Appendix I Return to table of contents
Holding times, containers
and preservatives for wastewater samples. from 40CFR136, Table II, as amended 31Jan94, 59 FR 4504.
|
Parameter |
Container [1] |
Sample volume mL |
Maximum Holding time [4] |
|
| Bacterial Tests | ||||
| Coliform, Fecal and total | Sterile P or G |
100 |
Cool 4 ºC ,0.008% Na2S2O3 [5] | 6 hours from time of collection |
| Fecal Sterile streptococci | Sterile P or G |
100 |
Cool 4 ºC ,0.008% Na2S2O3 [5] | 6 hours from time of collection |
| Inorganic Tests | ||||
| Acidity | P,G |
500 |
Cool 4 ºC | 14 days |
| Alkalinity | P,G |
500 |
Cool 4 ºC | 14 days |
| Ammonia | P,G |
500 |
Cool 4 ºC, H2SO4 to pH <2 | 14 days |
| BOD | P,G |
1000 |
Cool 4 ºC | 48 hours |
| Bromide | P,G |
500 |
None required | 28 days |
| CBOD | P,G |
1000 |
Cool 4 ºC | 48 hours |
| COD | P,G |
500 |
Cool 4 ºC, H2SO4 to pH <2 | 28 days |
| Chloride | P,G |
500 |
None required | 28 days |
| Chlorine, total residual | P,G |
500 |
None required | Analyze immediately |
| Color | P,G |
500 |
Cool 4 ºC | 48 hours |
| Cyanide, tota land amenableto chlorination | P,G |
1000 |
Cool
4 ºC, NaOH to pH <2 > 12, 0.6 g ascorbic acid5 |
14 days[6] |
| Fluoride | P |
1000 |
None required | 28 days |
| Hardness | P,G |
500 |
HNO3 to pH <2, H2SO4 to pH <2 | 6 months |
| Hydrogen ion (pH) | P,G |
500 |
None required | Analyze immediately |
| Kjeldahl and organic Nitrogen | P,G |
500 |
Cool 4 ºC, H2SO4 to pH <2 | 28 days |
|
Parameter |
Container [1] |
Sample volume mL |
Maximum Holding time [4] |
|
| Metals tests[11] | ||||
| Boron | P (PTFE) |
500 |
HNO3 to pH <2 | 6 months |
| Chromium VI | P,G |
500 |
Cool 4 ºC | 24 hours |
| Mercury | P,G |
500 |
HNO3 to pH <2 | 28 days |
| Metals, other | P,G |
500 |
HNO3 to pH <2 | 6 months |
| Inorganic Tests | ||||
| Nitrate | P,G |
500 |
Cool 4 ºC | 48 hours |
| Nitrate-nitrite | P,G |
500 |
Cool 4 ºC, H2SO4 to pH <2 | 28 days |
| Nitrite | P,G |
500 |
Cool 4 ºC | 48 hours |
| Oil and grease | G |
1000 |
Cool 4 ºC, HCl or H2SO4 to pH <2 | 28 days |
| Organic carbon | G |
500 |
Cool 4 ºC, HCl , H2SO4 o rH3PO4 to pH <2 | 28 days |
| Orthophosphate | P,G |
500 |
Filter immediately, Cool 4 ºC | 48 hours |
| Oxygen, dissolved | ||||
|
PROBE |
in situ |
in situ |
in situ | in situ[12] |
|
WINKLER |
G |
300 |
Fix (add manganous sulfate, alkaline iodide azide and sulfuric acid) on site and store in dark | 8 hours |
| Phenols, total | G |
500 |
Cool 4 ºC, H2SO4 to pH <2 | 28 days |
|
Parameter |
Container [1] |
Sample volume mL |
Maximum Holding time [4] |
|
| Phosphorous | ||||
|
elemental |
G |
500 |
Cool 4 ºC | 48 hours |
|
total |
G |
500 |
Cool 4 ºC, H2SO4 to pH <2 | 28 day |
| Inorganic Tests | ||||
| Residue, total (TS) | P,G |
500 |
Cool 4 ºC | 7 days |
| Residue, | ||||
|
Filterable (TDS) |
P,G |
500 |
Cool 4 ºC | 7 days |
|
Nonfilterable (TSS) |
P,G |
500 |
Cool 4 ºC | 7 days |
|
settleable |
P,G |
1000 |
Cool 4 ºC | 48 hours |
|
volatile |
P,G |
500 |
Cool 4 ºC | 7 days |
| Silica | P or Quartz |
500 |
Cool 4 ºC | 28 days |
| Specific Conductance | P,G |
500 |
Cool 4 ºC | 28 days |
| Sulfate | P,G |
500 |
Cool 4 ºC | 28 days |
| Sulfide | P,G |
1000 |
Cool 4 ºC, add zinc acetate and NaOH to pH >9 | 7 days |
| Sulfite | P,G |
500 |
None required | Analyze immediately |
| Surfactants | P,G |
1000 |
Cool 4 ºC | 48 hours |
| Temperature | P,G |
500 |
None required | Analyze immediately |
| Turbidity | P,G |
500 |
Cool 4 ºC | 48 hours |
| Organic Tests (method) | ||||
| Purgeable halocarbons (601, 624, or 1624) | 40 mL glass, Teflon lined silicon septum |
|
Cool 4 ºC, 0.008% Na2S2O35 | 14 days |
|
Parameter |
Container [1] |
Sample volume mL |
Maximum Holding time [4] |
|
|
Parameter |
Container [1] |
Sample volume mL |
Maximum Holding time [4] |
|
[1] Polyethylene (P) or Glass (G).
[2]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, the chemical samples may be preserved by maintaining at 4 ºC until compositing and sample splitting is completed.
[3] When any sample is to be shipped by common carrier or sent through the US Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of the Table, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 SU or greater); Nitric acid (HNO3) in water solutions of 0.15% by weight or less (pH about 1.62 SU or greater); Sulfuric acid (H2SO4 ) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 SU or greater); and Sodium Hydroxide (NaOH) in water solutions of 0.080 % by weight or less (pH about 12.30 or less).
[4]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. Samples my be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for longer time, and has received a variance from the Regional Administrator under 40 CFR 136.3(e). Some samples may not be stable for the maximum time period given in the Table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.
[5] Should only be used in the presence of residual chlorine.
[6]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 of 12.
[7]Polyethylene (P) or Glass (G).
[8]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, the chemical samples may be preserved by maintaining at 4 ºC until compositing and sample splitting is completed.
[9]When any sample is to be shipped by common carrier or sent through the US Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of the Table, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 SU or greater); Nitric acid (HNO3) in water solutions of 0.15% by weight or less (pH about 1.62 SU or greater); Sulfuric acid (H2SO4 ) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 SU or greater); and Sodium Hydroxide (NaOH) in water solutions of 0.080 % by weight or less (pH about 12.30 or less).
[10]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. Samples my be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for longer time, and has received a variance from the Regional Administrator under 40 CFR 136.3(e). Some samples may not be stable for the maximum time period given in the Table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.
[11]Samples should be filtered immediately on-site before adding preservative for dissolved metals.
[12]in situ means that the probe is inserted into the actual mass to be sampled, recording the readout including profiles.
[13]Polyethylene (P) or Glass (G).
[14]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, the chemical samples may be preserved by maintaining at 4 ºC until compositing and sample splitting is completed.
[15]When any sample is to be shipped by common carrier or sent through the US Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of the Table, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 SU or greater); Nitric acid (HNO3) in water solutions of 0.15% by weight or less (pH about 1.62 SU or greater); Sulfuric acid (H2SO4 ) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 SU or greater); and Sodium Hydroxide (NaOH) in water solutions of 0.080 % by weight or less (pH about 12.30 or less).
[16]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. Samples my be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for longer time, and has received a variance from the Regional Administrator under 40 CFR 136.3(e). Some samples may not be stable for the maximum time period given in the Table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.
[17] Polyethylene (P) or Glass (G).
[18]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, the chemical samples may be preserved by maintaining at 4 ºC until compositing and sample splitting is completed.
[19] When any sample is to be shipped by common carrier or sent through the US Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of the Table, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 SU or greater); Nitric acid (HNO3) in water solutions of 0.15% by weight or less (pH about 1.62 SU or greater); Sulfuric acid (H2SO4 ) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 SU or greater); and Sodium Hydroxide (NaOH) in water solutions of 0.080 % by weight or less (pH about 12.30 or less).
[20]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. Samples my be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for longer time, and has received a variance from the Regional Administrator under 40 CFR 136.3(e). Some samples may not be stable for the maximum time period given in the Table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.
[21] Should only be used in the presence of residual chlorine.
[22]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 of 12.
[23]Polyethylene (P) or Glass (G).
[24]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, the chemical samples may be preserved by maintaining at 4 ºC until compositing and sample splitting is completed.
[25]When any sample is to be shipped by common carrier or sent through the US Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of the Table, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 SU or greater); Nitric acid (HNO3) in water solutions of 0.15% by weight or less (pH about 1.62 SU or greater); Sulfuric acid (H2SO4 ) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 SU or greater); and Sodium Hydroxide (NaOH) in water solutions of 0.080 % by weight or less (pH about 12.30 or less).
[26]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. Samples my be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for longer time, and has received a variance from the Regional Administrator under 40 CFR 136.3(e). Some samples may not be stable for the maximum time period given in the Table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.
[27]Samples should be filtered immediately on-site before adding preservative for dissolved metals.
[28]in situ means that the probe is inserted into the actual mass to be sampled, recording the readout including profiles.
[29]Polyethylene (P) or Glass (G).
[30]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, the chemical samples may be preserved by maintaining at 4 ºC until compositing and sample splitting is completed.
[31]When any sample is to be shipped by common carrier or sent through the US Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of the Table, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 SU or greater); Nitric acid (HNO3) in water solutions of 0.15% by weight or less (pH about 1.62 SU or greater); Sulfuric acid (H2SO4 ) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 SU or greater); and Sodium Hydroxide (NaOH) in water solutions of 0.080 % by weight or less (pH about 12.30 or less).
[32]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. Samples my be held for longer periods only if the permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are stable for longer time, and has received a variance from the Regional Administrator under 40 CFR 136.3(e). Some samples may not be stable for the maximum time period given in the Table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.