Preservation & Holding Times
Holding times should be from the documented time a sample was collected, not based on midnight of the last day. For example, if a semivolatile water sample (with a holding time of 7 days) was taken at 8:30 am on Tuesday, October 15, 2024, then the laboratory can extract that sample at any time up until 8:30 am on Tuesday, October 22, 2024 and be considered within the method's holding time.
Holding times are distinctions in the methods to try to reduce the effect of degradation on the results due to analyte decomposition, reaction, evaporation and any number of other effects of time on a sample matrix. However, a line has to be drawn somewhere for unacceptable losses and the method's holding time represents the best data available as to when the analysis is still completely valid. If an exact sample collection time is known, then the exact time should be used in calculating the holding times. If the collection time is recorded to the hour, the holding time should be interpreted to the hour. If the collection time is recorded to the hours and minutes, the holding time should be interpreted to the hours and minutes.
Ideally, laboratories should try to do the required preparation steps (i.e., extraction, digestion, etc.) in advance of the hold time's expiration so as to avoid hold time problems.
All chain of custody forms and sample acceptance forms will indicate the temperature of samples upon receipt. The sample acceptance form will indicate if thermal preservation requirements for the analysis request have not been met. This information is transferred during log-in to the LIMS record. Metals analysis for all matrices including low level mercury, PCB analysis of a chemical waste, samples requiring radiological analyses, and soil samples requiring pH only analysis do not require thermal preservation. Samples received for these analyses have met thermal preservation requirements even when received above 6oC.
METALS
Parameter |
Method |
Hold Time |
Preservative |
Container |
ID |
---|---|---|---|---|---|
Total Metals (excluding Hg) | 6010/200.7 6020/200.8 | 6 months | HNO3 to pH<2 | 1-500cc P | J |
Dissolved Metals (excluding Hg) | 6010/200.7 6020/200.8 | 6 months | Field Filtered, HNO3 to pH<2 | 1-500cc P | I |
Chromium, hexavalent | 7196A 3500Cr,B | 24 hours* | Cool 4oC | 1-500cc P | F |
Mercury | 7470A/245.1 | 28 days | HNO3 to pH<2 | 1-500cc P | J |
INORGANIC NON-METALS
Parameter | Method |
Hold Time |
Preservative |
Container |
ID |
---|---|---|---|---|---|
Acidity, Total | 2310B | 14 Days | 4°C | 1-500cc P | L |
Alkalinity, Total (CaCO3) | 2320B | 14 Days | 4°C | 1-500cc P | L |
Ammonia (as N) | 350.1R2.0 4500NH3, D | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
BOD, 5 Day | 5210B | 48 Hours | 4°C | 1-500cc P | L |
Bromide | 300.0 | 28 Days | 4°C | 1-500cc P | L |
CBOD, 5 Day | 5210B | 48 Hours | 4°C | 1-500cc P | L |
Chloride | 4500Cl, E 4500Cl, C | 28 Days | 4°C | 1-500cc P | L |
Chlorine Residual, Free | 4500Cl, G | Immed. | 4°C | 1-500cc P | L |
Chlorine Residual, Total | 4500Cl, G | Immed. | 4°C | 1-500cc P | L |
Chlorophyll a | SM10200H | 2 Days | 4°C | 1-1L AG | N |
Chromium, Hexavalent | 3500Cr,B 7196A | 28 Days* | NaOH,4°C | 1-250cc P | F |
COD | 5220D | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Coliform, Fecal | COLILERT | 7 Hours | Sterile | Bact | P |
Coliform, Total | SM9222B | 1 Day | Sterile | Bact | P |
Color, true | 2120B | 2 Days | 4°C | 1-960cc P | L |
Conductivity | 2510B | 28 Days | 4°C | 1-500cc P | L |
Cyanate | 4500CN, L | 10 Days | NaOH,4°C | 1-250cc P | F |
Cyanide, Amenable | 4500CN,C,G | 14 Days | NaOH,4°C | 1-250cc P | F |
Cyanide, Total | 335.4R1.0 4500CN,C,E 9010B/9014 | 14 Days | NaOH,4°C | 1-250cc P | F |
Cyanide, WAD | 4500CN-I,E | 14 Days | NaOH,4°C | 1-250cc P | F |
Dissolved Oxygen | 4500O,G | Immed. | 4°C | 1-500cc P | L |
Fluoride | 4500F,C | 28 Days | 4°C | 1-500cc P | L |
Hardness, Total (as CaCO3) | 2340C | 6 Months | 4°C | 1-960cc P | L |
Hydrolyzable Phosphorus (as P) | 4500P,B,E | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Iron Bacteria | SM9222B | 1 Day | Sterile | Bact | P |
Iron, Ferrous | 3500Fe. B | 4°C | 1-500cc P | L | |
MBAS | SM5540C | 48 Hours | None | 1-250cc P | L1 |
Nitrate (as N) | 353.2R2.0 | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Nitrate + Nitrite (as N) | 4500NO3, E | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Nitrite (as N) | 4500NO2,B | 48 Hours | 4°C | 1-500cc P | L |
Oil & Grease | 1664A | 28 Days | HCL, 4°C | 1-1L AG | M |
Organic and Volatile Acids | HPLC-UV | 14 Days | 4°C | 1-500cc P | L |
Organic Phosphorus (as P) | 4500P, A | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Orthophosphate (as P) | 4500P,E | 48 Hours | 4°C | 1-500cc P | L |
pH @ 25°C | 4500H+,B 9040B | Immed. | 4°C | 1-500cc P | L |
Phenols | 9066 420.4R1.0 | 28 Days | H2SO4, 4°C | 1-250mL AG | H |
Phosphate (as PO4) | 4500P,B,E | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Phosphorus (as P) | 4500P,B,E | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Settable Organic Solids | 2540F, b | 7 Days | 4°C | 1-500cc P | L |
Settable Solids | 2540F, b | 48 Hours | 4°C | 1-500cc P | L |
Silica (as SiO2) | 4500SiO2,C | 28 Days | 4°C | 1-500cc P | L |
Soluble COD | 5220D | 28 Days | None | 1-500cc P | L |
Sulfate | 375.2R2.0 4500S04,E | 28 Days | 4°C | 1-500cc P | L |
Sulfide | 4500S2C,D | 7 Days | NaOH/ZnAc | 1-250cc P | O |
Sulfite | 4500SO3,B | Immed. | 4°C | 1-500cc P | L |
Threshold Odor | 2150B | Immed. | 4°C | 1-960cc P | L |
TIC | 5310C | 28 Days | No Treat | 1-250mL AG | D1 |
TOC | 5310C 9060 | 28 Days | H2SO4, 4°C | 1-250mL AG | H |
Total Carbon | 5310C | 28 Days | H2SO4, 4°C | 1-250mL AG | H |
Total Dissolved Solids | 2540C | 7 Days | 4°C | 1-500cc P | L |
Total Kjeldahl Nitrogen (TKN) | 351.2R2.0 | 28 Days | H2SO4, 4°C | 1-250cc P or AG | H |
Total Non-Volatile Suspnd Solids | 2540E | 7 Days | 4°C | 1-500cc P | L |
Total Solids | 2540B | 7 Days | 4°C | 1-500cc P | L |
Total Suspended Solids | 2540D | 7 Days | 4°C | 1-500cc P | L |
Total Volatile Solids | 2540E | 7 Days | 4°C | 1-500cc P | L |
Total Volatile Suspended Solids | 2540E | 7 Days | 4°C | 1-500cc P | L |
TOX | 9020B | 14 Days | H2SO4, 4°C | 1-500mL AG | E1 |
TPH (SGT-HEM) | 1664A | 28 Days | HCL, 4°C | 1-1L AG | M |
Turbidity | 2130B | 48 Hours | 4°C | 1-500cc P | L |
KEY to container types: P = Plastic; AG = Amber Glass
* If unpreserved the Hexavalent chromium HT is 24 hours.
ORGANIC PARAMETERS
Parameter | Method |
Hold Time |
Preservative |
Container |
---|---|---|---|---|
EDB/DBCP (Method 8011) | 8011 | 28 Days | 4°C | 2-40mL Vials |
Pesticides/PCBs | 8081A/8082 | 7 Days Extraction 40 Days Analysis | 4°C1 | 1-1L AG |
Pesticides | 608/8081A | 7 Days Extraction 40 Days Analysis | 4°C | 1-1L AG |
Polychlorinated biphenyls (PCBs) | 8082 | None | 4°C | 1-1L AG |
Carbamate Pesticides | 531.1R3.1 | 28 Days | 4°C | 2-40mL Vials |
Endothall | 548.1R1.0 | 7 Days | 4°C | 1-125mL AG |
Non-Halogenated Organic Compounds | 8015B | 7 Days Extraction 40 Days Analysis | 4°C | 2-40mL Vials |
Organophosphorus Pesticides | 8141A | 4°C | 1-1L AG | |
Dioxin, High Resolution | 8290 | 30 Days Extraction 45 Days Analysis | 4°C | 2-1L AG |
Dioxin, Low Resolution | 8280 | 30 Days Extraction 45 Days Analysis | 4°C | 2-1L AG |
Formaldehyde | 8315A | 30 Days | 4°C | 1-125mL AG |
Herbicides | 8321A | 7 Days Extraction 40 Days Analysis | 4°C1 | 1-1L AG |
Dissolved Gases | RSK175/D1946 | 14 Days | HCL, 4°C | 2-40mL Vials |
Trihalomethanes (THMs) | 524.2 | 14 Days | HCL, 4°C | 3-40mL Vials |
Semi-Volatile Compounds (SVOCs) | 625/8270C | 7 Days Extraction 40 Days Analysis | 4°C1 | 1-1L AG |
Polynuclear Aromatic Hydrocarbons | 8270C | 7 Days Extraction 40 Days Analysis | 4°C1 | 1-1L AG |
TOC | 5310C/9060 | 28 Days | H2SO4, 4°C | 1-250mL AG |
TOX | 9020B | 14 Days | H2SO4, 4°C | 1-500mL AG |
TPH | 8015B | 7 Days Extraction 40 Days Analysis | 4°C | 1-1L AG |
Volatile Organic Compounds | 624/8260B | 14 Days | HCL, 4°C1 | 2-40mL Vials |
KEY to container types: Vials = zero-headspace 40mL vial; AG = Amber Glass
SAMPLE BOTTLE PRESERVATIVES AND HOLDING TIMES FOR SOILS & SEDIMENT SAMPLES
METALS
Parameter |
Hold Time |
Preservative |
Container |
---|---|---|---|
General, total | 6 Months | None | 4 or 8 oz. Wide-mouth Glass Jar |
Chromium, hexavalent | 30 Days to Extraction 7 Days to Analysis | None | 4 or 8 oz. Wide-mouth Glass Jar |
Mercury | 28 Days | None | 4 or 8 oz. Wide-mouth Glass Jar |
ORGANIC PARAMETERS
Parameter |
Hold Time |
Preservative |
Container |
---|---|---|---|
Pesticides and PCBs | 14 Days to Extraction 40 Days to Analysis | Unpreserved Cool 4o C |
4 or 8 oz. Wide-mouth Glass Jar |
GC/MS Semivolatiles (including PNAs) | 14 Days to Extraction 40 Days to Analysis | Unpreserved Cool 4o C | 4 or 8 oz. Wide-mouth Glass Jar |
Volatile Organics | 14 Days | Method 5035 sampling Cool 4o C | 4 or 8 oz. Wide-mouth Glass Jar plus Method 5035 Vials |
PCBs (Only) | None | Cool 4o C | 4 or 8 oz. Wide-mouth Glass Jar |