Is That Really bis (2-chloroisopropyl) ether: Potential Issues for EPA Methods 625 and 8270

you I’d like to welcome you all to specs line-up perhaps webinar is that really biz two chlorides Oh provo ether potential issues issues for EPA method 625 and eight 270 I’d like to introduce myself i’m amy williams i’m the marketing administrator for specs turner prep and i’ll be moderating the presentation today before we begin I’d like to only get a few housekeeping tips-off out of the highway everyone in attendance looked forward to receiving emails with the presentation slithers and links to the webinar recording on our YouTube channel if you’re going to questions during the presentation please type them in the question box on your screen and we’ll answer them during the Q& A period following the webinar now I’d like to introduce our presenters for today’s webinar symbol boat is the GCMs technical consultant for the ecs split of specs irda prep he has worked with GC and GC ms arrangements for over 30 years in his areas of expertise include epa 500 600 and 8000 sequences GC and GC ms programmes he structured environmental environmental consulting and supplies in 1991 which was acquired by specs in 2015 and Julian Burton is the director of organic manufacturing inspector to prep he is a PhD in chemistry from Rutgers and affiliate specs in 2012 and prior to joining us he was in R& D play-act instrument and perception algorithm design for trace detection organizations now I’d like to hand the presentation over to distinguish thanks for coming Amy welcome everyone the first thing you’re probably wondering is why would anyone want to hold a webinar on vis to chloro isopropyl ether it’s not the most glamorous of subjects but there is a problem ripening and needs to be addressed so the idea for this webinar followed to me several years ago when I was purchasing this new material and they notice the expenditure had gone up from three hundred dollars a gram to about three thousand dollars a gram so I started looking into why that was and I decided at some point to hold the webinar to not only address that issue but to likewise clarify some ambiguities that have been existing for this compound and its isomer 22 prime oxy biz one claw propane really since i started in mass spec 30 years ago so we’re going to address those problems those ambiguities and we’re also going to propose a solution to these problems then finally at the end we’re going to solicit input from the lab and too eventually to other standards providers but the intent of contacting the EPA so we can solve this problem okay now why is biz to chloro isopropyl ether important well it’s a target combination on epa technique 625 and 82 7 and it’s become an issue over the past few years because of the following number one there’s been widespread fluster among laboratories and both providers and on epa approaches as to the correct cas number specify and structure for this compound and its isomers number two as I mentioned earlier the cost has risen from $ 300 a gram to three thousand dollars per gram that overhead that will be passed on to the labs unless something can be done to bring down the cost and even more troublesome than the rising cost is that is frequently unavailable if you call the water it will regularly be backordered which threatens the capacities of suppliers to stimulate mingles that contain the spacecraft and then therefore jeopardizing the ability of the labs to obtain standards in the timely manner now the first thing is what what disorder exists on ETA method 625 8270 as well as on lab reporting documents and unser tificate civ analysis from suppliers one might seem either or both of the following isomers registered is to claw isopropyl ether and two to primary oxy biz one claw propane no these are two separate compounds with different designs and different CAS figures to use them interchangeably as if they’re the same compound is incorrect and that’s what we regularly consider people mix and accord CAS numbers they use them as if they’re the same compound but they’re really not at this level I will now turn the presentation over to Julie thank you buck here we investigate the two isomers on screen and the top isomer is the biz 2400 isopropyl ether “youre seeing” the shoot numbers of the two isomers there are very different as is typical with with this sort of comp and we’ve seen the difference between a change in a branched substance and in the best to acquire aiza properly that we have one carbon between up or another oxygen and in the other isomer we have two core two carbons between the chlorine in the oxygen so what does that planned when we actually run the sample with substances in it we discover both of these pigs they’re not resolved on a GCMs system that’s not peculiar like most isomers you would expect that they’re going to have similar physical characteristics most boiling points though I loop closely on on most articles that we would used for the analysis they have very similar mass spectra we are therefore see is that in most cases you see it’s over either one large-hearted top or flower with a shoulder it not really fully sparkler isolated on on most GC arrangements so what that conveys is that laboratories will typically integrate a total locality of work 45 and report the result desire the visit to claw isopropyl ether ether or two to pry Mopsy beers one for protein now what they should be doing is reporting a combined total of both of them and that’s one of the issues that we’ve identified horse all right let’s talk a little bit more about the cost and availability questions which is what really started me on this path when the toll proceeded from three hundred dollars a gram or five years ago to 500 hours a gram to a thousand dollars a gram to its current three thousand dollars a majestic premium I started asking why is this happening so I contacted domestic suppliers and suppliers abroad and we believe that the answer to that is that the process necessary to obtain the two isomer is to claw raisa propyl ether standard from the three isomers starting textile is quite costly so now I’ve innovated a new expression there’s a third isomer yes there’s a third isomer and that’s i believe the root of the problem apparently when us suppliers obtain this biz to claw isopropyl ether it actually contains a third isomer which has been saw and impure so service suppliers either now or abroad have to go through some extreme weighs apparently some complex fractional distillation procedure to remove ninety percent of this third isomer so let’s talk more about that third isomer data obtained by ecs scrutinizes with our in-house GCMs organizations in conjunction with information provided by s’appelle Co application note 18 would seem to indicate that the third isomer is biz 3 chloro propyl ether and the structure of vis 3 chloro propyl ether is indicated on the screen you notice that it has a separate CAS number from the other two isomers and that there are three carbons between the chlorine and the oxygen and the other two isomers are shown on the right side of the screen so you can see that they are three distinct isomers three separate compounds let’s take a look at the chromatography you with a tycoon on the top person is the two isomer standard that EC as in specs and virtually all suppliers have been used you noting that you attend two on our organisation we have a high resolution column we’re able to separate actually you see all three isomers you receive two sharp-witted heydays and then you encounter the third largest little shoulder on me right here that’s that’s the third isomer if you were to buy the three isomers standard that can not had the purification process you picture three distinct tops so in both illustrations the first two isomers are busy two chlorides of propylene thur and 22 prime oxy biz one claw propane I don’t know which isomers which for the purposes of this webinar it really doesn’t matter because as Julian said you’re going to integrate the combined neighbourhood and report it as a sum so you can see on the top chromatogram that third isomer is a very small blip on the shoulder of the second peak it’s only about 2.5 percent of the total area we’re on the bottom the unpurified three factor isomer the third isomers twenty-five percent of the total area and we know what the isomers are because we do a library rummage of both chromatograms it comes up with a ninety percentage match with is three chloro propyl ether in our n IST library so that conducted us to conclude that what’s happening is the raw material has the three isomers and suppliers are now going through a process to remove 90 plus percentage of that third isomer okay “were having” three isomers now what that as I “ve told you” the removing this third isomer so that parents three questions number one why are they doing this number two is this biz three chlorophyl either genuinely an pollution and three why not only equip the three isomer assortment and on the screen you can see that those of you familiar with the EPA methods 625 and 8270 will recognize this the mass spectrum there as the biz to Claire isopropyl ether and on the top screen you get a zoom and you can actually hear the the shoulder of the second peak which is that third eye so much better of which we’ve been pertaining okay so let’s answer those questions that I time announce why are they doing this in my opinion it’s just because it’s the inertia that has always existed in the industry I’ve been doing GCMs since 1985 this is when I started doing procedure 625 and on every EP a technique I’ve ever seen on every lab reporting certificate I’ve ever seen when I got into consulting I would go from lab to lab throughout the United Nation I would verify certificates of analysis from other suppliers the only two combinations I ever participated where biz to claw isopropyl ether and 22 prime ox ibas one claw propane there was no mention of their isomer know probably most of you probably didn’t even realize it existed until just now so it’s understandable that suppliers would continue along that course unless there was some motivation some reason to change namely eat the EPA changing UK 6 25 and 8270 methods given the lack of that it’s unlikely that there’s going to be any any mutate next question is the biz 3 chloro propyl either truly an pollutant well no it’s not an pollutant it’s a third isomer that would naturally appear if the other two isomers were currently if you would ever find it in a natural industrial test third question why not just furnish the three isomer and mixture well that’s what we think should be going on since the three I sarma mix in our opinion would represent what a laboratory might find if it had an industrial waste sample a real-world sample that they’re analyzing in their lab it seems logical that if information materials in the an environment has three isomers then the calibration standard too should have three isomers so why is the three isomers standard superior reservoir information materials itself is easier to synthesize it doesn’t expect quote-unquote purification because it doesn’t expect the purification it’s readily available at only three hundred dollars a gram not three thousand dollars of RAM and it doesn’t have availability issues because it doesn’t have to go through this fractional distillation process most importantly it best represents what the lab might see in a real-world sample so we’ve been using this two ingredient biz to Claire isopropyl ether for 30 -plus years in actuality they’ve been removing this third isomer which we now think that they should not have been doing we should have been using this three isomer standard all along so better late than never we’re feel you know I came to light only because the cost ran up so high-pitched but now we’re aware of it I think that we should originate some conversions now what about quantitation you might think to yourself okay what if we were to have this three component standard and we had a PT sample that he’ll exclusively had the two factor standard is available to would we be able to quantitate it accurately and get accurate PT outcomes well the answer is no there’s a difference in the responses between the two and three isomers standards and the two isomer mix I on 45 which is the qua non represents about thirty-nine percent of the total area in the three isomer mingle I on 45 represents only about thirty-five percent of the total area so that’s a 12 -percent built in error right there now the reason for that is because in that third isomer biz 3 chloro propyl ether I am 45 is abundance relative to the total i am from a chart is slightly less than it is in the other two isomers there’s more I on 41 that’s just the fragmentation pattern of that special complex is that you get more 41 and it comes out at the expense of ion 45 that induces this skewing in the quantitation so unless the ability ampules and the calibration standards are both of the same type you’re going to get a 12 -percent built-in air and that’s obviously not good this is why it’s important that the entire industry decide whether we want to stick with the two-component isomer mix or swap the three isomer assortment so where do we go from here well that really depends on the labs we don’t have the power to change the EPA methods exclusively the EPA does but what we really need is a consensus in the environmental industry in order to effect some kind of change so we want to contact other suppliers in the sector and eventually to the EPA with the hopes that they will change the methods and make it state unequivocally you should have a three isomers standard and you are able to some the entire area of I am 45 over those three isomers and report the some in order to do that we need to get some inputs on the labs first of all we presented our opinion on this this is none of this is a fact this is just our opinion that the three eyesore simulates would be superior now that you’ve heard our opinion we’d like to know your opinion you’ve been doing these methods for many years you are used to the two isomer mix do you agreed to accept us that we should the industry should switch the three a time combination or would you rather just stay with the two isomer mix so we’d like you to email us with your opinion on that the other thing I’m interested in is have you ever obtained any of the biz to claw isopropyl isomers in any test if you have you remember if you found one isomer two isomers are all three isomers just trying to get a feel for how rampant this complex is in nature so my email address is right there on the screen if you could please email me with your opinion and if you’ve ever feel these this deepen in any tests we’d applauded the fact okay I’ll turn this back over to Amy okay thank you very much mark and to Julian we do have a few questions that we’d like to to have answered now so I’ll question differentiate what do you plan to do with all the feedback we receive from the webinar alright what we plan to do is you know if there’s not a an overwhelming consensus among the labs then we probably won’t do very much however if the overwhelming consensus is that the labs you know think that the three isomer concoction is superior we then we’re going to start proceeding with this we’re going to contact other suppliers who make this mingle get opinion on it and if we get enough laboratories that are interested in change and fairly suppliers that are interested in change then we’re going to contact the EPA and try to get the method altered there any other compounds that has already been seen what similar concerns um well there are other complexes that are quite expensive some of the PAH neat textiles can be seven eight nine hundred dollars a gram but I don’t know of any complex on the EPA 500 or 600 8000 successions procedures that are anywhere near three thousand dollars a gram I’m also concerned that if something doesn’t happen that this these compounds could be four or five thousand dollars a gram in another couple times if they’re even available at all so to my knowledge this is the only compound where the premium has gone up you know drastically over the last three years and we’re availability has been a problem so I think it’s to restrict really this one compound does this compound have another name I the questions I cannot find it in that the drizzle ms 2011 library well when we get our rummage we actually learnt all three you go back to the slide here if you look on the bottom if I do if you do a background subtracted mass spectrum of the first peak you’ll it will be published either biz to claw raisa propyl either or two to primary oxy biz one claw propane if you do the mass spectra are so similar that if you do a mess library inquiry of the second peak you’ll come up with the same two results and if you do a library pursuit of the third peak you can’t really make love on the top one because it’s such a small peak but if you do it on the bottom one on the three-component mix if “youre supposed to” do a library scour of this one you would come up with a ninety percentage match of biz three chloro police or so I have the 98 k library and the system had no problem at all identifying all three isomers and we have another question when you say eight 270 what revision figure and time are you quoting um actually don’t have an answer for that I precisely yeah there’s so many revisions this is just the method this is just the standards that we’ve always used to my knowledge there’s been no changes in this compound in numerous revisions if anyone knows of any revisions of the EPA methods where this deepen is addressed we that would certainly factor into what’s going on now so you know please email us with that if to the best of my knowledge they they just list these complexes there’s no mention of the third isomer but if there is we’d like to know about it one more question or question as per your justification about the isomers I think that the EPA has to agree that the three isomers can be found in real samples not only one is that true well I been GCMs for 30 times and I can honestly say that at no laboratory that I ever work out or consultant for that I ever find this combination so it seems logical that if when it’s constructed you get the three isomers that if it were to show up in an industrial waste sample that you are able to picture three isomers but I have no direct know with it which is why i was asking for parties to tell us what have you find I’ve never seen any of these isomers in any sample I’m just saying what if it were to be present it seems most logical to me that you are able to envision all three isomers but I can’t say for sure I’m hoping that some of you will some of you who are in the lab will have seen this compound and I’ll trust what you tell me with regard to this sure what are typical spiking degrees for these methods normally anywhere from 50 to 100 ppb for ocean tests or 250 to 500 ppv for soil tests well thank you very much again to mark and Julian I’m going to be sending out the slithers for this presentation to everyone a little bit later today so you’ll be getting those by email and you also be coming a reproduce within a week or so of sound recordings of the presentation so we very much appreciate you attending this today and we look forward to seeing you at future webinars thank you

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