Standard Methods and EPA Comparison Tables

1 Askew Scientific Consulting LLC Page 1 Standard Methods and EPA Comparison Tables Edward F. Askew PhD. Askew Scientific Consulting Technical Director Askew Scientific Consulting LLC Page 2 Contents 40 CFR (2) table (7-1-03 Edition) ..3 Water Methods Comparison table ..4 table II Method Update Rule ..6 table II MUR-End Notes ..8 CWA Comparison table EPA MUR to Standard Methods 21st Edition ..13 Standard Methods 21st Edition Sample Preservation and Storage Comparison to the MUR table IIA ..17 Comparison of Standard Methods for the Examination of Water and Wastewater Editions, Part 1000 ..22 Use of this document in part or in entirety requires the express permission of Askew Scientific Consulting LLC, 2952 155th street, Muscatine, Iowa 52761.

2 40 CFR (2) table (7-1-03 Edition) Contaminant Preservative (1) Container (2) Time (3) Antimony HNO3 P or G 6 months Arsenic Conc HNO3 to pH <2 P or G 6 months Asbestos 4 C P or G 48 hours 4 Barium HNO3 P or G 6 Months Beryllium HNO3 P or G 6 Months Cadmium HNO3 P or G 6 Months Chromium HNO3 P or G 6 Months Cyanide 4 C, NaOH P or G 14 days Fluoride None P or G 1 month Mercury HNO3 P or G 28 days Nickel HNO3 P or G 6 Months Nitrate 4 C P or G 48 hours 5 Nitrate-Nitrite 6 H2SO4 P or G 28 days Nitrite 4 C P or G 48 hours Selenium HNO3 P or G 6 Months Thallium HNO3 P or G 6 Months 1.

3 For cyanide determinations samples must be adjusted with sodium hydroxide to pH 12 at the time off collection. When chilling is indicated the sample must be shipped and stored at 4 C or less. Acidification of nitrate or metals samples may be with a concentrated acid or a dilute (50% by volume) solution of the applicable concentrated acid..Acidification of samples for metals analysis is encouraged and allowed at the laboratory rather than at the time of sampling provided the shipping time and other instructions in Section 83 of EPA Methods or or are followed. 2. P=plastic, hard or soft; G=glass, hard or soft. 3. In all cases samples should be analyzed as soon after collection as possible. Follow additional (if any) information on preservation, containers or holding times that is specified in method.

4 4. Instructions for containers, preservation procedures and holding times as specified in Method must be adhered to for all compliance analyses including those conducted with Method 5. If the sample is chlorinated, the holding time for an unacidified sample kept at 4 C is extended to 14 days. 6. Nitrate-Nitrite refers to a measurement of total nitrate. Page 3 Askew Scientific Consulting LLC Askew Scientific Consulting LLC Page 4 Water Methods Comparison table Water Certification Manual, table IV-6 5th Edition, 2005 Standard Method table 1060, 21st Edition MUR table 2 2007 Parameter/ Method Preservative Sample Holding TimePreservative Sample Holding Time Preservative Sample Holding TimeMetals (except Hg) HNO3 pH<2 6 months For dissolved metals filter immediately, add HNO3 to pH < 2 6 months HNO3 to pH<2 or at least 24 hours prior to analysis, 6 months Mercury HNO3 pH<2 28 days Add HNO3 to pH < 2, 4 C, refrigerate 28 days CVAA: HNO3 to pH<2 CVAFS.

5 5 ml/L 12N HCL or 5 ml/ L BrCl 28 days 90 days Alkalinity Cool, 4C 14 days Refrigerate 24 h Cool 6 C 14 days Asbestos Cool, 4C 48 hours NA NA NA NA Chloride none 28 days None required NS None required 28 days Residual Disinfectant none immediately Analyze immediately 025 Hours None required Analyze within 15 minutes Color Cool, 4C 48 hours Refrigerate 48 hours Cool 6 C 48 hours Conductivity Cool, 4C 28 days Refrigerate 28 days Cool 6 C 28 days Cyanide Cool, 4C, Ascorbic acid (if chlorinated), NaOH pH>12 14 days Add NaOH to pH >12, refrigerate in dark If sample is chlorinated, see text for pretreatment 24 hours Cool 6 C, NaOH to pH>12, reducing agent 14 days Fluoride none 1 month None required 28 days None required 28 days Foaming Agents Cool, 4C 48 hours NA NA Cool 6 C 48 Hours Nitrate (chlorinated) Cool, 4C non-acidified 14 days Analyze as soon as possible; refrigerate At least 14 days Cool 6 C 48 hours Nitrate (non chlorinated) Cool, 4C, non-acidified 48 hours Analyze as soon as possible; refrigerate 48 hours Nitrite Cool, 4C 48 hours Analyze as soon as possible.

6 Refrigerate None Cool 6 C 48 hours Askew Scientific Consulting LLC Page 5 Water Methods Comparison table Water Certification Manual, table IV-6 5th Edition, 2005 Standard Method table 1060, 21st Edition MUR table 2 2007 Parameter/ Method Preservative Sample Holding TimePreservative Sample Holding Time Preservative Sample Holding TimeNitrate+ Nitrite H2SO4 pH<2 28 days Add H2SO4 to pH <2, refrigerate 1-2 days Cool 6 C H2SO4 to pH<2 28 days Odor Cool, 4C 24 hours Analyze as soon as possible; refrigerate 6 Hours NA NA pH none immediately Analyze immediately 025 Hours None required Analyze within 15 minutes o-Phosphate Cool, 4C 48 hours For dissolved phosphate filter immediately.

7 Refrigerate 48 hours Cool 6 C Filter within 15 minutes Analyze within 48 hours Silica Cool, 4C 28 days Refrigerate, do not freeze 28 days Cool 6 C 28 days Solids (TDS) Cool, 4C 7 days Refrigerate 7 Days Cool 6 C 7 days Sulfate Cool, 4C 28 days Refrigerate 28 days Cool 6 C 28 days Temperature none immediately Analyze immediately 025 hours None required Analyze Turbidity Cool, 4C 48 hours Analyze same day; store in dark up to 24 h, refrigerate 24 hours Cool 6 C 48 Hours See citation10 for possible differences regarding container and preservation requirements NS = not stated in cited reference; stat = no storage allowed; analyze immediately. Citation 10 US ENVIRONMENTAL PROTECTION AGENCY 1992 Rules and Regulations 40 CFR Parts 100-149.

8 Askew Scientific Consulting LLC Page 6 table II Method Update Rule Parameter number/name Container 1 Preservation 2,3 Maximum holding time 4 table Tests: 1. Acidity P, FP, G Cool 6 C 18 14 days 2. Alkalinity P, FP, G Cool 6 C 18 14 days 4. Ammonia P, FP, G Cool 6 C 18, H2SO4 to pH<2.

9 28 days 9. Biochemical oxygen demand P, FP, G Cool 6 C 18 48 hours 10. Boron P, FP, or Quartz HNO3 to pH<2 6 months 11. Bromide P, FP, G None required 28 days 14. Biochemical oxygen demand, carbonaceous P, FP G Cool 6 C 18 48 hours 15. Chemical oxygen demand P, FP, G Cool 6 C 18, H2SO4 to pH<2. 28 days 16. Chloride . P, FP, G None required 28 days 17. Chlorine, total residual P, G None required Analyze within 15 minutes 21. Color P, FP, G Cool 6 C 18 48 hours Cyanide, total or available (or CATC) P, FP, G Cool 6 C 18, NaOH to pH>12 6, reducing agent 5.

10 14 days 25. Fluoride P None required 28 days 27. Hardness P, FP, G HNO3 or H2SO4 to pH<2. 6 months 28. Hydrogen ion (pH) P, FP, G None required Analyze within 15 minutes 31, 43. Kjeldahl and organic N P, FP, G Cool 6 C 18, H2SO4 to pH<2. 28 days table : 7 18. Chromium VI P, FP, G Cool 6 C 18, pH = 20. 28 days 35. Mercury (CVAA) P, FP, G HNO to pH<2 28 days 35. Mercury (CVAFS) FP, G; and FP-lined cap 17. 5 mL/L 12N HCl or 5 mL/ L BrCl 17. 90 days 17 3, 5 8, 12, 13, 19, 20, 22, 26, 29, 30, 32 34, 36, 37, 45, 47, 51, 52, 58 60, 62, 63, 70 72, 74, 75. Metals, except boron, chromium VI, and mercury. P, FP, G HNO3 to pH<2, or at least 24 hours prior to analysis 19. 6 months 38. Nitrate P, FP, G Cool 6 C 18 48 hours Askew Scientific Consulting LLC Page 7 table II Method Update Rule Parameter number/name Container 1 Preservation 2,3 Maximum holding time 4 39.