Screening parameters in water analysis
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The document discusses the significance of water analysis, particularly focusing on the determination of organic pollutants using various methods such as Biological Oxygen Demand (BOD), Chemical Oxygen Demand (COD), and Total Organic Carbon (TOC). It presents the challenges associated with traditional analysis methods and highlights the advantages of TOC analysis as a faster and safer alternative. Additionally, it emphasizes the importance of water protection and innovative analytical technologies in environmental monitoring.
![TC
TC [total Carbon] = TIC [total inorganic carbon] + TOC [total organic carbon]
TOC = POC [purgable organic carbon] + NPOC [non-purgable organic carbon]
TOC + TIC
POC + NPOC
Elementar Webinar 2015
TOC](https://image.slidesharecdn.com/screeningparametersinwateranalysis-150803135506-lva1-app6892/85/Screening-parameters-in-water-analysis-14-320.jpg)
![TC [total Carbon]
Oxidation Detection
Sample [R-C-R + CO3
2-] + O2 CO2 + H2O +
...
Total carbon can be determined by oxidation and decomposition
of the sample and detection of the deriving CO2
Elementar Webinar 2015
How to determine TC](https://image.slidesharecdn.com/screeningparametersinwateranalysis-150803135506-lva1-app6892/85/Screening-parameters-in-water-analysis-15-320.jpg)
![NPOC [total Carbon]
Oxidation Detection
Acidified and purged Sample [R-C-R ]
Non-Purgable Organic Carbon can be determined by purging
the acidified sample in advance to remove TIC and POC,
oxidation of the remaining components and detection of the
deriving CO2
Oxidation:
R-C-R(non vol.) + O2 CO2 + H2O + ...
Purging:
[R-C-R (volatile and non volatile) + CO3
2-] + 3 H+ CO2 + H3O+ + R-C-R
(vol.)
if POC = 0
NPOC = TOC
Elementar Webinar 2015
How to determine NPOC](https://image.slidesharecdn.com/screeningparametersinwateranalysis-150803135506-lva1-app6892/85/Screening-parameters-in-water-analysis-17-320.jpg)
Screening parameters in water analysis
- 1. Screening parameters in water analysis 31.08.2015 Ralf Dunsbach Webinar
- 2. The elementargroup – About us Elementar Webinar 2015 • The technology leader in • Elemental Analysis (EA) • Isotope Ratio Mass Spectrometry (IRMS) • Offers an unmatched combination of • innovative technologies, • tailor-made solutions and • comprehensive support.
- 3. The elementargroup – Key Markets Elementar Webinar 2015 AgricultureChemicals EnvironmentalEnergy MaterialsForensics
- 4. Tailor-Made to Customer Needs • Elemental analyzer optimized for different analytical tasks • vario Series - Industry-leading versatility in elemental analysis • rapid Series - Dedicated instruments serving today’s customer needs • trace Series - Trace-level detection of elements • TOC Series - Fast and easy determination of total organic carbon Elementar Webinar 2015
- 5. Screening parameters in water analysis Elementar Webinar 2015 Water analysis The main focus within environmental analysis is the subject of water. Our instruments are used to carry out routine analysis of organic impurities in the water industry.
- 6. Introduction Elementar Webinar 2015 H2O Contains • Inorganic compounds (salts like NaCl) • Organic compounds (humic substances + man-made waste) Only 0,3% of the global water resources is availble as drinking water Water protection, technology and analysis gain more and more importance! One of the most important quality criteria for water is Pollution with organic compounds
- 7. How to determine organic pollutants Pollution with organic compounds - how to determine? Elementar Webinar 2015 Single compound analysis by chromatographic methods? Drawback: Nearly impossible due to the huge number of possible compounds – applicable only for certain classes of substances (e.g. polycyclic aromatic hydrocarbons) Screening parameter analysis for all organic compounds - BODx - biological oxygen demand - COD - chemical oxygen demand - TOC -total organic carbon
- 8. How to determine organic pollutants BODx and CSB are indirect methods to determine the amount of organic carbon by the determination of the biological and chemical oxygen demand during the decomposition of its compounds. Disadvantage: • slow • insufficient or wrong oxidation • depending from biological activity • heavy metal containing reagents • no automation Elementar Webinar 2015
- 9. BOD5 - biological oxygen demand after 5 days DIN 38 409 H51 DIN 38 409 H52 Disadvantage: particulates are not sufficiently oxidized slow (5 days) Elementar Webinar 2015 Reference: Fonds der chemischen Industrie - Umweltbereich Wasser BOD
- 10. DIN 38 409 H41 Disadvantage: higher or fluctuating results, if dichromate is consumed due to the oxidation of sulfur containing compounds Reagents: concentrated sulfuric acid H2SO4 – corrosive! potassium dichromate K2Cr2O7 - toxic! mercury substance (masking of chloride) – toxic! Analysis time: > 2 hours, automation very difficult Dichromate out of use in EU latest 2017!! Elementar Webinar 2015 Reference: Fonds der chemischen Industrie - Umweltbereich Wasser COD
- 11. Recovery rates COD According to Janicke (WaBoLu report 1/1983): n-hexane 2% Urea 82% Cyclohexane 5% benzene 63% Chloromethane 8% EDTA 78% Trimethylamine 1% starch 91% Nicotinic acid 12% stearic acid 60% Poor recovery for alcanes, amines Elementar Webinar 2015
- 12. False COD readings • High false readings by chlorides, bromides, iodides, certain sulfur compounds, nitrites and certain metal compounds • False low readings by chromium (VI)-compounds, nitrates, peroxides Elementar Webinar 2015
- 13. TOC EN 1484 - European Standard Water analysis - Guidlines for the determination of the total organic carbon (TOC) and dissolved organic carbon (DOC) The EN 1484 approves the determination of TOC and DOC as appropriate method to determine the contamination of water with organic compounds. Elementar Webinar 2015 R-C + O2 CO2 + H2O + further products
- 14. TC TC [total Carbon] = TIC [total inorganic carbon] + TOC [total organic carbon] TOC = POC [purgable organic carbon] + NPOC [non-purgable organic carbon] TOC + TIC POC + NPOC Elementar Webinar 2015 TOC
- 15. TC [total Carbon] Oxidation Detection Sample [R-C-R + CO3 2-] + O2 CO2 + H2O + ... Total carbon can be determined by oxidation and decomposition of the sample and detection of the deriving CO2 Elementar Webinar 2015 How to determine TC
- 16. Detection Acidified Sample: CO3 2- + 3 H+ CO2 + H3O+ TIC Total inorganic carbon can be determined by degradation of the carbonates by acid, purging and detection of the deriving CO2 Gas Elementar Webinar 2015 How to determine TIC
- 17. NPOC [total Carbon] Oxidation Detection Acidified and purged Sample [R-C-R ] Non-Purgable Organic Carbon can be determined by purging the acidified sample in advance to remove TIC and POC, oxidation of the remaining components and detection of the deriving CO2 Oxidation: R-C-R(non vol.) + O2 CO2 + H2O + ... Purging: [R-C-R (volatile and non volatile) + CO3 2-] + 3 H+ CO2 + H3O+ + R-C-R (vol.) if POC = 0 NPOC = TOC Elementar Webinar 2015 How to determine NPOC
- 18. Method Advantages Disadvantages Differential: TOC=TC - TIC includes volatile organic compounds Less suitable for high TIC concentrations (TOC << TIC) long measuring times Direct: NPOC Non-purgeable organic carbon = TOC in case no volatile compounds are present suitable for high TIC concentrations (TIC >> TOC) fast results Does not include volatile organic compounds if present in the sample Elementar Webinar 2015 How to determine TOC
- 19. EN 1484 - European Standard Elementar Webinar 2015 Determination of TOC and DOC by: • Wet chemical - UV-persulfat method (DOC only) • Combustion method How to determine TOC
- 20. How to determine TOC Elementar Webinar 2015 Wet chemical - UV-persulfat method Quelle: Deutschen Bundesstiftung Umwelt (DBU) R-C + O2 CO2 + H2O + further products UV-light + oxidation agent Advantage: • large sample volume (up to 20mL) • high sensitivity Disadvantage: • insufficient oxidation of particulates • not applicable for electrolytes or chlorine containing samples • not for highly contaminated samples • not for solid samples • not for nitrogen
- 21. Elementar Webinar 2015 Combustion method R-C + O2 CO2 + H2O + further products Advantage: • quantitative oxidation of all carbon containing compounds • low matrix influence • applicable for waste water and solids • applicable for TNb as additional parameter Disadvantage: • lower injection volume • problematically with salts • lower sensitivity High temperature in presence of catalyst How to determine TOC
- 22. State-of-the-art TOC analyzer Elementar Webinar 2015
- 23. The Concept Elementar Webinar 2015
- 24. Easy maintenance Elementar Webinar 2015 • Temperatur programmable up to 1100°C • Matrix separation (patent pending) to keep salt away from the catalyst • Multiway valve on top of the combustion tube for fast and easy injection • All maintenance parts easily accessible
- 25. Solids analysis Elementar Webinar 2015 • Only TOC in water analyzer worldwide with automatic sample feeder for solids • Sample feeding by reliable ball valve technique • Sample carousel with 80-120 positions • Solids expansion kit for carbon amounts up to 20mg C abs.
- 26. Drinking water: 0.5 ppm – 2 ppm TOC Surface waters: 0.5 ppm – 10 ppm TOC Waste waters: 5 ppm – 10,000 ppm TOC Waste and soil: upper ppm to percentage range of TOC Waters in pharmacy: 0.05 – 0.5 ppm TOC Waters in power plants: 0.05 – 1 ppm TOC Waters in semiconductor industries: 0.005 – 0.5 ppm TOC Elementar Webinar 2015 Typical TOC contents
- 27. Correlation TOC/COD Elementar Webinar 2015 Oxalic acid Ethanol Both compounds have the same TOC (in mol/l), but COD is 5* higher than oxalic acid.
- 28. COD/TOC of certain compounds Elementar Webinar 2015
- 29. COD/TOC in different samples I Origin COD/TOC SD Influent MWWTP <1000 r 3,23 0,42 Influent MWWTP 1000-5000 r 3,16 0,41 Influent MWWTP 5000-10000 r 2,99 0,37 Influent MWWTP 10000-100000 r 2,99 0,37 Influent MWWTP >100000 r 2,92 0,39 Edible oil refinery 3,64 0,70 Fish processing 3,51 0,45 Meat industry 3,26 0,41 Glue production 4,28 1,62 Elementar Webinar 2015 MWWTP: municipal waste water treatment plant
- 30. COD/TOC in different samples II Origin COD/TOC SD Ore processing 4,05 0,15 Sugar production 2,92 0,36 Paper production 2,75 0,18 Iron+steel production 3,78 1,02 Textile production 3,05 0,27 Glas and inorganic fiber production 2,62 0,25 Chemical cleaning 3,64 0,24 Waste deposit 3,04 0,2 Oil refineries 3,32 0,25 Elementar Webinar 2015 Source: Verbesserung der Einleiterüberwachung durch die Einführung der Meßgrößen TOC, TNb and Pges., Wasserwirtschaft Forschungsbericht 296-22-322
- 31. Summary • TOC analysis require minimum manpower • TOC can be measured within 4 minutes • The only chemicals required for TOC are diluted, non-oxidizing mineral acids • No special workbench (fume) required for TOC • Therefore: it needs some work to replace COD by TOC, but it‘s worth it! Elementar Webinar 2015Elementar Webinar 2015
- 32. Elementar thanks for your attention! Elementar Webinar 2015