TABLE 1 | |||
REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIME FOR WATER SAMPLES | |||
PARAMETER | SAMPLE CONTAINER1 | SAMPLE PRESERVATION2,3 | RECOMMENDED HOLDING TIMES4 |
Bacterial Test: | |||
Coliform, fecal and total | 250-mL P | Cool, 4°C, 0.008% Na2S2O35 | 6 hours |
Fecal streptococci | 250-mL P | Cool, 4°C, 0.008% Na2S2O35 | 6 hours |
Inorganic Tests: | |||
Acidity | 250-mL P | Cool, 4°C | 14 days |
Alkalinity | 250-mL P | Cool, 4°C | 14 days |
Ammonia | 100-mL P | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Biochemical oxygen demand | 1-L P | Cool, 4°C | 48 hours |
Bromide | 100-mL P | None required | 28 days |
Biochemical oxygen demand, carbonaceous | 1-mL P | Cool, 4°C | 48 hours |
Chemical oxygen demand | 100-mL amber G | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Chloride | 100-mL P | None required | 28 days |
Chloride, total residual | 250-L P | None required | Analyze immediately |
Color | 250-mL P | Cool, 4°C | 48 hours |
Cyanide, total and amenable to chlorination | 1-mL P | Cool, 4°C, NaOH to pH > 12, 0.6 g asorbic acid | 14 days6 |
Fluoride | 100-mL P | None required | 28 days |
Hardness | 250-mL P | HNO3 to pH < 2, H2SO4 to pH < 2 | 6 months |
Hydrogen ion (pH) | 100-mL P | None required | Analyze immediatley |
kjeldahl and organic nitrogen | 250-mL P | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Chromium VI | 250-mL P | Cool, 4°C | 24 hours |
Mercury | 130 mL G | HNO3 to pH < 2 | 28 days |
Metals, except chromium VI and mercury | 250-mL P | HNO3 to pH < 2 | 6 months |
Nitrate | 100-mL P | Cool, 4°C | 48 hours |
Nitrate-nitrite | 100-mL P | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Nitrite | 100-mL P | Cool, 4°C | 48 hours |
Organic carbon | 125-mL amber G | Cool, 4°C, HCl or H2SO4 to pH < 2 | 28 days |
Orthophosphate | 100-mL P | Filter immediately, cool, 4°C | 48 hours |
Oxygen, dissolved (Probe) | G bottle & top | None Required | Analyze immediately |
Winkler | G bottle & top | Fix on site and store in dark | 8 hours |
Phosphorus (elemental) | G | Cool, 4°C | 48 hours |
Phosphorus, total | 250-mL P | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Residue, total | 500-mL P | Cool, 4°C | 7 days |
kResidue, filterable (TDS) | 500-mL P | Cool, 4°C | 7 days |
Residue, nonfilterable (TSS) | 500-mL P | Cool, 4°C | 7 days |
Residue, settleable | 500-mL P | Cool, 4°C | 48 hours |
Residue, volatile (VSS) | 500-mL P | Cool, 4°C | 7 days |
Silica | 250-mL P | Cool, 4°C | 28 days |
Specific Conductance | 100-mL P | Cool, 4°C | 28 days |
Sulfate | 100-mL P | Cool, 4°C | 28 days |
Sulfide | 250-mL P | Cool, 4°C, add zinc acetate plus sodium hydroxide to pH > 9 | 7 days |
Sulfite | 100-mL P | None required | Analyze immediately |
Surfactants | 1-mL P | Cool, 4°C | 48 hours |
Temperature | 100-mL P | None required | Analyze immediately |
Turbidity | 250-mL P | Cool, 4°C | 48 hours |
Organic Tests:8 | |||
Purgeable halocarbons | 4 x 40-mL G, Teflon-lined septum | Cool, 4°C, 0.008% Na2S2O35, or 0.06% ascorbic acid5 | 14 days |
Purgeable aromatic hydrocarbons | 4 x 40-mL G, Teflon-lined septum | Cool, 4°C, 0.008% Na2S2O35, adjust pH to 4-510 or 0.06% ascorbic acid5 | 14 days |
Acrolein and acrylonitrile | 1-L G, Teflon-lined septum | Cool, 4°C, 0.008% Na2S2O35 | 14 days |
Phenols11 | 1-L G, Teflon-lined cap | Cool, 4°C | Extraction-7 days Analysis-40 days |
Benzidines11,12 | 1-L G, Teflon-lined cap | Cool, 4°C, 0.008% Na2S2O35 | Extraction- 7 days13 |
Phthalate esters11 | 1-L G, Teflon-lined cap | Cool, 4°C | Extraction-7 days |
Nitrosamines11,14 | 1-L G, Teflon-lined cap | Cool, 4°C, Store in dark, 0.008% Na2S2O35 | Extraction-7 days Analysis-40 days |
Pesticides11 | 1-L G, Teflon-lined cap | Cool, 4°C, pH 5-915 | Extraction-7 days Analysis-40 days |
PCBs11 | 1-L G, Teflon-lined cap | Cool, 4°C | Extraction-7 days Analysis-40 days |
Nitroaromatics and isophorone11 | 1-L G, Teflon-lined cap | Cool, 4°C, 0.008% Na2S2O35 | Extraction-7 days Analysis-40 days |
Polynuclear aromatic hydrocarbons11 | 1-L G, Teflon-lined cap | Cool, 4°C, 0.008% Na2S2O35 | Extraction-7 days Analysis-40 days |
Haloethers11 | 1-L G, Teflon-lined cap | Cool, 4°C, 0.008% Na2S2O35 | Extraction-7 days Analysis-40 days |
Chlorinated hydrocarbons11 | 1-L G, Teflon-lined cap | Cool, 4°C | Extraction-7 days Analysis-40 days |
TCDD11 | 1-L G, Teflon-lined cap | Cool, 4°C, 0.008% Na2S2O35 | Extraction-7 days Analysis-40 days |
Total organic halogens | 500-mL amber G, Teflon-lined cap | Cool, 4°C H2SO4 to pH < 2 | 28 days |
Total petorleu hydrocarbons | 1-L G, Teflon-lined cap | Cool, 4°C HCl to < 2 | 28 days |
Phenols, total recoverable | 1-L G | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Oil and grease | 1-L G | Cool, 4°C, H2SO4 to pH < 2 | 28 days |
Radiological Tests: | |||
Alph, beta and radium | P,G | HNO3 to pH< 2 | 6 months |
Footnotes:
- Polyethylene (P) or Glass (G). In cases where more than one inorganic parameter with the sample preservative is required, a single sample container of sufficient size for all analyses is usually preferred. Such grouping of parameters will be indicated when bottles are provided for client sampling.
- Sample preservation should be performed immediately upon sample collection. For composite chemical samples, each aliquot should be preserved at the time of collection. When use of an automated sampler makes it impossible to preserve each aliquot, chemical samples may be preserved by maintaining at 4?C until compositing and sample splitting are completed.
- When any sample is to be shipped by common carrier or sent through the United States mail, it must comply with the Department of Transportation Hazardous materials Regulations (49 CFR Part 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements, the Office of Hazardous Materials, Materials Transportation bureau, Department of Transportation has determined that the Hazardous Material Regulations do not apply to the following: Hydrochloric Acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric Acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less).
- Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before analysis and still be considered valid.
- Sodium thiosulfate or ascorbic acid may be used only if residual chlorine is present. The dechlorination agent and hydrochloric acid must not be combined in pre-preserved vials.
- Maximum holding time is 24 hours when sulfide is present. Optionally, all samples may be tested with lead acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is filtered and then NaOH is added to pH 12.
- Samples should be filtered immediately on-site before adding preservative for dissolved metals.
- Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
- Sample receiving no pH adjustments must be analyzed within seven days of sampling.
- The ph adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no ph adjustment must be analyzed within three days of sampling.
- When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times would be observed for optimum safeguard of sample integrity. When the analytes of concern fall within two or more chemical categories, the sample may be preserved by cooling to 4?C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 609; samples preserved in this manner may be held for seven days before extraction and for forty days after extraction.