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PRESERVATION AND HOLDING TIMES

GENERAL CHEMISTRY

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General Chemistry Parameter

New Method10

Previous

Holding Time

Minimum Volume

Water Sampling


MUR 04/11/07

C&T Method

Water

Soil

Water

Soil

Container

Preservative

Acidity

SM 2310B

EPA 305.1

14 days

- -

100 mL

- -

250mL P

None

Alkalinity (as CaCO3)

SM 2320B

EPA 310.1

14 days

NS5

100 mL

- -

250mL P

None

Ammonia Nitrogen

SM 4500NH3-D

EPA 350.3

28 days

- -

100 mL

- -

250mL P

H2SO4

Asbestos

various

various

NS5

NS5

1 L

50 g

1L P

None

Bicarbonate Alkalinity

SM 2320B

EPA 310.1

14 days

- -

100 mL

- -

250mL P

None

Bioassay, %survival

NPDES

NPDES

36 hr

- -

5 gallons

- -

5gal cube

None

Bioassay, screen

CCR Title 22

CCR Title 22

36 hr

36 hr

500 mL

200 g

1L G

None

Biochemical Oxygen Demand (BOD)

SM 5210B

EPA 405.1

48 hr

- -

600 mL

- -

1L P

None

Carbon, Total Organic

SM 5310C

EPA 415.2

28 days

- -

40 mL

- -

2 x 40mL VOA

H2SO4

Walkley-Black

Walkley-Black

- -

NS5

- -

25 g

- -

- -

Carbon, Total Inorganic

SM 5310C

EPA 415.2

28 days

- -

40 mL

- -

2 x 40mL VOA

H2SO4

Carbonate Alkalinity

SM 2320B

EPA 310.1

NS5

- -

100 mL

- -

250mL P

None

Cation Exchange Capacity

EPA 9081

EPA 9081

- -

6 mo

- -

10 g

- -

- -

Chemical Oxygen Demand (COD)

SM 5220D

EPA 410.4

28 days

- -

100 mL

- -

250mL P

H2SO4

COD, Filtered

SM 5220D

EPA 410.4

28 days

- -

100 mL

- -

250mL P

H2SO4

Chloride

EPA 300.0

EPA 300.0

28 days

- -

100 mL

- -

250mL P

None

Chlorine, Residual

SM 4500Cl-G

EPA 330.5

15 min

- -

100 mL

- -

250mL G

Foil wrapped

Coliform, Fecal



6 hr

- -

100 mL

- -

sterile 100mL

Na2S2O3

Color

SM 2120B

EPA 110.2

48 hr

- -

50 mL

- -

250mL G

None

Conductivity

SM 2510B

EPA 120.1

24 hr4

- -

100 mL

- -

250mL P

None

Corrosivity to Steel (NACE)

EPA 1110

EPA 1110

NS5

NS5

1 L

1000 g

1L G

None

Chromium, Hexavalent

EPA 7196A

EPA 7196A

24 hr

30 days

100 mL

40 g

500mL P

None

EPA 7199

EPA 7199

24 hr

- -

50 mL

- -

250mL P

None

SM 3500Cr-D

SM 3500Cr-D

24 hr

- -

50 mL

- -

250mL P

None

Cyanide

SM 4500Cn-E

EPA 335.2

14 days

- -

500 mL

- -

500mL P

NaOH

EPA 9010B/9014

EPA 9010B/9014

14 days

14 days

500 mL

5 g

500mL P

NaOH

Cyanide, Amenable

SM 4500Cn-E

EPA 335.2

14 days

- -

500 mL

- -

500mL P

NaOH

EPA 9010B/9014

EPA 9010B/9014

14 days

14 days

500 mL

10 g

500mL P

NaOH

Cyanide, Reactive

SW846 Ch.7

SW846 Ch.7

NS5

NS5

25 mL

10 g

500mL P

None

Density

ASTM or AOCS

ASTM or AOCS

NS5

- -

200 mL

- -

250mL P or G

None

Dissolved Oxygen

SM 4500O-G

EPA 360.1

15 min

- -

100 mL

- -

250mL G

None

Dissolved Sulfide

SM 4500S2-D

EPA 376.2

7 days

- -

50 mL

- -

500mL P

NaOH

Ferrous Iron (Fe2+)

SM 3500Fe-D

SM 3500Fe-D

15 min

- -

50 mL

- -

100mL P or G

HCL

Ferric Iron (Fe3+)

SM 3500Fe-D

SM 3500Fe-D

24 hr

- -

see Notes

- -

2 x 100mL P

see Note(6)

Flash Point

EPA 1010A

EPA 1010A

NS5

- -

60 mL

NA

250mL P

None

Fluoride

EPA 300.0

EPA 300.0

28 days

28 days

100 mL

10 g

250mL P

None

Free Liquids (Paint Filter Test)

EPA 9095

EPA 9095

NS5

NS5

100 mL

50 g

500mL wide

None

Halogens, Total Organic

EPA 9020

EPA 9020

28 days

28 days

200 mL

10 g

250mL P or G

H2SO4

Hardness, as CaCO3

SM 2340B

EPA 130.2

6 mo

- -

100 mL

- -

250mL P

HNO3

Hexavalent Chromium

EPA 7196A

EPA 7196A

24 hr

30 days

100 mL

40 g

500mL P

None

EPA 7199

EPA 7199

24 hr

- -

50 mL

- -

250mL P

None

SM 3500Cr-D

SM 3500Cr-D

24 hr

- -

50 mL

- -

250mL P

None

Ignitability

SW846 Ch.7

SW846 Ch.7

- -

NS5

- -

10 g

- -

None

Iron, Ferrous (Fe2+)

SM 3500Fe-D

SM 3500Fe-D

24 hr

- -

50 mL

- -

100mL P

HCL

Iron, Ferric (Fe3+)

SM 3500Fe-D

SM 3500Fe-D

24 hr

- -

see Note(6)

- -

2 x 100mL  P

see Note(6)

MBAS (Surfactants)

SM 5540C

EPA 425.1

48 hr

- -

250 mL

- -

1L P

None

Moisture

ASTM D2216/CLP

CLP-SOW

- -

NS5

- -

25 g

- -

None

Nitrate Nitrogen

EPA 300.0

EPA 300.0

48 hr

- -

100 mL

- -

250mL P

None

Nitrite Nitrogen

EPA 300.0

EPA 300.0

48 hr

- -

100 mL

- -

250mL P

None

Nitrate/ Nitrite Nitrogen

EPA 300.0

EPA 300.0

28 days

- -

100 mL

- -

250mL P

None

Nitrogen, Ammonia

SM 4500NH3-D

EPA 350.3

28 days

28 days

100 mL

10 g

250mL P

H2SO4

Nitrogen, Total Kjeldahl (TKN)

SM 4500NH3-C

EPA 351.4

28 days

28 days

50 mL

5 g

1L P

H2SO4

Oil & Grease, Petroleum (H.E.M.-SG)

EPA 1664A

EPA 1664A

28 days

- -

1 L

- -

1L G

HCL

Oil & Grease, Total (H.E.M.)

EPA 1664A

EPA 1664A

28 days

- -

1 L

- -

1L G

HCL

Organic Carbon, Total (TOC)

SM 5310C

EPA 415.2

28 days

- -

40 mL

- -

2 x 40mL VOA

H2SO4

Walkley-Black

Walkley-Black

- -

NS5

- -

25 g

- -

None

Organic Lead

CA LUFT7

CA LUFT7

14 days

14 days

100 mL

50 g

250mL P

None

Oxygen Demand, Biochemical

SM 5210B

EPA 405.1

48 hr

- -

600 mL

- -

1L P

None

Oxygen Demand, Chemical

SM 5220D

EPA 410.4

28 days

- -

100 mL

- -

250mL P

H2SO4

Oxygen, Dissolved

SM 4500O-G

EPA 360.1

15 min

- -

100 mL

- -

250mL G

None

Paint Filter Test

EPA 9095

EPA 9095

NS5

NS5

100 mL

50 g

500mL wide

None

Perchlorate

EPA 314.0

EPA 314.0

28 days

- -

100 mL

- -

250mL P

None

pH

EPA 9040B/9045C

EPA 9040B/9045C

24 hr

14 days

100 mL

50 g

250mL P

None

SM 4500H+B

EPA 150.1

15 min

- -

100 mL

- -

250mL P

None

Phenolic Compounds

EPA 420.1

EPA 420.1

28 days

- -

500 mL

- -

1L G

H2SO4

Phosphate, ortho-

SM 4500P-E

EPA 365.2

48 hr

- -

50 mL

- -

100mL P

None

Phosphate, Total

SM 4500P-E

EPA 365.2

28 days

28 days

50 mL

10 g

250mL P

H2SO4

Reactive Cyanide

SW846 Ch.7

SW846 Ch.7

NS5

NS5

25 mL

10 g

500mL P

None

Reactive Sulfide

SW846 Ch.7

SW846 Ch.7

NS5

NS5

25 mL

10 g

500mL P

None

Residual Chlorine

SM 4500Cl-G

EPA 330.5

15 min

- -

- -

100mL P

None

Resistivity

SM 2510B

EPA 120.1

28 days

- -

100 mL

- -

250mL P

None

Salinity

SM 2520B

SM 2520B

NS5

- -

250 mL

- -

250mL G

wax seal

Silica

SM 4500SiO2-C

EPA 370.1

28 days

28 days

50 mL

10 g

100mL P

None

Solids, Settleable

SM 2540F

EPA 160.5

48 hr

- -

1 L

- -

1L G

None

Solids, Total Dissolved

SM 2540C

EPA 160.1

7 days

- -

100 mL

- -

250mL G

None

Solids, Total Suspended

SM 2540D

EPA 160.2

7 days

- -

100 mL

- -

250mL G

None

Solids, Total Volatile

SM 2540E

EPA 160.4

7 days

NS5

100 mL

50 g

250mL P

None

Sulfate

EPA 300.0

EPA 300.0

28 days

- -

100 mL

- -

250mL P

None

Sulfide, Total

SM 4500S2-D

EPA 376.2

7 days

- -

50 mL

- -

500mL P

NaOH + ZnAc

Sulfide, Dissolved

SM 4500S2-D

EPA 376.2

7 days

- -

50 mL

- -

500mL P

NaOH

Sulfide, Reactive

SW846 Ch.7

SW846 Ch.7

NS5

NS5

25 mL

10 g

500mL P

None

Sulfite

SM 4500SO3-B

EPA 377.1

15 min

- -

100 mL

- -

500mL  P

None

Surfactants (MBAS)

SM 5540C

EPA 425.1

48 hr

- -

250 mL

- -

1L P

None

Total Dissolved Solids (TDS)

SM 2540C

EPA 160.1

7 days

- -

100 mL

- -

250mL P

None

Total Inorganic Carbon

SM 5310C

EPA 415.2

28 days

- -

40 mL

- -

2 x 40mL VOA

H2SO4

Total Kjeldahl Nitrogen (TKN)

SM 4500NH3-C

EPA 351.4

28 days

28 days

50 mL

5 g

1L P

H2SO4

Total Organic Carbon (TOC)

SM 5310C

EPA 415.2

28 days

- -

40 mL

- -

2 x 40mL VOA

H2SO4

Walkley-Black

Walkley-Black

- -

NS5

- -

25 g

- -

None

Total Organic Halogens (TOX)

EPA 9020B

EPA 9020B

28 days

28 days

200 mL

10 g

250mL P or G

H2SO4

Total Suspended Solids (TSS)

SM 2540D

EPA 160.2

7 days

- -

100 mL

- -

250mL G

None

Total Volatile Solids

SM 2540E

EPA 160.4

7 days

NS5

100 mL

50 g

250mL P

None

Tributyl Tin

GC/FPD

GC/FPD

NS5

NS5

1 L

10 g

1L P or G

None

Turbidity

SM 2130B

EPA 180.1

48 hr

- -

100 mL

- -

250mL G

None

Viscosity

ASTM methods

ASTM methods

NS5

- -

25 mL

- -

50mL P

None




General Minerals

New Method10

Previous

Holding Time

Minimum Volume

Water Sampling


MUR 04/11/07

C&T Method

Water

Soil

Water

Soil

Container

Preservative

Alkalinity (as CaCO3)

SM 2320B

EPA 310.1

14 days

NS5

100 mL

- -

250mL P

None

Chloride, Sulfate

EPA 300.0

EPA 300.0

28 days

- -

100 mL

- -

250mL P

None

Conductivity

SM 2510B

EPA 120.1

24 hr4

- -

100 mL

- -

250mL P

None

PH

SM 4500H+B

EPA 150.1

15 min

14 days

100 mL

- -

250mL P

None

Total Dissolved Solids (TDS)

SM 2540C

EPA 160.1

7 days

- -

100 mL

- -

250mL P

None

Ca, Fe, Mg, Na, Zn, Hardness

EPA 200.7 or 6010B

EPA 200.7 or 6010B

6 mo

6 mo

100 mL

- -

250mL P

HNO3

Optional Analysis (can be added to list):

Surfactants (MBAS)

SM 5540C

EPA 425.1

48 hr

- -

250 mL

- -

1L P

None




Major Cations

Method

Holding Time

Minimum Volume

Water Sampling



Water

Soil

Water

Soil

Container

Preservative

Ca, Mg, K, Na

EPA 200.7 or 6010B

6 mo

6 mo

100 mL

- -

250mL P

HNO3




Major Anions

New Method10

Previous

Holding Time

Minimum Volume

Water Sampling


MUR 04/11/07

C&T Method

Water

Soil

Water

Soil

Container

Preservative

Bicarbonate, Carbonate Alkalinity

SM 2320B

EPA 310.1

14 days

NS5

100 mL

- -

250mL P

None

Chloride, Sulfate

EPA 300.0

EPA 300.0

28 days

- -

100 mL

- -

250mL P

None




RCI

Method

Holding Time

Minimum Volume

Water Sampling



Water

Soil

Water

Soil

Container

Preservative

Reactive Cyanide

SW846 Ch.7

NS5

NS5

25 mL

10 g

500mL P

None

Reactive Sulfide

SW846 Ch.7

NS5

NS5

25 mL

10 g

500mL P

None

PH

EPA 9040B/9045C

24 hr

14 days

100 mL

50 g

250mL P

None

Ignitability

SW846 Ch.7

- -

NS5

- -

10 g

- -

None




Ion Chromatography

Method

Holding Time

Minimum Volume

Water Sampling



Water

Soil

Water

Soil

Container

Preservative

Bromide

EPA 300.0

28 days

NS5

100 mL

1 g

250mL P

None

Chloride

EPA 300.0

28 days

NS5

100 mL

1 g

250mL P

None

Nitrate-Nitrogen

EPA 300.0

48 hr

NS5

100 mL

1 g

250mL P

None

Nitrite-Nitrogen

EPA 300.0

48 hr

NS5

100 mL

1 g

250mL P

None

ortho-Phosphate Phosphorus

EPA 300.0

48 hr

NS5

100 mL

1 g

250mL P

None

Sulfate

EPA 300.0

28 days

NS5

100 mL

1 g

250mL P

None

Hexavalent Chromium

EPA 7199

24 hr

NA

100 mL

- -

250mL P

None

Perchlorate

EPA 314.0

28 days

NA

100 mL

- -

250mL P

None



Notes

4.

Holding time for conductivity may be extended to 28 days if the samples are filtered within 24 hours of collection.

5.

NS: No holding time is specified in the regulations for these methods.

6.

Ferric Iron (Fe 3+) is the difference between total and ferrous iron.

Requires submission of two polyethylene bottles, one preserved with HCl and one with HNO3.

7.

CA LUFT: California Department of Health Services Leaking Underground Fuel Tank Manual, October 1989.

8.

Holding times specified in 40CFR 136.3 Table 2 (Clean Water Act/NPDES) and SW-846 Table 2-36 Rev 3, Dec 1996.

9.

Samples should be preserved within 15 minutes of collection and kept at 40C from time of collection until analysis.

Preserved containers can be supplied by C&T.

HCL: hydrochloric acid to pH<2, H2SO4: sulfuric acid to pH<2,  NaOH: sodium hydroxide to pH > 12,  ZnAc: Zinc Acetate.

10.

40CFR MUR (Methods Update Rule) was published in the Federal Register on March 12, 2007 and became effective on April 11, 2007.



General Legend

mg/L:

milligrams per liter (ppm)

µg/L:

micrograms per liter (ppb)

mg/Kg:

milligrams per kilogram (ppm)

µg/Kg:

micrograms per kilogram (ppb)

VOA:

Amber VOA vial

G:

Glass

P:

Polyethylene