified EC681 sample with low value elements that is part of the start up for the equipment each day.
3. The only validation I have had was when I rejected materials that where then re-inspected by the manufactures source. Out of five suspected items only one has not been confirmed, the one I used for this discussion.
Sgray 11th July 2007, 04:13 PM While your supplier does not seem to be very co-operative and apparently is not concerned about being your long term supplier they may very well be correct. Your XRF is only checking a very thin layer of the part which you stated is plated and may well be above the RoHS limits, but if they are digesting the entire part/unit and then checking that by ICP they could be getting a much lower concentration and this would be the unit concentration and pass RoHS. You stated you checked the plating and the leads without the plating, calculate the total Pb concentration based on your XRF results and weight of each component, if your within spec you can justify using the parts, otherwise I would send them out to an independent certified lab. Long term I would look for a more cooperative supplier.
sfkevin 11th July 2007, 04:26 PM We are small to this supplier but we have no choice since we are a contract manufacture and our customer has only this one supplier sourced.
They did use ICP where they dipped in an 8 molar Chloride acid solution in order to dissolve tin superficial layer with a pre and post weight to calculate the PPM. While my method does not use weight the obvious differences between the manually removed plating and raw leads shows there is a difference that still needs to be determining. We are going to a local third part for a test and will pass this information on to our end customer which ever way it may go for there records.
harry 11th July 2007, 11:27 PM We are small to this supplier but we have no choice since we are a contract manufacture and our customer has only this one supplier sourced.
They did use ICP where they dipped in an 8 molar Chloride acid solution in order to dissolve tin superficial layer with a pre and post weight to calculate the PPM. While my method does not use weight the obvious differences between the manually removed plating and raw leads shows there is a difference that still needs to be determining. We are going to a local third part for a test and will pass this information on to our end customer which ever way it may go for there records.
Hi Kevin
I think you are moving in the right direction. When dealing with RoHS, always remember the concept of 'due diligence (http://www.rohs.gov.uk/content.aspx?id=7)'. Simply put, if you have reasons to suspect an irregularity somewhere, actions must be taken to ensure that everybody's interest are protected.
Paul Simpson 12th July 2007, 05:59 AM The concept of due diligence is only (currently) applicable in UK law as the regulations (as implemented in the UK) are for absolute prohibition of supply of materials with these hazardous chemicals.
Hi Kevin
I think you are moving in the right direction. When dealing with RoHS, always remember the concept of 'due diligence (http://www.rohs.gov.uk/content.aspx?id=7)'. Simply put, if you have reasons to suspect an irregularity somewhere, actions must be taken to ensure that everybody's interest are protected.
If you are looking to apply a "due diligence" defence the onus is on the supplier to demonstrate they:
* have taken all reasonable steps or precautions and
* have exercised all due diligence to avoid committing the offence
Now "reasonable steps" and "due diligence" will be decided in the courts if your company is prosecuted.
harry 12th July 2007, 07:20 AM The concept of due diligence is only (currently) applicable in UK law as the regulations (as implemented in the UK) are for absolute prohibition of supply of materials with these hazardous chemicals.
If you are looking to apply a "due diligence" defence the onus is on the supplier to demonstrate they:
* have taken all reasonable steps or precautions and
* have exercised all due diligence to avoid committing the offence
Now "reasonable steps" and "due diligence" will be decided in the courts if your company is prosecuted.
You are right that this law is only applicable in UK but along the chain, key players are required to provide undertakings in black and white. So whether you are a parts provider in Asia or resin supplier in US, you will eventually be dragged along and perhaps share out any cost in fines/damages.
I think it's good practice to take 'reasonable steps' when in doubt. While I agree these are up to the courts to decide, you would have put yourself and your organization in a much better position by doing so.
sfkevin 12th July 2007, 11:12 AM Harry & Paul,
Thank you for your feed back :agree1: and you are correct. Our management has support me in regards to go further by having the third party review of the item. I as a quality person need to know if our process is good and if the material meets the requirements of my customer. The customer sates they must have RoHS material and the part manufacture states they have RoHS parts. So with the current information I scrap the material at our cost or verify one of us is wrong with our measurements. If am I wrong will that will lead to more validation of our process and suspect results of all past findings to assure our end customers have been receiving RoHS parts.
keung830 28th August 2007, 11:42 PM a little bit out of scope. pls. forgive me !!
Are all materials regarding the packaging purposed under EU directive. for example: plastic, metal, paper and silk screen logo...........etc?
If yes, what is the criteria?
sfkevin 29th August 2007, 11:35 AM :topic:
Keung
The main EU directives I have to look at are Directive 2002/96/EC of 27 January 2003 on waste electrical and electronic equipment (WEEE) and Directive 2002/95/EC of 27 January on the restriction of the use of certain hazardous substances in electrical and electronic equipment (RoHS).
These directives as you can tell from the titles do not directly deal with “packaging purposed under EU directive. for example: plastic, metal, paper”. I do not know of hand of any requirements for packaging materials waste.
Sorry
:cfingers:
fuhrmann 15th January 2008, 11:46 AM This post has been informative; I have an issue where our XRF test found 2,000 PPM of Lead (Pb) on the leads. The manufacture states there Inductively Coupled Plasma test only came up with 137 PPM.
...
I removed of the plating from the parts leads and found the leads passed but the material I removed had 1,500 PPM Pb. Now what, they will not take them back and the parts we feel still cannot be used.
It is frustrating not getting any follow up information from the testing party to use as validation if we used the part and there is an issue for our customer they and we could be in trouble.
The RoHS directives apply to each seperable (including grinding to seperate) part independantly.
The plating fails which makes the part fail, and anything that it is used in fail.
If they won't take them back, it is time for your purchasing department to let them know that they are no longer a supplier and that it may be necessary to get legal people involved.
fuhrmann 15th January 2008, 11:58 AM I'm curious how this turned out.
Since the customer specified the vendor, I would have contacted them to indicate that there is reason to believe that the parts were non-complient and that the vendor that they specified was not providing details to show their claim of compliance.
Under the British documents, which are not binding to anyone else but are the only ones that are useable, a certificate of compliance from a vendor does not constitute due dilligence unless you have also verified that they are reliable.
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