Application Bulletin
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1 Application Bulletin Of interest to: General analytical laboratories; Water analysis A B E G I K 1, 2, 7 Standard methods in water analysis use of Metrohm instruments Summary This bulletin gives a survey of standard methods from the field of water analysis. You will also find the analytical instruments required for the respective determinations and references to the corresponding Metrohm Application Bulletins and Application Notes. The following parameters are dealt with: electrical conductivity, ph value, fluoride, ammonium and Kjeldahl nitrogen, anions and cations by means of ion chromatography, heavy metals and NTA/EDTA by means of voltammetry, chemical oxygen demand (COD), water hardness, free chlorine as well as a few other water components. Abbreviations AOAC Official Methods of Analysis of the Association of Official Analytical Chemists (USA) ASTM American Society for Testing and Materials Schweizerisches Lebensmittelbuch Schweizer Methoden für Lebensmittelund verwandte Analysen EPA United States Environmental Protection Agency DIN Deutscher Normenausschuss ISO International Organization for Standardization ISWS Illinois State Water Survey USP United States Pharmacopoeia 1. Electrical conductivity AOAC (1990) Specific conductance of water. 2.3 Bestimmung der spezifischen elektrischen Leitfähigkeit. EPA (1983) Conductance (Specific conductance, µmhos at 25 C). DIN Teil 8 (1982) Physikalische und physikalisch-chemische Kenngrössen. Bestimmung der elektrischen Leitfähigkeit.
2 Standard methods in water analysis Page 2 ISO 7888: 1985 Water quality Determination of electrical conductivity. USP (645) Water conductivity. 712 Conductometer with conductivity measuring cell conductivity standard: c(kcl) = mol/l Metrohm Application Bulletin No ph value AOAC (1990) ph of water. 2.2 Bestimmung des ph-wertes. DIN Teil 5 (1983) Physikalische und physikalisch-chemische Kenngrössen. Bestimmung des ph- Wertes. EPA (1983) ph (Electrometric). ISO 10523: 1994 Water quality Determination of ph. 691, 704, 713 or 744 ph Meter combined LL double-junction ph glass electrode or LL Porotrode or combined LL ph glass electrode with electrode cable buffer set: 50 ml each concentrate ph = 4.00, ph = 7.00, c(kcl) = 3 mol/l Metrohm Application Bulletin No Fluoride ASTM D 1179-A Fluoride Ion in Water using Distillation. ASTM D 1179-B Fluoride Ion in Water using ISE. ASTM D 3868 Fluoride Ions in Saline Water.
3 Standard methods in water analysis Page Bestimmung von Fluorid, Potentiometrie. DIN Teil 1 (1982) Bestimmung des Fluoridions mittels Fluorid-ionensensitiver Elektrode. EPA (1983) Fluoride (Potentiometric, ion-selective electrode). ISO : 1992 Water quality Determination of fluoride Part 1: Electrochemical probe method for potable and lightly polluted water. 692 ph/ion Meter with Magnetic Stirrer 776 Dosimat including Exchange Unit, with cable for automatic standard additions ion-selective fluoride electrode with electrode cable LL Ag/AgCl reference electrode with electrode cable NaF ion standard: c(naf) = mol/l electrolyte solution: c(kcl) = 3 mol/l Metrohm Application Bulletin No Ammonium and Kjeldahl nitrogen EPA (1983) Nitrogen, Ammonia (Colorimetric, titrimetric, potentiometric - distillation procedure). EPA (1983) Nitrogen, Ammonia (Potentiometric, ion-selective electrode). EPA (1983) Nitrogen, Kjeldahl, Total (Colorimetric, titrimetric, potentiometric). EPA (1983) Nitrogen, Kjeldahl, Total (Potentiometric, ion-selective electrode). ISO 6778: 1984 Water quality Determination of ammonium Potentiometric method. 692 ph/ion Meter with Magentic Stirrer 776 Dosimat including Exchange Unit, with cable for automatic standard additions NH 3 selective electrode Metrohm Application Bulletin No. 133
4 Standard methods in water analysis Page 4 and/or 702 SET/MET Titrino, 716 DMS Titrino, 719 SET Titrino, 736 GP Titrino, 751 GPD Titrino or 785 DMP Titrino with Magnetic Stirrer and Exchange Unit combined LL ph glass electrode with electrode cable Metrohm Application Bulletin No Anions and cations by means of ion chromatography ASTM D (1997) Standard Test Method for Anions in Water by Chemically Suppressed Ion Chromatography. ASTM D (1995) Standard Test Method for Determination of Chloride, Nitrate and Sulfate in Atmospheric Wet Deposition by Chemically Suppressed Ion chromatography. ASTM D (1994) Standard Test Method for Trace Anions in High Purity Water by Ion Chromatography. ASTM D (1996) Standard Test Method for Measuring Anionic Contaminants in High Purity Water by On-Line Ion Chromatography. AOAC Inorganic Anions in Water. 4.4 Chlorid, Nitrat, Sulfat mittels Ionenchromatographie (1988). DIN Teil 19 (1988) Anionen. Bestimmung der Anionen Fluorid, Chlorid, Nitrit, Orthophosphat, Bromid, Nitrat und Sulfat in wenig belasteten Wässern mit der Ionenchromatographie. DIN Teil 20 (1989) Anionen. Bestimmung der gelösten Anionen Bromid, Chlorid, Nitrat, Nitrit, Phosphat (ortho) und Sulfat in Abwasser mit der Ionenchromatographie. EPA The determination of inorganic anions in water by ion chromatography. ISO 276: 1993 Water quality Determination of dissolved chlorate, chloride and chlorite by liquid chromatography of ions - Part 4: Method for water of low contamination ISO : 1992 Water quality Determination of dissolved fluoride, chloride, nitrite, orthophosphate, bromide, nitrate and sulfate ions using liquid chromatography of ions Part 1: Method for water with low contamination. ISO : 1995 Water quality Determination of dissolved anions by liquid chromatography of ions Part 2: Determination of bromide, chloride, nitrate, nitrite, orthophosphate and sulfate in waste water.
5 Standard methods in water analysis Page 5 ISO : 1997 Water quality Determination of dissolved anions by liquid chromatography of ions Part 3: Determination of chromate, iodide, sulfite, thiocyanate and thiosulfate. ISO : 1997 Water quality Determination of dissolved anions by liquid chromatography of ions Part 4: Determination of chlorate, chloride and chlorite in water with low contamination. ISO 14911: 1998 Water quality Determination of dissolved Li, Na, ammonium, K, Mn(II), Ca, Mg, Sr and Ba using ion chromatography Method for water and waste water. ISWS (1986) Chloride, orthophosphate, nitrate and sulfate in wet deposition by ion chromatography. ISWS (1986) Dissolved sodium, ammonium, potassium, magnesium and calcium by ion chromatography Compact IC with Metrohm Suppressor Module MSM or X10 IC Detector X30 IC Separation Center with Metrohm Suppressor Module MSM X10 IC Pump 752 IC Pump Unit Pulsation dampener X0 IC Interface including Metrodata IC-Net 2.0 software Possibly 791 VA Detector with mini carbon paste electrode (for the electrochemical detection of nitrite traces) Possibly 766 IC Sample Processor Recommended IC separation columns: For the determination of anions: Metrosep Anion Dual 1, possibly preconcentration cartridge For the determination of cations: Metrosep Cation 1-2, possibly precolumn cartridge Different Metrohm Application Bulletins and Application Notes
6 Standard methods in water analysis Page 6 6. Polarographic/voltammetric determinations ASTM D (1995) Standard Test Methods for Cadmium in Water. ASTM D (1996) Standard Test Methods for Lead in Water. Polarographische Bestimmung von Kupfer, Blei, Cadmium und Zink. DIN Part 16 (1990) Determination of 7 metals by voltammetric methods ( Zn, Cd, Pb, Cu, Tl, Ni, Co). Water analysis. DIN Teil 5 (1990) Einzelkomponenten. Bestimmung von Ethylendinitrilotetraessigsäure (EDTA) und Nitrilotriessigsäure (NTA) mittels Polarographie. EPA 7063 (1996) Arsenic in aqueous samples and extracts by anodic stripping voltammetry (ASV). EPA 7472 (1996) Mercury in aqueous samples and extracts by anodic stripping voltammetry (ASV). 757 VA Computrace or 746 VA Trace Analyzer with 747 VA Stand Possibly 705 UV Digester Different Metrohm Application Bulletins and Application Notes 7. Chemical oxygen demand (COD) EPA (1983) Chemical Oxygen Demand (Titrimetric, mid-level). EPA (1983) Chemical Oxygen Demand (Titrimetric, low-level). EPA (1983) Chemical Oxygen Demand (Titrimetric, high-level for saline waters). ISO 6010: 1989 Water quality. Determination of the Chemical Oxygen Demand.
7 Standard methods in water analysis Page SET/MET Titrino, 716 DMS Titrino, 736 GP Titrino, 751 GPD Titrino or 785 DMP Titrino or 726 or 796 Titroprocessor 730 Sample Changer As far as additional accessories are concerned, please ask for an offer. Metrohm Application Bulletin No Water hardness ASTM 314 (1985) Hardness (water hardness). ASTM D (1998) Standard Test Methods for Calcium and Magnesium in water. 6.1 Bestimmung der Gesamthärte; 6.2 Säureverbrauch bis ph = 4,3 bzw. 8,2. DIN Teil 3 (1982) Kationen (Gruppe E). Bestimmung von Calcium und Magnesium. EPA (1983) Hardness, total (mg/l as CaCO 3 ). Titrimetric, EDTA. EPA (1983) Acidity (Titrimetric). EPA (1983) Alkalinity (Titrimetric, ph = 4.5). ISO 6058: 1984 Water quality Determination of calcium content EDTA titrimetric method. ISO 6059: 1984 Water quality Determination of the sum of calcium and magnesium EDTA titrimetric method. 702 SET/MET Titrino, 716 DMS Titrino, 736 GP Titrino, 751 GPD Titrino or 785 DMP Titrino or 726 or 796 Titroprocessor Possibly 730 Sample Changer combined LL double-junction ph glass electrode or LL Porotrode ion-selective calcium electrode with double-juction Ag/AgCl reference electrode Possibly X Spectrode 610 nm As far as additional accessories are concerned, please ask for an offer. Metrohm Application Bulletins No. 125 and 178 Metrohm Application Notes T-52 and T-57
8 Standard methods in water analysis Page 8 9. Free chlorine EPA (1983) Chlorine, total residual (Titrimetric, amperometric). EPA (1983) Chlorine, total residual (Titrimetric, back, iodometric). EPA (1983) Chlorine, total residual (Titrimetric, iodometric). 702 SET/MET Titrino, 716 DMS Titrino, 736 GP Titrino, 751 GPD Titrino or 785 DMP Titrino or 726 or 796 Titroprocessor Depending on the choosen method double Pt wire electrode or Pt Titrode Metrohm Application Bulletin No. 249 Additional literature: E. Barbolani, G. Piccardi, F. Pantani Potentiometric titration of chlorine and its oxy compounds in water Anal. Chim. Acta 132 (1981) G. Gordon, W. J. Cooper, R. G. Rice, G. E. Pacey Methods of measuring disinfectant residuals J. AWWA (1988) Other titrimetric determinations (bromide, chloride, sulfate, sulfide) EPA (1983) Bromide (Titrimetric). EPA (1983) Chloride (Titrimetric). EPA (1983) Sulfide (Titrimetric). 702 SET/MET Titrino, 716 DMS Titrino, 736 GP Titrino, 751 GPD Titrino or 785 DMP Titrino or 726 or 796 Titroprocessor Ag Titrode with Ag 2 S coating X Spectrode 525 nm Metrohm Application Bulletins No. 25, 130 and 178 Metrohm Application Notes T-1, T-7, T-32 and T-53
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