Having carryover issues with selenium and molybdenum (7900)

I run a 7800 doing EPA 200.8 MET and 6020B methods. Recently, we've had an instrument serviced and have been seeing Mo and Se carryover into ICB and CCBs at levels > ½RL. 

Here are the things I've tried to address this:

  • Loaded an old batch and tune from before the PM
  • Replaced the nebulizer
  • Cleaned the rotary valve
  • Replaced the spray chamber
  • Cleaned the torch
  • Replaced cones
  • Dramatically increased rinse time by a minute 

So far, no luck. I'm suspecting it's something in the software, like some tune settings or something like that. 

Does anyone have any ideas on what it could be?

Update: 

After doing some research I've come to the conclusion that the issue is the switching valve. When it switches over to "inject" the Mo comes through. It seems the inside isn't being cleaned well enough to. 

  • Replaced both the stator and rotor
  • Cleaned the heck out of the valve

No matter how long I have my rinses (within reason) it still carries over. 

Parents
  • Do you rinse with HCl?  Mo, Sb, Se, Hg, Ag, Al can get "hung up" in the capillary.  Rinsing using a mixture of nitric and HCl will help remove those.  With 200.8, you will want to run a nitric only rinse after the nitric/HCl mix will clear out the Chloride to minimize interferences.  Be careful how long and at what concentration you add the HCl.  The standard Ni sample cone does not stand up well against HCl >0.5%.  For that much HCl we suggest using the Ni plated sample cone.  Typically to clean stubborn elements, 2%nitric with 2%HCl will do it.  It just depends on how high they are in solution to be cleaned out. You could try a short rinse in 2%nitric with 0.5%HCl for 10-15 seconds before going to your Nitric rinse for the time you have it set now.  Play with the timing of the two rinses to remove the Mo and Se without getting interference on As, Se and V from Cl-.

    Are you using Preemptive Rinse in your Batch?  This can help minimize the time the high concentration sample is in the line.

Reply
  • Do you rinse with HCl?  Mo, Sb, Se, Hg, Ag, Al can get "hung up" in the capillary.  Rinsing using a mixture of nitric and HCl will help remove those.  With 200.8, you will want to run a nitric only rinse after the nitric/HCl mix will clear out the Chloride to minimize interferences.  Be careful how long and at what concentration you add the HCl.  The standard Ni sample cone does not stand up well against HCl >0.5%.  For that much HCl we suggest using the Ni plated sample cone.  Typically to clean stubborn elements, 2%nitric with 2%HCl will do it.  It just depends on how high they are in solution to be cleaned out. You could try a short rinse in 2%nitric with 0.5%HCl for 10-15 seconds before going to your Nitric rinse for the time you have it set now.  Play with the timing of the two rinses to remove the Mo and Se without getting interference on As, Se and V from Cl-.

    Are you using Preemptive Rinse in your Batch?  This can help minimize the time the high concentration sample is in the line.

Children
  • > Do you rinse with HCl? 

    Yes, the rinses are as follows:

    The rinse port and vials 1 and 2 are both 2% nitric 1% HCl. Rinse vial 3 is 4% nitric 2% HCl. I've been running it this way for ages and haven't had any interference issues until lately but I suppose I could try changing out Rinse 3 for only 2% HNO3 and adjusting the timings and post run so it's flushing the loop and spray chamber with that. 

    >The standard Ni sample cone does not stand up well against HCl >0.5%.  For that much HCl we suggest using the Ni plated sample cone. 

    Yep, that's what we use

    >You could try a short rinse in 2%nitric with 0.5%HCl for 10-15 seconds before going to your Nitric rinse for the time you have it set now.  Play with the timing of the two rinses to remove the Mo and Se without getting interference on As, Se and V from Cl-.

    So what I'm hearing here is that I should be rinsing with only HNO3, with maybe a short rinse of HCl early on that gets washed out by a later HNO3 rinse. 

  • HCl is to help move along the "sticky" elements like Mo, and some others. The HNO3 only at the end of things is to get rid of the Cl- as you can't use gas mode for 200.8 Drinking Water analysis.  As, Se, V have Cl- interferences in no-gas.

    I see from the program you are using an ISIS, have you pulled that off and cleaned the valve head and rotor seal?  With the valve off, and all connections removed, I spray soap solution through the openings for all the ports to clean them out.  Then spray DI through them to rinse out the soap.  For the rotor seal, make sure there is no material in the small channels of the face.  Clean with a cotton tip swab and some DI.

  • >you can't use gas mode for 200.8 Drinking Water analysis. 

    A point of clarification: We're doing 200.8 MET, so we have gas.

    >have you pulled that off and cleaned the valve head and rotor seal? 

    Yeah, I've cleaned that out. There was no change

  • After doing some research I've come to the conclusion that the issue is the switching valve. When it switches over to "inject" the Mo comes through. It seems the inside isn't being cleaned well enough to. 

    I've replaced both the stator and rotor and cleaned the heck out of the valve. No matter how long I have my rinses (within reason) it still carries over. 

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