210454031 ASTM D 4542 07 Standard Test Method for Pore Water Extraction and Determination of the...

Designation: D 4542 07

Standard Test Method forPore Water Extraction and Determination of the Soluble SaltContent of Soils by Refractometer1

This standard is issued under the fixed designation D 4542; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope*1.1 This test method covers a rapid procedure for squeezing

pore water from fine-grained soils for the purpose of determin-ing the amount of soluble salts present in the extracted porewater.

1.2 This test method was developed for soils having a watercontent equal to or greater than approximately 14 %, forexample, marine soils. An extensive summary of proceduresfor extracting pore water from soils has been presented byKriukov and Manheim (1).2

1.3 This test method is not generally applicable for deter-mining the soluble salt content of the pore water extracted fromcoarse-grained soils, such as clean sands and gravels.

1.4 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.

1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.

1.6 All observed and calculated values shall conform to theguidelines for significant digits and rounding established inPractice D 6026.

2. Referenced Documents2.1 ASTM Standards: 3D 653 Terminology Relating to Soil, Rock, and Contained

FluidsD 3740 Practice for Minimum Requirements for Agencies

Engaged in the Testing and/or Inspection of Soil and Rock

as Used in Engineering Design and ConstructionD 6026 Practice for Using Significant Digits in Geotechni-

cal DataE 832 Specification for Laboratory Filter Papers2.2 Federal Document:GG-S-945a Specification for Syringe and Needle, Dispos-

able, Hypodermic, Sterile, Single Injection4

3. Terminology3.1 Definitions:3.1.1 For definitions of terms in this standard, refer to

Terminology D 653.

4. Significance and Use4.1 The soluble salt content may be used to correct the index

properties of soils (water content, void ratio, specific gravity,degree of saturation, and dry density).

4.2 It is necessary to minimize the time period betweensampling and testing due to chemical changes which may occurwithin the soil sample.

NOTE 1The quality of the result produced by this standard isdependent on the competence of the personnel performing it, and thesuitability of the equipment and facilities used. Agencies that meet thecriteria of Practice D 3740 are generally considered capable of competentand objective testing/sampling/inspection/etc. Users of this standard arecautioned that compliance with Practice D 3740 does not in itself assurereliable results. Reliable results depend on many factors; Practice D 3740provides a means of evaluating some of those factors.

NOTE 2Hulbert and Brindle (2) and Torrance (3) have shown thatprolonged storage should be avoided as unpredictable and nonreproduc-ible chemical changes may occur.

5. Apparatus5.1 RefractometerA temperature compensated refracto-

meter scaled to either index of refraction or ppt (parts perthousand). A typical hand held refractometer is shown in Fig.1.

5.2 Soil PressThe apparatus shall conform to the require-ments shown in Fig. 2.

1 This test method is under the jurisdiction of ASTM Committee D18 on Soil andRock and is the direct responsibility of Subcommittee D18.06 on Physical-ChemicalInteractions of Soil and Rock.

Current edition approved July 1, 2007. Published July 2007. Originally approvedin 1985. Last previous edition approved in 2001 as D 4542 95 (2001).

2 The boldface numbers in parentheses refer to the list of references appended tothis standard.

3 For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at [email protected]. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.

4 Available from Naval Publications and Forms Center, 5801 Tabor Ave.,Philadelphia, PA, 19120.

1

*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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Not for Resale, 07/24/2008 08:01:57 MDTNo reproduction or networking permitted without license from IHS

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5.3 SyringeA 25-cm3 syringe without needle, in accor-dance with Fed. Std. GG-S-945a.

5.4 BalanceA balance capable of weighing with a sensi-tivity of 60.01 g.

5.5 Filter Paper:5.5.1 A general purpose quantitative filter paper in accor-

dance with Specification E 832, Type II, Class F, for mediumcrystalline precipitates in the size range from 5 to 10 m, withan ash content of 0.13 mg/12.5-cm circle. Cut filter paper to adiameter of 55 mm (2.25 in.).

5.5.2 A general purpose quantitative filter paper in accor-dance with Specification E 832, Type II, Class G, for finecrystalline precipitates in the size range from 0.45 m, with an

ash content of 0.13 mg/12.5-cm circle. Cut filter paper to adiameter of 25 mm (0.98 in.).

5.6 RefrigeratorCooling unit capable of maintaining auniform temperature between 1 and 5C.

5.7 Micro-Syringe Filter HolderA device to filter a liquiddirectly from a syringe.5

5.8 100-mL Polyethylene or Glass Bottle and Cap.5.9 Miscellaneous SuppliesDistilled water, alcohol, di-

luted HCl (1:10), detergent, and optional sterile bags forsample storage (see 7.6).6. Preparation of Apparatus

6.1 Wash all parts of the press thoroughly. Rinse twice withdistilled water and dry. Normally, rust should not be present,but if it is to be removed, especially inside or around the top ofthe cylinder, scrub gently with steel wool and soap or chromic

acid. Rinse well with tap water and then twice with distilledwater and dry.

6.2 If the press parts have been coated with rust preventive,wash them with alcohol and rinse once with tap water andtwice with distilled water.

6.3 Dry by a method that will not contaminate the press.Clean compressed air, oven or air drying, or rinsing withacetone followed by air drying are acceptable.

6.4 Assemble the press.

5 An apparatus such as the stainless steel Millipore Micro-Syringe Filter HolderXX30-025-00 is satisfactory for this purpose.

FIG. 1 Typical Hand-Held Refractometer

FIG. 2 Soil Press

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NOTE 3To prevent mud from circumventing the stainless steel wirescreen use flexible TFE-fluorocarbon gaskets on each side.

7. Sampling and Test Specimen Squeezing7.1 Select a representative soil sample of approximately 50

g and place into the cylinder on top of a single sheet of 5 to10-m (55-mm) filter paper.

7.2 Apply pressure slowly until the first drops of water areexpelled, then insert a clean, disposable, plastic syringe (25mL) in the effluent passage shown in Fig. 2. This is done tominimize the amount of air in the syringe and therefore, theamount of evaporation.

7.3 Apply pressure gradually to a maximum of 80 MPa(11 520 psi), and hold until no more water is expelled or untilthe syringe is full (see Note 4 and Note 5).

7.4 Withdraw the syringe when the pressure is at a maxi-mum and immediately expel the fluid from the syringe througha stainless steel micro-syringe holder, fitted with fresh 0.45-m(25-mm) filter paper, into a clean 100-mL bottle (see Note 6).Cap the bottle. Expose the collected water to the atmosphere aslittle as possible.

7.5 Repeat 7.1-7.4, using the same syringe and filter ifadditional water is needed for experimentation and can becollected. Usually about 25 mL of pore water may be collectedfrom 50 g of sediment (see Note 7 and Note 8). Store the waterat a temperature between 1 and 5C (see Note 9 and Sections8 and 9).

7.6 Remove the soil from the press. If additional tests areanticipated, store soil in a sterile plastic bag at a temperaturebetween 1 and 5C (see Note 9).

NOTE 4Only a few drops (0.05 mL) of pore fluid are required toconduct the soluble salt determination by refractometer. It is recom-mended that 25 mL of pore water be collected, if possible, to allow forretesting or additional tests, or both.

NOTE 5Kriukov and Komarova (4) have found that at a pressure of 59MPa (8500 psi) the chloride content drops in homogeneous soils.Manheim (5) reports using 101 MPa (14 700 psi) routinely. An average ofthese two recommendations is 80 MPa (11 520 psi).

NOTE 6Polyethylene or glass bottles should be washed with detergentand rinsed with tap water. They should then be rinsed once with dilutedHCl (1:10) and twice with distilled water and then drained thoroughly.

NOTE 7The amount of water expelled will depend on the initial watercontent of the sample. For example, using a 50-g sample of moist soil andassuming that 1 cm3 of liquid is required to fill the apparatus, thefollowing water contents are required to achieve the indicated amounts ofexpelled water:

Initial Water Content Amount of Water Expelled (mL)

104 2570 2047 1528 1014 52 0

NOTE 8The addition of fluid to a sample to increase its water contentso that an increased amount of water can be expelled may result in theleaching of salts present in the soil and may distort the original salt contentof the pore water.

NOTE 9A storage temperature of about 5C is recommended toreduce the growth of sulfate-reducing bacterium called Desulfovibrio.

8. Procedure8.1 Method ASalinity Determination Using a Refractome-

ter With a Refraction Index Scale:8.1.1 Filter specimen through a 0.45-m filter.8.1.2 Thoroughly wash with distilled water and dry the

refractometer, shown in Fig. 1.8.1.3 Place a few drops of liquid on the refractometer

platform and close the slide gently.8.1.4 Hold the refractometer at right angles to a light source

and read the refractive index.8.1.5 Obtain salinity from the accompanying graph (Fig. 3),

where n is the refractive index of the liquid and no therefractive index of distilled water (1.330 at 20C).

NOTE 10A typical temperature-compensated instrument is accurate to0.1 % between 15.6 and 37.8C; the instrument is most accurate between18.3 and 21.1C.

8.2 Method BSalinity Determination Using a Refractome-ter With a ppt Scale:

8.2.1 Thoroughly wash with distilled water and dry therefractometer, shown in Fig. 1.

8.2.2 Place one to two drops of liquid into the semicircle ofthe white plastic area, which is held firmly against the glassplatform. Allow the liquid to escape only under the whiteplastic area.

8.2.3 Hold the refractometer at right angles to a light sourceand read the salinity. If the liquid is properly introduced, thereshould be a distinct black/white boundary. Read where thebottom of the hairline touches the beginning of the blackboundary. Read to the nearest whole number.

NOTE 11Salinity is given in parts per thousand parts (0/00). Salinityis the total amount of solid material, in grams, contained in 1 kg of seawater when all the carbonate has been converted to oxide, the bromine andiodine replaced by chlorine, and all organic matter completely oxidized(Sverdrup, Johnson, Fleming, (6)).

NOTE 12Error in reading directly from the salinity scale is 60.3 ppt.NOTE 13Actual sea water samples may have a black/yellow/white

boundary when reading the refractometer. Readings are always taken atthe beginning of the black boundary. Two to three readings should alwaysbe taken to ensure accuracy and precision.

FIG. 3 Graph of Salinity versus Refraction Index

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9. Report: Test Data Sheet(s)/Forms(s)9.1 The methodology used to specify how data are recorded

on the test data sheet(s)/form(s), as given below, is covered in1.6.

9.2 For each test, a record of the following observations isrequired:

9.2.1 Location,9.2.2 Depth,9.2.3 Soil type,9.2.4 ppt or percent soluble solids,9.2.5 Water content, and9.2.6 Total density of undisturbed sample.

10. Precision and Bias10.1 PrecisionTest data on precision is not presented due

to the nature of the soil materials tested by this test method. It

is either not feasible or too costly at this time to have ten ormore laboratories participate in a round-robin testing program.In addition, it is either not feasible or too costly to producemultiple specimens that have uniform physical properties. Anyvariation observed in the data is just as likely to be due tospecimen variation as to operator or laboratory testing varia-tion.

10.1.1 Subcommittee D18.06 is seeking any data from theusers of this test method that might be used to make a limitedstatement on precision.

10.2 BiasThere is no accepted reference value for this testmethod, therefore bias cannot be determined.

11. Keywords11.1 marine soils; porewater; refractometer; salt content;

soluble salt; soluble salt content

APPENDIX

(Nonmandatory Information)

X1. MASS COMPOSITION

X1.1 Mass Composition TermsX1.1.1 A mass composition diagram for partially saturated

soils with soluble salts is shown in Fig. X1.1. Based on thisfigure the following terms and definitions are defined fordescribing various relationships among soil phases as proposedby Noorany (7). There are other phase relationship conventionsproposed in several references below which offer differentapproaches to calculating corrections (8-10) to the relatedindex properties.

M = wet massMd = oven dried mass (105C)Ms = mass of soil solids (excluding salt)Msa = mass of saltMsw = mass of sea waterr = salinity = Msa/Msw = mass of salt/mass of sea waterMw = mass of distilled water = M MdV = total volumeVs = volume of soil solids (excluding salt)Vsw = volume of sea saltVw = volume of distilled waterVg = volume of gasVv = volume of voids = Vsw + Vgrs = density of solids excluding saltro = density of distilled water at 4C = 1 g/cm3r sw = density of salt water at test temperature = 1.029

g/cm3Gs = specific gravity of solids excluding salts = rs/ro.

X1.2 Definitions and Phase Relations (7)X1.2.1 Using the terms defined in X1.1.1 and referring to

Fig. X1.1, Mw = M Md = Msw Msa = Msw(1 r) whichyields the following:

Msw 5M 2 Md

1 2 r (X1.1)FIG. X1.1 Mass Composition Diagram for Soils ContainingSoluble Salts

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Ms 5 M 2 Msw 5Md 2 rM

1 2 r (X1.2)

Vsw 5Mswrsw

5M 2 Md

~1 2 r!rsw(X1.3)

Vs 5Ms

Gsro5

MsGsro

5Md 2 rM

~1 2 r!Gs ro(X1.4)

X1.2.2 The following terms are defined as follows:

Density r 5MV (X1.5)

Dry density rd 5MsV 5

Md 2 rMV~1 2 r! 2 (X1.6)

Water content ~%! w 5MwMd

3 100 5M 2 Md

Md3 100 (X1.7)

Fluid content ~%! w 5MswMs

3 100 5M 2 MdMd 2 rM

3 100 (X1.8)

Void ratio e 5VvVs

5V~1 2 r!Gsro

Md 2 rM2 1 (X1.9)

Porosity n 5VvV 3 100 % (X1.10)

n 5 F1 2 ~Md 2 rM!v~1 2 r!GsroG 3 100 (X1.11)

Degree of saturation

s 5VswVv

3 100 (X1.12)

s 5Gs~M 2 Md!

v~1 2 r!Gsro 2 Md 1 rMrorsw

3 100 (X1.13)

X1.3 Other Useful Relationships

Md 5M

1 1 w (X1.14)

Ms 5M

1 1 w (X1.15)

rd 5r

1 1 w (X1.16)

n 5e

1 1 e (X1.17)

w 5w

1 2 r 2 rw (X1.18)

e 5VGsro~1 1 w!

M 21 (X1.19)

or

e 5wGs

S 3rorsw

(X1.20)

REFERENCES

(1) Kriukov, P. A., and Manheim, F. T., Extraction and InvestigativeTechniques for Study of Interstitial Waters of Unconsolidated Sedi-ments: A Review, Dynamic Environment of the Sea Floor, LexingtonBooks, Lexington, MA, pp. 326.

(2) Hulburt, W. H., and Brindle, M. P., Effects of Sample Handling on theComposition of Marine Sedimentary Pore Water, Geological Societyof American Bulletin, Vol 86, January 1975, pp. 109110.

(3) Torrance, J. K., Pore Water Extraction and the Effect of SampleStorage on the Pore Water Chemistry of Leda Clay, Soil SpecimenPreparation for Laboratory Testing, ASTM, STP 599, ASTM, 1976,pp. 147157.

(4) Kriukov, P. A., and Komarova, N. A., Issledovanie rastovorov pochu,ilovi gornykh porod (Studies on the Interstitial Waters of Soils, Muds,and Rocks), Mezhdunarodnomu Kongressu pochvovedov, 2nd Komis-siya, Doklady VI, 1956, pp. 151184.

(5) Manheim, F. T., A Hydraulic Squeezer for Obtaining Interstitial Water

from Consolidated and Unconsolidated Sediments, U. S. GeologicSurvey Professional Paper 550-e, 1966, pp. 256261.

(6) Sverdrup, H. U., Johnson, M. W., and Fleming, R. H., The Oceans,Prentice-Hall, Inc., New York, 1946, p. 1087.

(7) Noorany, I., Phase Relations In Marine Soils, Journal of Geotech-nical Engineering, ASCE, Vol 110, No. 4, April 1994, pp. 539543.

(8) Boyce, R. E., Appendix I. Physical Property Methods. In InitialReports of the Deep Sea Drilling Project, ed. N. T. Edgar, J. B.Saunders, et al., Vol. 15, 1973, pp. 1115 1127, Washington, DC: U.S.Government Printing Office.

(9) Hamilton, E. L., Prediction of In-Situ Acoustic and Elastic Propertiesof Marine Sediments, Geophysics, Vol. 36:2, 1971, pp. 266 284.

(10) Imai, G., Tsuruya, K. and Yano, K., A Treatment of Salinity in WaterContent Determinations of Very Soft Clays, Soils and Foundations,Vol. 19, September 1979, No. 3.

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SUMMARY OF CHANGES

Committee D18 has identified the location of selected changes to this standard since the last issue (June 10,2001) that may impact the use of this standard. (Approved July 1, 2007.)

(1) Add 1.6 referencing requirement to conform with PracticeD 6026.(2) In 2.1, add Practice D 6026 to list of referenced docu-ments.(3) In 2.1, add Practice D 3740 to list of referenced docu-ments.(4) Added Section 3 on Terminology.(5) Renumbered subsequent sections and references to sec-tions.

(6) In Section 4 (old 3), added Note 1 that includes referenceto Practice D 3740.(7) Renumbered subsequent notes and references to motes.(8) Revised Section 9 (old 8) to conform with Committee D18guidelines on Report section.(9) Revised Section 10.1 (old 9) to conform with CommitteeD18 guidelines on Precision statements.(10) In Appendix X1.1, added to statement that other phaserelationships were available in References.(11) Add References 8-10.

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ScopeReferenced DocumentsTerminologySignificance and UseApparatusPreparation of ApparatusFIG. 1 FIG. 2 Sampling and Test Specimen SqueezingProcedureFIG. 3 Report: Test Data Sheet(s)/Forms(s)Precision and BiasKeywordsX1. MASS COMPOSITIONX1.1 Mass Composition TermsFIG. X1.1 X1.3 Other Useful Relationships Md M1 w (X1.14) Ms M1 w (X1.15) d 1 w (X1.16) n e1 e (X1.17) w w1 r rw (X1.18) e VGso1 wM 1 (X1.19) REFERENCES

210454031 ASTM D 4542 07 Standard Test Method for Pore Water Extraction and Determination of the...

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