TABLE B Sample Preservation, Containers and Maximum Holding Times for Inorganic Parameters |
Parameter | Preservation1 | Container2 | Holding Time3 |
METALS |
Aluminum | HNO3 | P or G | 6 months |
Antimony | HNO3 | P or G | 6 months |
Arsenic | Conc.HNO3 to pH<2 | P or G | 6 months |
Barium | HNO3 | P or G | 6 months |
Beryllium | HNO3 | P or G | 6 months |
Cadmium | HNO3 | P or G | 6 months |
Copper | HNO3 | P or G | 6 months |
Chromium | HNO3 | P or G | 6 months |
Iron | HNO3 | P or G | 6 months |
Lead | HNO3 | P or G | 6 months |
Manganese | HNO3 | P or G | 6 months |
Mercury | HNO3 | P or G | 28 days |
Nickel | HNO3 | P or G | 6 months |
Selenium | HNO3 | P or G | 6 months |
Silver | HNO3 | P or G | 6 months |
Thallium | HNO3 | P or G | 6 months |
Zinc | HNO3 | P or G | 6 months |
OTHER PARAMETERS |
Asbestos | Cool, 4°C | P or G | 48 hours4 |
Bromate | Ethylenediamine | P or G | 28 days |
Chloride | None | P or G | 28 days |
Chlorite | 50 mg/L EDA, Cool to 4°C | P or G | 14 days |
Color | Cool, 4°C | P or G | 48 hours |
Cyanide | Cool, 4°C+NaOH to pH>12 | P or G | 14 days |
Fluoride | None | P or G | 28 days |
Foaming Agents | Cool, 4°C | P or G | 48 hours |
Nitrate (as N) Chlorinated Non-Chlorinated | Cool, 4°C Cool, 4°C | P or G P or G | 14 days 48 hours5 |
Nitrite (as N) | Cool, 4°C | P or G | 48 hours |
Nitrate + Nitrite6 | Conc. H2SO4 to pH<2 | P or G | 1428 days |
Odor | Cool, 4°C | G | 48 hours |
pH | None | P or G | Analyze Immediately |
Solids (TDS) | Cool, 4°C | P or G | 7 days |
Sulfate | Cool, 4°C | P or G | 28 days |
Turbidity | Cool, 4°C | P or G | 48 hours |
1 If HNO3 cannot be used because of shipping restrictions, sample may be initially preserved by icing and immediately shipping it to the laboratory. Upon receipt in the laboratory, the sample must be acidified with conc HNO3 to pH < 2. At time of analysis, sample container should be thoroughly rinsed with 1:1 HNO3; washings should be added to sample.1 For cyanide determinations samples must be adjusted with sodium hydroxide to pH 12 at the time of 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 8.3 of EPA Methods 200.7 or 200.8 or 200.9 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. |
4 Instructions for containers, preservation procedures and holding times as specified in Method 100.2 must be adhered to for all compliance analyses including those conducted with Method 101.1. |
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. |
Contaminant | MCL (mg/l) | Methodology | Detection limit (mg/l) |
Antimony | 0.006 | Atomic Absorption; Furnace | 0.003 |
Atomic Absorption; Platform | 0.00085 |
ICP-Mass Spectrometry | 0.0004 |
Hydride-Atomic Absorption | 0.001 |
Arsenic | 0.010 | Atomic Absorption; Furnace | 0.001 |
Atomic Absorption; Platform—Stabilized Temperature | 0.00056 |
Atomic Absorption; Gaseous Hydride | 0.001 |
ICP-Mass Spectrometry | 0.00147 |
Asbestos | 7 MFL1 | Transmission Electron Microscopy | 0.01 MFL |
Barium | 2 | Atomic Absorption; furnace technique | 0.002 |
Atomic Absorption; direct aspiration | 0.1 |
Inductively Coupled Plasma | 0.002 (0.001) |
Beryllium | 0.004 | Atomic Absorption; Furnace | 0.0002 |
Atomic Absorption; Platform | 0.000025 |
Inductively Coupled Plasma2 | 0.0003 |
ICP-Mass Spectrometry | 0.0003 |
Cadmium | 0.005 | Atomic Absorption; furnace technique | 0.0001 |
Inductively Coupled Plasma | 0.001 |
Chromium | 0.1 | Atomic Absorption; furnace technique | 0.001 |
Inductively Coupled Plasma | 0.007 (0.001) |
Cyanide | 0.2 | Distillation, Spectrophotometric3 | 0.02 |
Distillation, Automated, Spectrophotometric3 | 0.005 |
Distillation, Amenable, Spectrophotometric4 | 0.02 |
Distillation, Selective Electrode3, 4 | 0.05 |
UV, Distillation, Spectrophotometric9 | 0.0005 |
Micro Distillation, Flow Injection, Spectrophotometric3 | 0.0006 |
Ligand Exchange with Amperometry4 | 0.0005 |
Mercury | 0.002 | Manual Cold Vapor Technique | 0.0002 |
Automated Cold Vapor Technique | 0.0002 |
Nickel | X10.1 | Atomic Absorption; Furnace | 0.001 |
Atomic Absorption; Platform | 0.00065 |
Inductively Coupled Plasma2 | 0.005 |
ICP-Mass Spectrometry | 0.0005 |
Nitrate | 10 (as N) | Manual Cadmium Reduction | 0.01 |
Automated Hydrazine Reduction | 0.01 |
Automated Cadmium Reduction | 0.05 |
Ion Selective Electrode | 1 |
Ion Chromatography | 0.01 |
Capillary Ion Electrophoresis | 0.076 |
Nitrite | 1 (as N) | Spectrophotometric | 0.01 |
Automated Cadmium Reduction | 0.05 |
Manual Cadmium Reduction | 0.01 |
Ion Chromatography | 0.004 |
Capillary Ion Electrophoresis | 0.103 |
Selenium | 0.05 | Atomic Absorption; furnace | 0.002 |
Atomic Absorption; gaseous hydride | 0.002 |
0.002 | Atomic Absorption; Furnace | 0.001 |
Atomic Absorption; Platform | 0.00075 |
ICP-Mass Spectrometry | 0.0003 |
Contaminant | Detection Limit (mg/L) |
1. Alachlor | 0.0002 |
2. Aldicarb | 0.0005 |
3. Aldicarb sulfoxide | 0.0005 |
4. Aldicarb sulfone | 0.0008 |
5. Atrazine | 0.0001 |
6. Benzo[a]pyrene | 0.00002 |
7. Carbofuran | 0.0009 |
8. Chlordane | 0.0002 |
9. 2,4-D | 0.0001 |
10. Dalapon | 0.001 |
11. Dibromochloropropane | 0.00002 |
12. Di(2-ethylhexyl)adipate | 0.0060.0006 |
13. Di(2-ethylhexyl)phthalate | 0.0060.0006 |
14. Dinoseb | 0.0002 |
15. Diquat | 0.0004 |
16. Endothall | 0.009 |
17. Endrin | 0.00001 |
18. Ethylene dibromide | 0.00001 |
19. Glyphosate | 0.006 |
20. Heptachlor | 0.00004 |
21. Heptachlor epoxide | 0.00002 |
22. Hexachlorobenzene | 0.0001 |
23.Hexachlorocyclopentadiene | 0.0001 |
24. Lindane | 0.00002 |
25. Methoxychlor | 0.0001 |
26. Oxamyl | 0.002 |
27. Picloram | 0.0001 |
28.Polychlorinated biphenyls (PCBs as decachlorobiphenyls) | 0.0001 |
29. Pentachlorophenol | 0.00004 |
30. Simazine | 0.00007 |
31. Toxaphene | 0.001 |
32. 2,3,7,8-TCDD (Dioxin) | 0.000000005 |
33. 2,4,5-TP (Silvex) | 0.0002 |
Contaminant | EPA Methods1 | SM9 | SM Online10 | ASTM | Other |
Regulated Parameters: |
Synthetic Organic Chemicals |
2,3,7,8-TCDD (dioxin) | 1613 | 16131 |
2,4-D 2 (as acids, salts and esters) | 515.2, 555, 515.1, 515.3, 515.4 | D5317-93, 98 (Reapproved 2003) |
2,4,5-TP 2 (Silvex) | 515.2, 555, 515.1, 515.3, 515.4 | 6640 B, | 6640 B-01, B-0611 | D5317-93, 98 (Reapproved 2003) |
Alachlor | 507, 525.2, 525.32 508.1, 5058, 551.1 |
Atrazine 3 | 507, 525.2, 525.3 508.1, 5058, 551.1, 536 | Syngenta4 AG-625 |
Benzo(a)pyrene | 525.2, 525.3, 550, 550.1 |
Carbofuran | 531.1, 531.2 | 66105. 6610 B | 6610 B-04 |
Chlordane | 508, 525.2, 525.3, 508.1, 505 |
Dalapon | 552.1 515.1, 552.2, 515.3, 515.4, 552.3, 557 | 6640 B | 6640 B-01, 06 |
Di(2-ethylhexyl)adipate | 506, 525.2, 525.3 |
Di(2-ethylhexyl)phthalate | 506, 525.2, 525.3 |
Dibromochloropropane (DBCP) | 504.1, 551.1, 524.39 |
Dinoseb | 515.2, 555, 515.1, 515.3, 515.4 | 6640 B | 6640 B-01, 06 |
Diquat | 549.2 |
Endothall | 548.1 |
Endrin | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Ethylene dibromide (EDB) | 504.1, 551.1, 524.39 |
Glyphosate | 547 | 66516 6651 B | 6651 B-01, B-06 |
Heptachlor | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Heptachlor Epoxide | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Hexachlorobenzene | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Hexachlorocyclopentadiene | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Lindane | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Methoxychlor | 508, 525.2, 525.3, 508.1, 505, 551.1 |
Oxamyl | 531.1, 531.2 | 66105 6610 B | 6610 B-04 |
PCBs (as decachlorobiphenyl) | 508A7 |
(as Aroclors) | 508.1, 508, 525.2, 525,3 505 |
Pentachlorophenol | 515.2, 525.2, 525.3, 555, 515.1, 515.3, 515.4 | D5317-93, 98 (Reapproved 2003) |
Picloram 2 | 515.2, 555, 515.1, 515.3, 515.4 | 6640 B | 6640 B-01 | D5317-93, 98 s(Reapproved 2003) |
Simazine | 507, 525.2, 525.3, 523, 536, 508.1, 5058, 551.1 |
Toxaphene | 508, 508.1, 525.2, 525.3, 505 |
Unregulated Parameters: |
Aldicarb | 531.1, 531.2 | 66105 6610 B | 6610 B-04 |
Aldicarb sulfone | 531.1, 531.2 | 66105 6610 B | 6610 B-04 |
Aldicarb Sulfoxide | 531.1 , 531.2 | 66105 6610 B | 6610 B-04 |
Aldrin | 505, 508, 525.2, 525.3, 508.1 |
Butachlor | 507, 525.2, 525.3 |
Carbaryl | 531.1, 531.2 | 66105 6610 B | 6610 B-04 |
Dicamba | 515.1, 555, 515.2 515.3, 515.4 | 6640 B | 6640 B-01, B-06 |
Dieldrin | 505, 508, 525.2, 525.3, 508.1 |
3-Hydroxcarbofuran | 531.1, 531.2 | 66105 6610 B | 6610 B-04 |
Methomyl | 531.1, 531.2 | 66105 6610 B | 6610 B-04 |
Metolachlor | 507, 525.2, 525.3, 508.1 |
Metribuzin | 507, 525.2, 525.3, 508.1 |
Propachlor | 507, 525.2, 525.3, 508.1 |
Method | Preservative2 | Sample Holding Time | Extract Holding Time and Storage Conditions | Suggested Sample Size | Type of Container |
502.22 | Sodium Thiosulfate or Ascorbic Acid , 4ºC, HCl pH<2 | 14 days | NA | 40 – 120 mL | Glass with PTFE1 Lined Septum |
504.1 | Sodium Thiosulfate Cool, 4ºC | 14 days | 4ºC, 24 hours | 40 mL | Glass with PTFE1 Lined Septum |
505 | Sodium Thiosulfate Cool, 4ºC | 14 days (7 days for Heptachlor) | 4ºC, 24 hours | 40 mL | Glass with PTFE1 Lined Septum |
506 | Sodium Thiosulfate Cool, 4ºC, Dark | 14 days | 4ºC, Dark 14 days | 1 L | Amber Glass with PTFE1 Lined Septum |
507 | Sodium Thiosulfate Cool, 4ºC, Dark | 14 days (See method for exceptions.) | 4ºC, Dark 14 days | I L | Amber Glass with PTFE1 Lined Cap |
508 | Sodium Thiosulfate Cool, 4ºC, Dark | 7 days (See method for exceptions.) | 4ºC, Dark 14 days | I L | Glass with PTFE1 Lined Cap |
508A | Cool 4ºC | 14 days | 30 days | I L | Amber Glass with PTFE1 Lined Cap |
508.1 | Sodium Sulfite HCl pH<2 Cool, 4ºC | 14 days (See method for exceptions.) | 30 days | I L | Glass with PTFE Lined Cap |
515.1 | Sodium Thiosulfate Cool, 4ºC, Dark | 14 days | 4ºC, Dark 28 days | I L | Amber Glass with PTFE1 Lined Cap |
515.2 | Sodium Thiosulfate or Sodium Sulfite HCl pH<2 Cool, 4ºC, Dark | 14 Days | ≤4ºC, Dark 14 Days | I L | Amber Glass with PTFE1 Lined Cap |
515.3 | Sodium Thiosulfate Cool, 4ºC, Dark | 14 days | ≤4ºC, Dark 14 Days | 50 mL | Amber Glass with PTFE1 Lined Cap |
515.4 | Sodium Sulfite, Dark, Cool ≤10ºC for First 48 hrs, ≤6ºC thereafter | 14 days | ≤0ºC 21 days | 40 mL | Amber Glass with PTFE1 Lined Cap |
524.22 | Ascorbic Acid or Sodium Thiosulfate HCl pH<2, Cool 4ºC | 14 days | NA | 40 – 120 mL | Glass with PTFE1 Lined Septum |
524.32 | Maleic and Ascorbic Acids pH<2, ≤10ºC for first 48 hrs., ≤6 thereafter If only analyzing TTHM: Sodium Thiosulfate pH<2, ≤10ºC for first 48 hrs., ≤6 thereafter | 14 days | NA | 40 – 120 mL | Amber Glass with PTFE1 Lined Septum |
525.2 | Sodium Sulfite, Dark, Cool, 4ºC, HCl pH<2 | 14 days (See method for exceptions) | ≤4ºC 30 days | 1 L | Amber Glass with PTFE1 Lined Cap |
531.1, 6610 | Sodium Thiosulfate, Monochloroacetic Acid pH<3, Cool, 4ºC | Cool 4ºC from collection until storage at laboratory; <-10ºC at the laboratory; 28 days | NA | 60 mL | Glass with PTFE1 Lined Septum |
531.2 | Sodium Thiosulfate, Potassium Dihydrogen Citrate Buffer pH<4, Dark ≤10ºC for first 48 hrs., ≤6ºC thereafter | 28 days | NA | 40 mL | Glass with PTFE1 Lined Septum |
547 | Sodium Thiosulfate Cool, 4ºC | 14 days; 18 mos. Frozen | NA | 60 mL | Glass with PTFE1 Lined Septum |
548.1 | Sodium Thiosulfate; HCl pH 1.5 -2 if High Biological Activity; Cool, 4ºC, Dark | 7 days | ≤4ºC 14 days | ≥ 250 mL | Amber Glass with PTFE1 Lined Septum |
549.2 | Sodium Thiosulfate; H2SO4 pH<2, if Biologically Active; Cool 4ºC, Dark | 7 days | 21 days | ≥ 250 mL | High Density Amber Plastic or Silanized Amber Glass |
550 | Sodium Thiosulfate Cool 4ºC, HCl pH<2 | 7 days | 4ºC, Dark 30 days | 1 L | Amber Glass with PTFE1 Lined Septum |
550.1 | Sodium Thiosulfate Cool 4ºC, HCl pH<2 | 7 days | 4ºC, Dark 40 days | 1 L | Amber Glass with PTFE1 Lined Septum |
551.1 | Sodium Sulfite. Ammonium Chloride, pH 4.5-5.0 with Phosphate Buffer Cool, 4ºC | 14 days | 14 days <-10ºC | ≥ 40 mL | Glass with PTFE1 Lined Septum |
552.1 | Ammonium Chloride Cool, 4ºC, Dark | 28 days | ≤4ºC, Dark 48 hrs. | 250 mL | Amber Glass with PTFE1 Lined Cap |
552.2 | Ammonium Chloride Cool, 4ºC, Dark | 14 days | ≤4ºC, Dark, 7 days ≤-10ºC, 14 days | 50 mL | Amber Glass with PTFE1 Lined Cap |
555 | Sodium Sulfite HCl pH ≤2 Dark, Cool, 4ºC | 14 days | NA | ≥ 100 mL | Glass wit PTFE1 Lined Cap |
1613 | Sodium Thiosulfate Cool 0 - 4ºC, Dark | 1 year | 40 days recommended | 1 L | Amber Glass with PTFE1 Lined Cap |