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.This is just a sample listing and years old, please refer to 40CFR134 for the latest requirements.

Requirements for Samples

         Parameter 

  Container [1]

  Sample volume   mL

Preservation [2], [3]

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

Preservation [2], [3]

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

Preservation [2], [3]

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

Preservation [2], [3]

Maximum Holding time [4]

         
         
         
         

  Parameter 

Container [1]

Sample volume   mL

Preservation [2], [3]

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.