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May 18th, 2013, 4:38pm
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BOD sample super saturated (Read 670 times)
Plugbug
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BOD sample super saturated
Dec 28th, 2009, 4:36pm
 
You just knew it wouldn't take long to start a topic on the analysis we love to hate, BOD.
Any ideas on how to get a sample from super saturation to just saturation levels?  I've suggested; warming sample to room temp. and mixing gently to remove D.O.  How long would it take to lower the D.O. this way? The initial D.O. is still above 9.8mg/l.
Can one add a small amount of sodium sulfite solution to decrease the D.O.?  
What say you Perry?
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Re: BOD sample super saturated
Reply #1 - Dec 28th, 2009, 4:48pm
 
PlugBug:

You've already mentioned two ways of lowering DO and they are increasing temperature of sample to ambient temperature as well as gently mixing to release any dissolved oxygen.  A DO of 9.8 mg/L is unusual for typical wastewater unless the sample is extremely cold, not frozen, but cold--what was the temperature of the sample when DO was taken?  One thing that might artificially increase DO is peroxide being present in sample.  Any chance of industrial flow adding to DO?

Double check DO calibration?
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Re: BOD sample super saturated
Reply #2 - Dec 28th, 2009, 5:15pm
 
Thanks for the reply Victor, the facility is a zenon membrane style & treats only domestic waste from a plate glass manufacturing facility.  Samples are at 3 C when brought in to lab.  The lab tech is only there for a few hours in the morning, so it would be nice to adjust the D.O. quickly.  My reason for the sulfite comment.
Thanks again to recommend this forum, I'll hope to see you at the next class in Port Angeles!
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Re: BOD sample super saturated
Reply #3 - Dec 28th, 2009, 5:42pm
 
Plugbug:

I had to read SM to see how they addressed this issue.  I know that it was explicitly detailed but it has been years since I've done BOD's that I had to refresh my mind.  SM addresses the issue of samples supersatured with DO--"Samples containing more than 9 mg DO/L at 20°C may be encountered in cold waters or in water where photosynthesis occurs.  To prevent loss of oxygen during incubation of such samples, reduce DO to saturation at 20°C in partially filled bottle while agitating by vigorous shaking or by aerating with clean filtered compressed air." (SM 17th Edition).  Nowhere does it state that one can use sodium sulfite other than for dechlorination purposes so I would have to say that your idea would not be acceptable other than what SM states in terms of adjusting sample temperature and shaking dissolve oxygen out of sample.  Get the lab tech to put the cold sample in a large water bath (fill up the sink) and bring temperature to about ambient temperature--as close to 20°C as possible.
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Re: BOD sample super saturated
Reply #4 - Dec 28th, 2009, 5:45pm
 
Much obliged Victor, thanks.  I'll let her know what the options are.
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Re: BOD sample super saturated
Reply #5 - Dec 29th, 2009, 9:31am
 
All of our wastewater samples are cold when brought to the lab as they are refrigerated while being sampled. We run warm water into the sink and place the sample container, about 80 ml in a liter bottle, in the warm water. The sample is shaken vigorously and the temperature checked. When the sample is at 20 C we take the sample out of the warm water and shake vigorously. The DO will be about 8.8 to 9.0 at that point. The sample is ready for analysis.
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Re: BOD sample super saturated
Reply #6 - Dec 30th, 2009, 9:01am
 
You definitely do NOT want to treat with sodium sulfite to reduce the DO.  That will mess with the analysis during incubation.  You want to go with the warm water bath treatment.  Aliquot out the portion that you need to work with and then divide that futher into smaller amounts, say 100 mL or so.  I would use beakers to hold it.  You can then warm these smaller aliquots in your water bath.  The smaller volumes will equilibrate faster than one large chunk.  Make sure you aerate the sample after warming.  We typically fill a 300 mL BOD incubation bottle half way, put a stopper in it, and shake the dickens out of it.
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Re: BOD sample super saturated
Reply #7 - Jan 4th, 2010, 10:11am
 
Thanks for all the input, I tried warming the sample and it brought the D.O. to acceptable levels.  We will soon see how the BOD results turn out.  Thanks again folks!
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Re: BOD sample super saturated
Reply #8 - Mar 11th, 2010, 8:04am
 
Can't you cut the sample with a fraction of dilution water that you've boiled/cooled, such that the combined DO falls below 9?

This is what I used to do.
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Re: BOD sample super saturated
Reply #9 - Mar 11th, 2010, 8:25am
 
Thst does not aid in dealing with effluent samples where you need, say, 250 mls of effluent in a 300 ml bottle.  The temperature needs to be adjusted and also the D.O. of the sample without cutting it with anything else.  

~Eric
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Re: BOD sample super saturated
Reply #10 - Mar 11th, 2010, 5:06pm
 
In the case that the OP cited, sure it does.

Adding 50 ml of completely deoxygenated dilution water to a 250 ml sample with a DO of 10 mg/l would bring the aggregate DO down into the high eights.

It beats heating the sample. That seems awfully invasive.
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Re: BOD sample super saturated
Reply #11 - Mar 12th, 2010, 8:39am
 
Adding sulfite would not be acceptable as it adds to the BOD value as it is oxidized. To deoxidize dilution water you would need to heat up the dilution water to remove DO and then cool the sample as not to injure your seed bacteria while adding it to the sample.

The simplist method it to quickly warm the sample to 20 to 23 oC in hot water in the sink, mixing the samples by shaking, remove the sample at 23 oC and shaking vigorously until excess DO is gone.

This is more time consuming with large volumes of samples but you need only to warm effluent and stream samples that have low BOD values. Influent samples already have low DO.
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Re: BOD sample super saturated
Reply #12 - Mar 15th, 2010, 7:33am
 
One other point on adding an amount of oxygen deficient dilution water to your sample.  This goes against methodology for creating dilution water, for it states that the dilution water is to be saturated with dissolved oxygen.  Simply warm up the sample and shake out excess DO.  Departing from accepted methodology is more invasive than following said methodology.

~Eric
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Re: BOD sample super saturated
Reply #13 - Apr 27th, 2010, 2:23pm
 
Plugbug wrote on Jan 4th, 2010, 10:11am:
Thanks for all the input, I tried warming the sample and it brought the D.O. to acceptable levels.  We will soon see how the BOD results turn out.  Thanks again folks!


I like to think I mastered the BOD ....actually love running the dang test. I dealt with DO saturation years ago and through experimenting with time/temp/stirrer speed I've found that pouring 800mls effluent in a one liter beaker (initial temp - 3C, Initial DO 9.5 to 10ppm) place on stirring hotplate so that the vortex draws to near the bottom (vigorous stirring) of the beaker and hotplate pre-warmed to allow temp to reach 20C in approximately 7 minutes. When temp is reached continue stirring at same speed on a non-heated stirrer for a remaining 15-20 min. Whalla!!! D.O.'s at 20C will be 8.5 - 9.0 mg/l - you can work on other things while this is being prepped.
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Re: BOD sample super saturated
Reply #14 - Apr 27th, 2010, 2:36pm
 
Thanks Jmayou.
I really like your procedure, especially when you can set this up and multi-task.  I'll send it along. This forum & its participants are the best, thanks to all who share their knowledge!
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