1. New Method for Analysis of Total Nitrogen
Taylor Reynolds
Midwest Water Analysts Association Winter Expo
January 26, 2018

2. The life science business of Merck KGaA, Darmstadt, Germany operates as MilliporeSigma in the U.S. and Canada.
Total Nitrogen New Method For Analysis |

3. Taylor Reynolds Environmental & Energy Marketing MilliporeSigma
400 Summit Drive
Burlington, MA 01803
Mobile:  

4. Total Nitrogen
Agenda
Introduction - Merck KGaA – MilliporeSigma
Introduction - Speakers Contact Info
Total Nitrogen - A Little Background
Current Methods for Detecting Total Nitrogen
Merck KGaA Total Nitrogen Test Method Introduction
Multi-Lab Validation Study Results
Current Status with State Regulators
What to Do if Interested in this Method 03 04 05 06 08 12 22 23
Total Nitrogen New Method For Analysis |

5. Total Nitrogen Background
Total Nitrogen became a compound of concern as our understanding of Eutrophication has increased and the impact it has on our water sources
Mississippi Dead Zone and Chesapeake Bay were two of the major
Total Nitrogen Is NOT defined as an analyte in 40 CFR part 136
Total Nitrogen and its removal efficiency IS being defined by the states in NPDES permits
Historically, states have defined Total Nitrogen as:
TKN + Nitrite + Nitrate
Source: developing-numeric-nutrient-water-quality-criteria 5
Total Nitrogen New Method For Analysis |

6. Currently Available Test Methods
Total Nitrogen
Currently Available Test Methods
Summation Determination
TKN + Nitrite + Nitrate
Lengthy
Generates substantial Waste
Hazardous
Summation of values is also summation of error
All tests have a +/- accuracy
Different methods can give different results
State of Iowa concerned by potential for false high or low reporting
Chemiluminescence
New to the market
Requires additional / specialized equipment
Requires Platinum Catalyst
Reports ALL Mineral Species. Even those that are not detected in NORMAL WASTEWATER EFFLUENT.
Total Nitrogen New Method For Analysis |

7. Problems with Current Analyses
Total Nitrogen
Problems with Current Analyses
Final Wastewater Effluent Standard Methods Summation Process
vs. MilliporeSigma TN
Nitrate
Nitrite
NH3
TKN
Total Nitrogen
19.7
<0.10
2.10
25.4
Summation = 21.8 mg/L SM 4500-N D = mg/L
Difference = 3.6 mg/L ~ 17 % Difference
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8. Our Solution – One Test, One Result
Total Nitrogen
Our Solution – One Test, One Result
Utilizes
16mm round Digestion Tubes
COD Type Heating Block
Simple Spectrophotometer
Benefits
Shorter digestion step
Reduced waste
Much safer compared to TKN
Eliminates uncertainty associated with adding multiple tests 8
Total Nitrogen New Method For Analysis |

9. Total Nitrogen Koroleff Reaction
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10. Nitrate Determination By Spectroscopy
Total Nitrogen
Nitrate Determination By Spectroscopy
Total Nitrogen New Method For Analysis |

11. Compounds In Mixed Standard
Total Nitrogen
Compounds In Mixed Standard
Ammonium
Glycine
Nitrite
Nicotinic Acid
Nitrate
EDTA
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12. Multi-LAb VAlidation study

13. Total Nitrogen ERA Blind Checks
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14. Total Nitrogen LFB Recoveries
Total Nitrogen New Method For Analysis |

15. Total Nitrogen MDL Spike
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16. Total Nitrogen MDL Blank
Total Nitrogen New Method For Analysis |

17. Final Effluent Matrix Recovery
Total Nitrogen
Final Effluent Matrix Recovery
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18. Other Matrixes Recoveries
Total Nitrogen
Other Matrixes Recoveries
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19. ~ 8 % Needed To Reach 80% Removal
Total Nitrogen
Removal Efficiency
City of Muscatine POTW
Influent mg/L TN-N
Primary Effluent mg/L TN-N
Final Effluent mg/L TN-N
Total Nitrogen Removal
= mg/L TN-N
72.3 % Removal
~ 8 % Needed To Reach 80% Removal
Total Nitrogen New Method For Analysis |

20. Other Total Nitrogen Result Uses for Wastewater Plants
Develop Waste Load Allocations for Industrial Dischargers to the Sewer System
Assess Waste Load Charges to Industrial Dischargers to the Sewer System
Set Up CMOM for Wastewater Collection System
Set Up Process Control for Wastewater Plant
Total Nitrogen New Method For Analysis |

21. Conclusion

22. Total Nitrogen Status with States
State of Utah has already approved this method
State of Iowa sponsored this study and currently evaluating the results of the test
MilliporeSigma is reaching out to as many other states as possible
Finding the right person is a challenge
Not all states concerned with TN
Not all states have a formalized structure to approve of new methods
Submitting the results of validation study when able to and responding to questions from regulators
Total Nitrogen New Method For Analysis |

23. What should you do if you’d like to evaluate this new method?
Total Nitrogen
What should you do if you’d like to evaluate this new method?
If in North America, contact Taylor Reynolds, he will:
Provide contact info for your assigned sales rep
Help coordinate on-site demonstrations
Help coordinate with your state contacts to get approval for the method
Answer technical questions
If outside of North America:
Contact your local Merck KGaA sales rep to get more information
If you can’t find your local rep, contact Taylor Reynolds, he will assist in finding them
Total Nitrogen New Method For Analysis |

24. Questions?