Page 48Line

1 2 3 4 5 6 7 8 9 10 1) 12 134—————L

100't

Contoured Depth•t———i———i———i———i———i———r———i———i

f jrompJe £

p =2

0+00

1+00 . . . . . . . . . . . . . . . .100 nm

2+00

3+OO

4+00

5+00

6+00

7+00

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Cooksvilfo/OnforioExample t

Model p, =200jimi

SR300668C-203

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e^ ^-^ . ' oo?£

o «u >o ^ ^ oo-— _ —_ » ^-

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Page 50

C-205 flR300670

Page 51

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C-20&-

EM31 MANUAL Page 52

APPENDIX I - Formulae for Geometrical Sounding of___________ .Two-Layered Earth _______________In the case of a two-layered earth the apparentconductivity is given by:

a^ ^ 1 - R + kR = R(k - 1) + i

with the instrument on the ground in its .normaloperating position, and

V- « 1 - R' + kR1 - Rf (k - i) + 1 (2)

with the instrument on the ground on its side.Case 1. Therefore

R aa-^ - 1

and from the first. and/or second equations, withk - a / ff-

067

{3}

(4)2 R R'

Case-2. When the conductivity of the lower layeris known, from equations (1) and (2)

R'°2 (5)

C-207

u*KTfT*TMANUAL Page 53*

APPENDIX I - Cont'd

Case 2. (cont'd)

- Rf _ "2

(6)

V - °2 = °1 " Rt°l + R'a2 " a2 (7)- (1 - RM (c - C) (8)

0 - a m (1 - R) (o. - a ) (9) ia * x - - - ** \

I - R OaclO2

- o.R ' ff ' - cr-R1a 2___1 - R 1 - R'

Case 3. When the upper layer is resistive and 02is much greater then a*, from equations (5) and (6)

a = o,Ra £

a .ILL , , . . . . . . . „ 114)-

anda o.' "j'

0 * _ * » _ * - - - -- - . . . .1— -i*1-' (15)

AR300673c-2"08 "TV '^":: • :~ r:" !'- :V

EM31 • •" • MANUAL page 54

-;;cpn.t!d,

Case-4. When the upper layer :is conductive and ais much less than OL, from equations (5) and (6) 2

a, (1.- -R)A (16}

(17)

1 - R' c*'

a

V- R 1 - R' (19)

• ttH30067U

EM31 MANUAL Page 55

APPENDIX II - "Determination of Two-Layered Earth Geometry___________ by Varying Instrument Height,,. ... _>. ^ -Ll ;

The electrical conductiv.ity of the earth often exhibitshorizontal layering and it is possible with the EM31 to .determine how closely this layering can be approximated ,bya two-layered earth geometry.

Suppose measurements made with the instrument on" the ground "have yielded different values of apparent conductivity whenthe instrument meter is (a) face-up (i.e. the instrument isin normal position), and (b) vertical (i.e. the instrumentis lying on its side). As discussed in Section 5.3 had thevalue of apparent conductivity been the same in both posi-tions we would know that the earth was homogeneous, butthe fact that the values are different for the two positionsshows that the electrical conductivity varies with depth.We would now like to know whether the earth is two-layered.

To determine this we make measurements of the apparentconductivity with the instrument at various heights abovethe ground, as measured by the distance between the groundand the nearest point of the white tube. It is suggestedthat measurements be made at increments at least as smallas one-half meter, for an example at 0, 0.5, 1, and 1,5meters. Measurements made at smaller increments will yieldgreater accuracy, as will measurements made up to 2 metersheight if possible. Measurements should be made both with"the instrument in its normal position (meter . face "upright ,i.e. vertical dipoles,) and with the instrument on its side(meter face vertical, horizontal dipoles) since it will be...seen from the curves that the fall-off with height for thesetwo configurations is quite, different and that this differ-ence is therefore of considerable diagnostic .value" "indetermining the two-layered . earth characteristic. ...It isimportant to make the measurements of height and apparent -conductivity as accurately as possible.

C-210

L

EM 31 MANUAL

APPENDIX II" - Cont'd. ... , _ .. , ., . . . 3ge

The curves in the two figures show the variation ofapparent conductivity {divided by upper layer conductivity)for instrument height varying from 0 to 2 meters and forfive values.of upper layer thickness vis. 0.5, 1.0, 1.5,2.0, and 3.0 meters. The relationship is shown for bothvertical dipoles .(meter -face .up, instrument in normalposition) and horizontal dipoles (meter face vertical,instrument on its side) for various values of upper layerto lower layer conductivity contrast.

#

To use the curves one proceeds as follows:(1) Place a piece of semi-transparent paper over either

one of the graphs and on it plot the measured valuesof apparent conductivity versus instrument height tothe scale used on the figures. Also sketch in on thetransparent paper at any point a horizontal or verticalline to insure that when the transparent paper istranslated over the figures in step 2 it does notrotate.

(2) Translate the transparent paper vertically and hori-zontally (i.e. without rotation} across the variousplots shown on the figures to see whether the datapoints can "be matched to. one of the curves. In the..event that.no "satisfactory match is achieved theearth cannot be -represented by a two-layered case.

(3) If a'satisfactory .match can'be achieved, the parametersof the two-layered earth are immediately calculated as .follows: suppose that the measured values of apparentconductivity with height are..

Height = ••-- —• --••- •- ~g, 0 0.5 ;.L:1..Q 1. 5 2. 0 meters

a (EM'31 upright) 20.7 ""20.7 19.3 17.1 14.1 mmho/maa1 (EM31 on side) 26.0 19.0 - 14.3 11..2 9.0 mmho/in

~——;——————flR3UUb/b

EM31 MANUAL ; Page 57APPENDIX II - Cont'd

Upon plotting these data values...to the scale .of"the figuresand translating them we see that best agreement is achievedfor an upper layer thickness of..1.5 meters 'and a "conduc-tivity contrast., k = 0.5. We f.urther observe, that thevalue of 20.7 millimhos per meter for. CT .(instrument up-./ aright) corresponds to a value of 0 /GI of 0.62*.

Since a - 0.62 when o =20.7 ~" "a a

20.7 = 33.4 mmho/m0.62

Since k * Z = 0.5<TI

*"• aj « 0.5x33.4 = 16.7 mmho/m

and t = 1.5m from the figure.

The two-layered earth is fully resolved.

It will be observed that in some regions on these twofigures the resolution or differentiation between thevarious curves is not very great. For example if oneexamines the curves for t » 1.0 meters, and k = 100, 50,or 20, one sees that these curve., pairs, are.. almost identi- .-,.cal.. If the process described ..in step 3 is carried .outfor each of these conductivity contrasts _the .result, of ,:the calculations will show that the lower. layer conductivityand the upper layer thickness are the same, regardless :of . .which of the three curve pairs are .used/ and that the only .calculated parameter that will .vary will ;be the .upper .layer conductivity which is very small.. This is an exampleof the well-known property of electromagnetic, systems toaccurately give both the distance to a good conductor and

*

C-21- 7

EM31 .......— -. MANUAL page 58

APPENDIX Il"-...Cprit'l_d._ „!..___.._ .- ....

the actual conductivity of the conductor but to poorlydefine the intervening resistive material. A problem inunambiguously matching the curves may also occur forlarger"" values of upper layer thickness, where the thick-ness is sufficiently great to prevent accurate resolutionof its value.

These features notwithstanding it will be found that thesecurves are useful in (a) deciding whether the ground re-sembles a two-layer case and if so (b) giving a reasonablyaccurate estimate of the electrical parameters.

flR300G78

too njrjrrjniiiE

TWO LAYER^CURVESHEIGHT VARIED,

Dipoies verticalDipoies horizontal

c-2i4:.:...

LiI

n-.......Page 6C

w ---T T- £T3E Z

LAYER CURVESVARIED, "

Dipoles verticalDipoles horizontal

C-215

MDTE TO EM31 AND EM34 USERS:

One of the most conrnon problems with the instrument is thecontamination of battery contacts. To._cleah these"contacts"use fine sand paper C^OO or higher) and wipe several tiinesover the contacts.

Ensure that the spring action of the battery holders is maintained.Bend holder sides slightly if necessary.

i

July 1985.

—————————————————————AR3Q068c-216 ——- -.: . _.: ._i: "_:._. JL±- ..__..

APPENDIX D

ANALYTICAL METHODOLOGY

flR300682

Designation: D 421 - 58 (Reapproved 1978)'1

Standard Method forDRY PREPARATION OF SOIL SAMPLES FOR PARTICLE-SIZE ANALYSIS AND DETERMINATION OF SOILCONSTANTS1

I hi- tundani a mued under ihe fixed designation D -Cl; the number immedUtely foUowiaf the doifiuuoo iadiaia (be ym of,«wiiul adopuM or. in ite CMC of idim. Ac year of la« rtvnion. A amber M pntatittw (•dJcnaikcYaroflttliapprmtf.\ •4tpcneripi eprioo (<) iadkua u •duanil dunft *kt the 1m mum or

I. Scope • individual tesb are as foOows:I.I TO* method coven the diy pvepantion *-

..l soil ampta as received from the field for *** " ^ matenal passini a No. 10 (2.00-panide ize analysis and the detenninaiion of mm) sieve is required in amounts equal to 115 1the sot! constants. of sandy soils and 65 1 of either sOt or day soils.

4.1.2 Teas for Soil Constants— For the tests;. Applicable Document for soil constants, material passini the No. 40:.l ASTM Standard: (425-jim)sieve is required in total amount of 220E 1 1 SpecificatJon for Wire-Goth Sieves for 8- allocated as follows:Testing Purposes2 - -- Test Grams

Liquid limit 100.V Appantitt PUsuc limii 13V , Bal - balanc. scn tivc to 0. , g. ' " 1 "3.2 A/ortar — A morur 2nd rubber-covered Check tesu 65

pestle suitable for breaking up the aggregationsof soil panicles, 5. Pre anitioii of Test Sample3.3 Sieves— A series of acves/of square mesh 5. j Select that portion of the aiixlried sample

*oven wire cloth, conforming to Specification selected for purpose of tesu and record the massH 1 1 . The sieves required are as follows: as the mass of the toui test sample uncomxted

No. 4 (4.7$-mm) for hygroscopic moisture. Separate the test sara-5J°- *J (2.0p.mm) pie by sieving with a No. 10 (2,00-ram) sieve.No. 40<425-iim) GHn(j lhat fraction 6 on No. ]0 sieve

14 Sampler — A rime sampler or sample split- in a mortar wijh a rubber-covered pestle untilI..T, for quartering the samples. the aggregations of soil particles are broken up

into ihe separate grains. Then separate the. Sampling ground soil into two fractions by sieving with a4. 1 Expose the soil sample as received From No. 10 sieve.

the :1eld to the air at room temperature untildi 'f d thoroughly. Break up the aggregations thor-

in ihe mortar with a rubber-covered pes- „- . - , p , D-18 on Soil and Rock u>4 a the diiw raporuaWiTy ofSelect a representative sample O! the amount SubewnfninctDH 03 oe Tenure. Ptaaiciry.iBd Deaaty Oar-

10 perform the desired tests by the aoerauc* of Sokf quancring or by the use of a sampler. "E S

I he amounts of material required to perform the J AMUO/ Boot of.\$TM Siewiar&, Voimethod of quancring or by the use of a sampler. "ES^'fTST ^ '"''

flR300683

that irac.ton retimed jricr thir •<,.• proximate!) M? g lor sand\ soils and appro**.onO «tf\m$ free o( all line material. Jrv and match 65 | for silt and clay soil for particle-sizeweigh, Record thts mass as in* mass oi coarse analysis.material. Sie\e ihe coarse material after beingwashed and dried, on the No. 4 (4.75-mm) sieve m _ _ ,,,-..,,-... . . v , /. Tesi Samp e for Soil Constantsand record the mass retained on ihe No. -t sieve. /

7.1 Separate the remaining portion of the mar6. Test Simple for Ptmcle-Size Analysis teria, passing No 10 (2.oO-mm) sieve into

6-1 Mi\ the fracrions passing the No. 10(2.00- two pans by.mcans of a No. 40 (425*vim) siev ,mm Isie^e in both seeing operations thorough^ Discard the fraction retained on the No. 40sievttogether, and b> the method of quartering or the Use the fraction passing the No. 40 sieve for theuse of a sampler, select a portion weighing ap- determination of the soil constants.

rv tmfnft* Suorrt tgr Ttatitgw \fatertais tanvt m>?c*ttt<Hi tetptctm ihe mlidav of our pair* nfkts astenfdMtf tx :%i a -wj I'tcnetito* itjnJjrdarrexprtssJi

aitjtttenittr nunrtfri*tw ff utfti nubs* jrrrwifrlvtlirirv**

Tint aanderlu utotri w wit** at MI- urn? M titr r«»ew«Wr tttimeal ttnumatt wirf mug be rmr+rl t*m-jht yttn «2imsed tutor rrtfpn*t* i* •wA*fra»«* >'mr rtwtinwwt are ittvard eithrr far mtjum of ika itlHdarl tr for

<rfA»J*/w«drf'rt»iw JJT.W Htettounm, Your canuntrui +iil rteettt t*re&l amsidimio* m t mttit&n£*t tTMtxttf. »*«* ,n«u nicy afl ntf /f itHrW/iter vnur nMimmr j Aorf not rwrrntf c/flfrAnnnf you

tST V C«mmuf *r on Storfanb. 1916 face St.. f*(/adWp/»«.

D-2.

Designation: D 422 - 63 (Reipproved

Standard Method forPARTICLE-SIZE ANALYSIS OF SOILS1

(•I* jundirf it tfuted under the fixed ''"•ITM""" D 422: the number immedittely foDowini the designation indicate the jtu of£uul adoption or. in thecueof ncvwon. tfje year of tut revmm, A number ia ptmuhcsa ifldicitej the yeu of liA nappnytil.MipenenpteiiiJQa<«)iBdicM8U«ditohaJch«nfe»cc the lan irnnoo or reappwal.

1>S4. _____

I. Scee* the material retained on a No. 10 sieve.I.I TWs method COVCT ihe quantitative d* ** StimagApparatta-Extber appantus A

termination of the distribution of particfe sizes «rB may be used.iff sdib. The distribution of particle SUB bujcr 3-2-1 Apparatus A sfaaH consist of a mecfaan-inan 73 Mm (retained on the No. 200 sieve) » »«0y operated stirrios device iawhicfa a suitably

mwiwm a vertical shaft at

The sbaft sbafl be equipped »nb a tepbceable4.seciNttlieaeeewy<bta<Noieiland2);

.nNt«adofiheNalO.Fbrwfaaiever«eyeuicd,tlieBtt not kss than *uM 19.0 mm) nor more thin IV,

be indicated ia ifae report. in. (38. 1 mm) above the bottom of the dispersionSort 2-Two types of disposon devka are pro- c . A d dispersion cup conforming to^ o'S ^ ^ **« of the designs sbown in F* 2 sM bedevices produce « .more |.pOiiriyt dnperaon provided to hold the sample while it is being

,f plunc soifa bdow the 20- im &ze tad ipprecubf)' dispersed,degradation on all sizes wbeo used with tiody sofls. 3 jj Apparatus B shall consist of an air-jet

upe* of devices differ ia masnitude, depewliai «poo _ « details ibown m FJJ; 3 {Notes 4 and 5).-oil i>pe. teadioi to muird differcoca is p«n£te size NOTE 3— Tbe amount of air required by ao tir-jn.liMMbutiocucspeoally for siza fioer than 20jun, dispenioo eupbof the order of 2 ftVfflin; some smaU

air compressed are oof ctpaNe of supplying sufficient1 Applicable Documents air to opente • cup.

•» I 4 STM Siandardr NOTT *~ Anotber «f-*yp« dispenwo device,^ , ,i: ,: r L ^ , «. -. t"0*0 « » disperson tube, devdopcd by Chu andD42I Method for Dry PrepaiatiOD of Soil D«v»d»n at lo*i Stti* CoUeje, DJD been shown to fiveSamples for Particle-Size Analysis and De- ^ . _

"t 1 1 Specification for Wire-Goth Sieves for D-II « Sod UK) ««t sod •Testing Purposes1 - - SubewnnuneeDI 1.03 ooTcnu«.n*socrty. and OwwtyClar-

P. 100 Specification for ASTM Hydromeiers' aaS£!'*£ii •porwd Nov. jj. 19*3.fahed !«5. Rrpfaco D<22-«.

V \ppantm ' WHa/AMt X TV dnd . Vol^OC.1 Mkd/ AM* of ASTM Slander*. VoJ 14.02.3.1 Balances— * balance sensitive to O.OJ j • Annual B<X* of ASTM Standard}, vat MOI.

i." v»trighing the materia] passing a No. 10 (2. CO- 'Druikd wtxtini dnwinp fo. iha csp_,- >•• •.• . A i a- j- ooraiuJ cos from ihe Ammcu Sanrry far TCBUC ind MX-mm) sieve, and a balance senauve to O.I % of tcmh> ,,,6 R phj p PA ,,,0j.

the mass of the sampk to be weighed for weighing Na i:-*o*2aw».

flR300685

*§.' D422

results equivalent to those secured t>> the air-j« duper- temperature. the water bath is not necessaryuon cyps. When « is a«d. soikin* of ihe umpie CLT 33 Beaker— A twaker of 250-mL capaci'tv.bedonem the wdimenution cylinder. thuiciimmatia^ 1Q T .„ -^ /-!«•„-„ 4 „ ,, v, ~, ~i _ L '.wthe need for umnsTeffiifc the duny. Wh« ^ „'. 3-? *-?'"""* Oni«-A *atch or clock with tdispersion lube a used, it shall be so indicated in the second hand.report. _Soil 5— Water ma> condense in air tines when noc 4. Dispersing Agent

,* me. This waier must fee removed, either by us, n, a 4 j A , • f h phosphatewiier trap on ihe air bae, or by blowing the waier on: : .- - , . - f <" "**of the tine before uuns any of the *r for disperuoo {sometimes called sodium meia phosphate) shallpurposes, be use<J in distilled or demineralized water, at the3.3 Hydnmaer-** ASTM hydrometer. rafle °f *° « °f ^ hexameiaphosphate/litre

graduated to read m either specific gravity of the of solunon tNote 7)' .suspension or grams per litre of suspension, and NoT* '-Solunons of this ait, if acidic, slowly re-ccnic ms « , fte ui«men« for hyd.ornc r SStST 2 'SSSrSS! 115 1H or 152H m Specifications E 100. Dimco- j^d te prepared frequently (ai lean once t month)sions of both hydrometers are the same, the soi; or adjmied to pH of 8 or 9 by means of sodiumbeini ihe only item of difference. cart-onaie. BonJes containtn* soJuuons should havt the3.4 Sedimentation Cylinder- A glass cylinder **•* of P P tion " ^ «» *«"•

essentially 1$ in. (457 mm) in height and 2'/: in. 4.2 All water used shall be either distilled or(63,5 mm) in diameter, and marked for a volume demineralized water. The water for a hydrometerof 1000 mL The inside diameter shall be sucfa ten shall be brought to the temperature mat kthat the 1000-mL mark is 36 * 2 cm from the expected to prevail during the hydrometer Kst ;bottom on the inside. For example, if the sedimentation cylinder is to3 J Thermometer— A thermometer accurate be placed in the water bath, the distilled or de- -

to 1*F (0.5"C). miheraiized water to be used shall be brought to •3.6 Sieves— A series of sieves, of square-mesh the temperature of the controlled water bath: or, *.

wcvea-wire doth, cooforminf to the require* if the sedimentation cylinder is used ia a room;ments of Specification E U. A full set of sieves with controlled temperature, the water for theincludes the foDowint; (Note 6): ten shall be at the temperature of the room. Tot- i~]

S-UL C75.mm) No. 10 (lOO-mm) *»«c temperature for the hydrometer test is 68T " j2-in. (50-ram) No. 20 (!5<Him) (20'Q. Small variations of temperature do not

(37.5 nm) No. 40 (425-um) introduce differences that are of practical sign*

No. 200 (75-jun) derived as prescribed,No.4(4.75-aun) 5. Test Sample

,-anaJ>-us as outhned in Method3-ia. (75-ram) No. 16 (LlS-mm) the preparation procedure the sample is divided1%-im. (37.5-mm) No. 30(60CHimi into two portions. One portion contains onty%-ia. (19.0-mm) No. 50 (300- m) particles' retained on the No. 10 (2.00-mm) sieveH-ia -(9.5-mm) No. lOO(15(Him) whi!e lhc other 0* contains only partida;No. 4{4.75-min) No. 200 (73-sim) . . vr 7T . _, e - i - ^ tNo, S (2.36-mm) passing the No. 10 sieve. The mass of air-dned.

„ , „„ ^ , - _ soil selected for purpose of tests, as prescribed Jt3.7 Vteer Bcih or Constant emperoa Method D 42l. shal] be sufTldcnt to yield quin,ocm-A water bath or constant-temperature unes foE raechanical inalysis „ fo!lows

room for mainoimnt the soil suspension at a s j , ^ flf n ^ Qn constant tempeniure dunng the hydromctrr NQ ,Q f d on m^mum analyas. A satisfactory water unk >s an insulated fl f ,e> accordl to foi]owing ^^tank that maintains the temperature of toe sus-pension at a conventeni consunt temperature at ^ S. App«um.« Miningor near 68"F (20"O. Such a device is illustrated in (mm) Mia of Ponxja. tin Fig, 4, In cases where the work is performed s (9 5) soo

1000

flR300686

<Sff! 0422

Nomuui Dumrter HYDROMETER AND SIEVE ANALYSIS OFoflutat Pinwtei, Apprqiimate Mm.mum PORTION PASSING THE NO. I0(2.00-aun)

in. fram) Mm of Portion, f SIEVEI I25-4) 2000 . ^ - - - - - „ _ID (3i.i> 3000 -7. Determination of Composite Correction for2 (»«) «oo Hvdromttef Readlnt3 (7«J) 5000 - . , . . ,"J Equations for percentages of so3 remain-

5.1.2 The size of the portion passing the No. ing in suspension, is given in 14.3, are based onin sieve shall be approximately 115 g for sandy the use of distilled or deminenlized water. Avwls and approximately 65 g for silt and dty dispersing agent is used in the water, however.Miils. and the specific gravity of the resulting liquid is5.2 Provision is made in Section 5 of Method appreciably greater than that of distilled or de-

, > 42 1 for weighing of the air-dry soil selected for mineralized water,. urpose of tests, the separation of the soil on the 7.1.1 Both soil hydrometers are calibrated at\a 10 sieve by dry-sieving and washing, and the 6ST (20*O> and variations in temperature from»otiiing of (he washed and dried fraction re- this standard temperature produce inaccuraciesttiined oo the No. 10 sieve. From these two {•the actual hydrometer readincL The amountmasses the percentages retained and pacing the of the inaccuracy increases as the variation fromNo. 10 sieve can be calculated ui accordance the standard temperature increases.with 12.1. 7.IJ HvdTomeimaregjadwttdbytheman-Nrm I— A check oaiaeatttf vitas and Aeraor- v&ctuicr tobe md at the bottom of the aeao-

cue formed by the Squid on the Stem. Since k *aotpon to tcnire reading of sofl suspension*

SIEVE ANALYSIS OF POVT1ON RETAINED 7.IJ The net amount of the unjcaiuas lorON NO. iff <2jft-u) SIEVE tr« three hems enumerikd is designated as the

composite correction, and may be determined*. Procedure experimentally.6.1 Separate the portion retained on the No. 7.2 For convenience, i graph or ubie of com-

l(J(2.00-mm)sieve into* seriesof fractions using posite corrections fora series of 1" temperatureihe 3Hn. (75-mm), 2-in. (50-mmX I'A-in. (37.5- differences for the range of expected test lemper-mm), I -in. (25.0-mroX %-in. (19.0-mmX H-tn. atures may be prepared and used ts needed.(9.5-mmX No. 4 (4.7$-mm), and No. 10 sieves, Measurement of the compos ts oorrectkms mayor as many as may be needed depeadi&i on the be made at two temperatures spanning the rangesample, or upon the specificatioDs for the mate- of expected test temperatures, ind correcoom forn;il under ten. the intermediate temperatures calculated assvm-6.2 Conduct the sieving operation by means ing a straight-line relationship between the two

:if a lateral and vertical motion of the sieve, observed vilues.accompanied by a jarring action in order to keep 7.3 Prepare 1000 mL of liquid composed ofihe sample moving continuously over the surface distilled or demineralizod water and dispersingof the sieve. In no case turn or manipulate frag- agent in the same proportion as wQ] prevail inmerits in the sample through the sieve by band the sedimentation (hydrometer) test Place theContinue sieving until not more than I mass % liquid in a sedimentation cydiader and the cyf-of (he residue on a sieve passes thai sieve during inder ic the constant-temperature witer bath, setf min of sieving. When mechanical sieving is for one of the two temperatures to be used. Whenuvd. test the thoroughness of sieving by using the temperature of the liquid becomes constant,itv hand method of sieving as described above. insert the hydrometer, and. after a short interval

ft.3 Determine the mass of each fraction on * to permit the hydrometer to come to the tmper-Mance conforming to the requirements of 3.1. alure of the liquid, read the hydrometer it theAI ihe end of weighing, the sum of the masses lop of the meoiicus formed on the stem. Forrvciined on all the sieves used should equal hydrometer J51H the composne cx>rrecrJoo H theiltncly ihe original mas of the quantity sieved. difference between this reading and one; for by-

< h 0422

drometer if^H it is the difference hct*«r the ^.? Place the co\cr cap on ihe cup and openrcidm| and zero Bnng the liquid and the h>- the air control \al\e unul ihe gage pressure is 20dromcter to the other temperature 10 be uwd, psi ( UO kPai, Disperse the soil according to theand secure the composite correction as before. following schedule:

8. Hjgroscopic M*n» ^ ,„„„S.I When the sample is weighed for the h>- t'mfcr J s

drometer test. *eigh out an auxiliary portion of 6 10 w ___ . 10from 10 to 15 | m a small metal or glass con- ^ **" M ISlamer. dr> the sample to a constant mass in an Soils remaining large percentages of mica needoven at 230 = 9*F (1 10 ± 5"C). and *eigh again, be dispersed for onl> 1 mm. After the disperaoaRecord the masses. penod. reduce the gage pressure to t psi prepar-

atory to transfer of soil -water slurry 10 the sed-9. Dispersion of Soil Simple imentation cylinder.

9.1 When the soil is mostly of the cla> and siltsizes. »«jh out a ample of air-dry soil of ap- 10. Hydrometer Testproxim«el> 50 g. When the soil is mosU\ sand IQ.I Immediately after dispenion. transfer thethe sample should be approximately 100 g. soil . water slurry to the glass sedimentation cyt9.2 Place the sample in the 250-mL beaker jnder. and add distilled or dcmineralized wttet

and cover «.ith 125 mL of sodium hexameia- untii the total volume is 1000 mL.phosphate solution (40 g/lX Stir until the soil is 10.2 Using the palm of Uw hand overthcopet-thoroughly wetted. Allow to soak for at least 16 end of the cylinder (or i rubber stopper in theh. open end), turn the cylinder upside down and9.3 At the end of the soaking period, disperse back for a period of 1 min to complete the

the simple further, using either stirring apparatus agitation of the slurry (Note 1 !). At the end of 1 ,AocB. If stirring apparatus A is used, transfer min set the cylinder in a convenient location and'the soil - water slurry front the beaker into the take hydrometer readings at the following inter..special dispersion cup shown in Fig. 2, washing vah of time (measured from the beginning trf-any residue from the beaker into the cup with sedimentation), or as many as may be needed,dialled or detnineralized water (Note 9). Add depending on the sample or the specification Cardistilled or deminenuozed water, if necessary, so the material under test: 2. 5. 1 5. 30. 60, 250, andthat the cup is more than half full SUr for a 1440 min. If the controlled water bath is used,period of 1 min. the sedimentation cylinder should be placed m,Norc 9— A laiae size syriaae is a coovtmirat device the bath between the 2- and 5*min readings.

94 If stirring apparatus B (Fig. 3) is used,

A air gage must be on the line between the cup 10.3 V/hen it is desired lo take a hydroroetrfand the control valve. Open the control valve so reading, carefully insert the hydrometer about &that the pie indicates 1 psi (7 kPa) pressure to 25 s before the reading is due to approximate(Note 10). Transfer the soil - water slurry from the depth it will have when the reading is ukethe beaker to the air-jet dispersion cup by *-ash- As soon as the reading is taken, carefully remove;mg with distilled or demineraJized water. Add the hydrometer and plact it with a spinningdistilled or detninerajized water, if necessary, so motion in a graduate of clean distilled or derniSthat Ihe total volume in the cup is 250 mL. but eraJized water. '_"'no more. _ NOTE 12— It n important 10 remove ihe hydromcarNOTE 10 — The initial air prasurc of 1 ps is required imme4iafci> after each readint Reading thai! be lake*

to pnrvem ihe vxl- water mixture from emcno$ ihe ai die top of the meniscui formed by ihe suspenao*ur-jet chamber »hco the mixture a transferred to the around the siern. nnce il ts not posufak 10

readings at ihe bonom of ihe mentscus.

t.

flR300688

* . <> 0422£-

iO.4 After each reading, uke the temperature tion factor../ the suspension by inserting the thermometer 14.2 Calculate the mass of a totaJ sample rep-,;uo the suspension. resented by the mass of soil used in the hydrom-

eter test, by dividing the oven-dry mass used byII. Sieve Analysis ^ percentage passing the No. 10 (2.00-mm")

11,1 Aftrr taking the final hydrometer read- sieve, and multiplying the result by 100. Thising. transfer the suspension to a No. 200 (75-jim) value is the weight W in the equation for per-steve and wash with tap water until the wash centage remaining in suspension.»aier is dear. Transfer the ma_tc=riaJ_op. tie No, 14.3 The percentage of soil remaining in sus-200 sieve to a suitable container, dry in an oven pension at the levd at which the hydrometer isji 230 ± 9'F (1 10 ± 5*Q and make a sieve measuring the density of the suspension may bejnaiysis of the portion retained, using as many calculated as follows (Note 13): For hydrometerMcves as desired, or required for the material, or . 15IH:upon the specification of the material under test /- [(100000/HO x G/{G- <?,)** -<7,)

CALCULATIONS AND IEPOKT NoTt '*"• *** bucketed portioa of the •qwboafor hydrometer I51H is constant fcr « stria of mdiati

12. Stew AmSyA Vatoes tor the Pwta *****atotoe?** tad then cutepfad by U*._

J2.I Calculate the percentage pairing the No, wwter I52R*

sieve by ine ma* of soil oriajnaDy spfc o* the when:No. 10 siei*. and multiplying the result by 100. a -conect»factk» to be applied to the read-lo obtain the aaau pasting the No. 10 sieve. ii* of hydrometer 152R (Values shown onsubtract the man retained oa the No. 10 sieve the scale are computed using a specific gw-from the original mass. jty of 165. Correction deters are given in12.2 To secure the total mass of sofl passing Table IX

i he No. 4 (4.75-mm) sieve, add to the mass of P • percentage of soil remauuncJn suspensionthe material passing the No, 10 sieve the mass of it the level at which the hydrometer mea-ihc fraction passing the No. 4 sieve and retained SUITS the density of the suspension,on the No. 10 sieve. To secure the total mass of R - hydrometer reading with composite correc-soil passing the H-in. (9.5-rom) sieve, add to the tion applied (Section 1\"-nai mass of soil passing the No. 4 sieve, the . W * oven-dry mass of soil in a total test samplemass of the fraction passing the H-in. sieve and represented by mass of soil dispersed (seeretained oo ihe No. 4 sieve. For the .remaining 'l4.2Xg.sieves, continue the calculations in the same G *• specific gravity of the sou" parddes, andmanner ; " " G\ * specific gravity of the liquid in which soil

12.3 To determine the total percentage pass- paiticfes are suspended. Use numericaling for each sieve, divide the total mass passing value of one in both instances in the eqoa-»ee 12.2) by the total mas of sample and mui- tion. In ue first instance any possible vari-uply the result by 100. . ao'on produces DO significant effect, and in

the second instance, the composite conec-13. Hygroscopic Moisture Correcrfoo Ftctor tion for Jf is based on a value of one for <?,.

J 3. 1 The hydroscopic moisture correction fac-lor is the ratio between the mass of the oven- <5- Diameter of Soil ParticlesJn^d sample and the air-dry mass before drying. 15.1 The diameter of a panicle corresponding[i is a number less than one, except when there to the. percentage indicated by a given hydrome-" no hygroscopic moisture, t£r reading shall be calculated according to

Siokes* law (Note 14), on the basis that a particleI J. Percwtt«« of Soil la Sospeasioo of this diameter was at the surface of the suspen-

14.1 Calculate the oven-dry mass of soil used son at the beginning of sedimentation and had•n ihe hydrometer analysis by multiplying the settled to the level at which the hydrometer isjir-dry mass by the hygroscopic moisture correc- measuring the density of the suspension. Accord-

AR3D0689D--7 - "

(jfi 0422

mg to Stoics' Ia*: fraction that *ould ha\e been retained on theCi)J * Uf ' No. '0 sievc na !t no1 °«n removed. This mass

is equal to the total percentage retained on the, No, lOsicveUOOmmustoulpercentagepassme)0 -diameter of particle, mm rime$ the mai$ flf lo(aj ,e reprtsentfid

n - coefficient of viscosii> of ihe suspending fav the ma&s of ^ (as ^ in ,4 2lmediamdntniscase water) in poises (vanes ^ the fewlt d dffj bv [(X)with changes m temperature of the sus- ^ QJ ^ next J,e tou| mass p ^ ^pending medium}. . N o . 200 sieve. Add together the fractional masse*

L - distance from the surface of the suspension reumcd Qn al, ^^ indudi ^ Nto the level at *h,ch the density of the sicve ^ ^ m ffom ||w masssuspens.cn IS being measured, cm. (For a wta] samp)e (as ^ ^ in ,4 2)>p,en hydrometer and sedimentation cyl- ,6<3 Calculate next the total masses passin,inder. values vary according to the hydrom- aeh rf l|w olher Hev<Si in a mannfir simiUr eter readings. This disunce is known as ^ ^ in P 2effective depth (Table 2)). 16.4 Calcula'te'last the total percentages pass,

7 -mtervalofumefromtejinrungofsedirncn. ing dividing thc mass passing (as calcu-tatjon io the taking of the rcadiai, nun. ,atcd in ,6J) ^ toul ma$s rf fe (

C? -speafic gravity of soil particles, and calculated in 142) and multiply the result bvG, «• specific gravity (relative density) of sus- IQO ""

pending medium (value may be used as1.000 for all practical purposes). 17. Graph

Son 14—Since Stt*«' law cotuiden ihe terminal 17.1 When the hydrometer analysis is per.velocity of a anjtesptocCi&niin aa infiniryof liquid, formed, a graph of the test results shall be made,tiuttw a H /a neM Se'S nicS"0 PIotlin* &* diameters of the particles on a loga-

rithmic scale as the abscissa and the percentages15.2 For convenience in calculations the smaller than the corresponding diameters to am

above equation may be written at follow* arithmetic scak as the ordinate. When the tyD - KJUf drometer analysis is not made on a portion of"

the soil, the precaution of the graph is optional."instant depeoding on the temperature of f"« **« "»* ** *<*"«* direclly *""* " 1the suspeosioo and the specific gravity of 1*led dau- Ithe soil putides. Values of K for a range of ig. Report

18.1 The report shall include the following: : ]18.1.1 Maximum size of partides, [ {18.1.2 Percentage passing (or retained OBI)

T/""4 n *"""LJ ™"Y,li %u f each sieve, which may be tabulated or presematValues of D may be computed with suf- . _;MM. .J./vi«* i«\ f).. ,-. ... by piotting on a grapo (Note lo),accuracy, using an ordinary I0-in. sade *. - _ ,*\-- . . . . . . ' tcles:

Nori IS-The vajue of L is divxicd \* Twint the , 8 , 3 , Shape-rounded or angular.A- aod J-*cate, ibe square root beinj mdiate4 on ihe _ ,, ,, _ . _ . , , j* ui. „„» j;O-iok. Without ascsruininj the value of the square ' 8- ! -3-2 Hardness-hard and durable, soft, atroot it may be rautaptel by It usinj either tbe C- or weathered and friable.C7-*aie. 18.1.4 Specific gravity, if unusually high at

low.16. S«ve An*J>sis Values for Portion Finer than , g j 5 Any difrICuhy in dispersing ihe fractiom

No, 10 (2.00-mm) Sieve passing the No. 10 (100-mm) sieve, indicating16.1 Calculation of percentages passing the any change in t>pe and amount of dispersinc

various sieves used in sieving the portion of the agem. andsample from the hydrometer test involves several 18.1.6 The dispersion device used and the*steps. The first step is lo calculate the mass of ihe length of ihe dispersion period.

f

D-a."flR300690

- <f[f! 042 . --

NOTI If*— This ubuiauon of graph represent ihe MI Clav iize. smaller than 0.005 mm <~,•jjjtion of ihe ample lesied, If panicles larger than Colloids, smaller than 0,001 mm <-,

, Mje contained rn tne sample *ere removed before,.x»ng. ihe report shaJI so stale giving the amount and 18.4 For materials for which compliance withnuvimum sze. - defimie specifications is noi indicated and when

1 8.2 For materials tested for compliance with th? wil "nUJnS matfrial re*ined °,n lhe No' 4icfiniie specifications, the fractions called for in S'CVC suffi™m 1°,ftquirt f SICve ana 's On,uch specifications shall be reported. The frac- {J ?" mul14 may fCpOrted *uons smaller than the No. 10 sieve shall be readrum the graph. Sim ANALYSIS

1 8.3 For materials for which compliance with,,; finite specifications is not indicated and when ^. ;c soil is composed almost entirely of particles 2.,

the No. 4 (4.75-mm) sieve, the results J*>in.from the graph may be reported as follows: ,'-'nGravel passing 3-i». and ntamedoe •No. < sieve • ' • ' * No. 4 (4.75-mm)

Sand. Btntni No. 4 lieve and rr- . No. 10 (2.00-rara)taJMdoa No. 200 sieve ""• * No.40{425nm»

andRiainedonNo.lO«ievcMedium sand. pOBnf No. 10s«v« and mtined M Mo. 40 -.W*V - jh f \m **

(,•) Fine stnd. pttsJOf !*>. 40 sieve . u'roi mmand retained oo No. 200 sieve ' " Non 17— No. 8 (2.36-mm) and No. 50

Sill size. 0.074 10 0.005 mm . ... )E sieves may be substituted Tor No. 10 and No 40 sieves.

D-9 flR30069

I\B!L I \«I«

SpeeifK Uf

2.95:i?:so» --j^ "X)26S2eO2.55250: 5

•« of Corrwwfl ftn«. a. fof Dirtcrri-ic Gnittm of >io«l P«r6cln*

*«> Ccrrraion r ior1094

0%09709Jo.wIX10110:103io«

<£> D422

1 \81 t : tonlmurd

.. H .mct

\CIU4lH \drom-

etcrReadmi

,O.Ht 0'2I 03.1IO.U

"JV H ..Hvdv^mM-H

PJ» H\- EfTev- Hv-~ drum- . ii\e dram-i ' nrf Depth. eier

Read- Lzm Read-ing inf

it I'9"t _._-• ;

--

Effec.live

DeptrtL. cm

'For use in equation for prrcenuff of »ii remain; :B '. U*~ t«sen uiini Hydrometer I52H 1 u.l8 62

* t aiun of eiTniixc depth are calculated from ihe equiooa.TABLE 1 Vth*n «f Eff cti** Dcytk i«*H a* H»4™«wwf

,~. K1U U^l———.—^ 1<>U »n*Tf,

,4 • eflitflive depth, cm, _ _Li • dnuncr *lon( the nem of the hydiometer from the top

of the bub 10 the mirk for • hvdrometer reading, cm.L- • otenii lenfiti at the hxdrorneter bulb. em.

KvdremetmSlH Hyd«»nct« 152H

ActuilHjdrora-

Kodinc

IhOOO1.0011.002I.OD?1.00*1J»5

1.00*1.0071.00*1.0091.010

101 11.0121.013L0141.015

1.01*1.0171.01X1.0191.020

1.0211 0221.02310241025

10261027io:x1019I 030

ESrtie1M15 J15 2ISA

14.714.414.213.»13.7

13.413.111912.*113

12.111J11.511J1IJ)

tO.710510.210097

9*92S9IbS*

AetuaJHy-dram*

Reri-

12345

«7S910

1112131415

1*17111920

2122232425

2627:i^JO

Effir-u*e

i-cm

It.llt.0ISJISAISJ

15 J15JIS.O14.S14.7

14.5I4J14.214.0

. 13J

13.713J13J13 213.0

11912.712.512.412.2

120tt 911 711-111 4

ActualHy-dront'

Rad-'•f

32333435

3637313*40

4142434445

4447a4950

515253<4

«

K17S£!960

Enec-a*e

n..I0.i10."10*

10410J1019*»"

9.f9.4»J9 1S.9

s.s*.*14IJ1.1

'91,1"6'4" ?

-I"06 f6fr»_»- -

4 • craa*iertioR>] »• of iediinenuitoa e>hnder. em1VaJua uied m aletdiunf the viiua m T»We 2 are K feUovcFor boOi Kydiarneien. !5lHudf? "'• "

For Irjdrorarm IMH^ * 10.5emfociradimo/0tl«re

- i3 cm ferirodini of Mi/litre

D-1.0 flR30CT692

©J 0422

T\BLL J \*lt»r» at A foe I tt in E upttoa (or Covpvnut DtMetef et Pvtxie In Hrdroeetrr Axufjsh

_ . Specific Cra*'

Ll

•ri<,1718jq:o:i2223242?,4272129JO

:.4*0,015100.015 II0.0149:0.014740.014*6

0414310.01421-04140*0.0 13M041372

0.013)70413420413270.01312041291

150.0.01505Q.OI4S60.014670.014490.01431

0.014140.013970.01 3110413650.01349

0413340.013190.01304•41290041274

- ,245O.OMSI0.014620.0 144J04142J0.01408

0.013910.013740.013510413420.01327

0.013120412970.012*3041269041254

=. .2 JO.O.OM57

, 0.01439OOM2I0014030.01JS6

0.013690.013530.01337o.o 1 3:10.01306

0.012910.012770012*40.01249041234

2,65.0.0 J 4 350.014170.013990.013820.01365

0413410413320.013170.0 1 3010012*6

0412720412510412440.012300.01217

-, 2.70

O.OH140.01396O.OI37S0413610.01344

0.01 3210413120.01 29'04i:i:041267

0412530.0 111900125*041212041199

2.750.013940,013760.013590.013420.01325

0413090412940.01279041264041249

04(2350412210.01201041195041 112

2.M0.013740,013560.013390.13230.01307

04I29I0.01276041261041246041232

04121*041204041191041 17|0411*5

2.150,0135*0.013380.013210.0130.'041219

0.012730412510.012430412290.01215

0412010.01 IW041 17501011420.01149

Cnromt Ptottd

0.203'io.oo)

1(a)

0.001 0049 OJ03 .. *t - "«.0.03 1-24 5.16 IJ.T J9.0

FIG. 1 DMall of Scirr f rSMki

SR300693

0422

IJ 2.* 3.7533 6* 95.2

FIG. n

D422

1 ...t

D __I jji i

_rfit ——————— !_ _ ————— ^ ———— w-iBiUSiii-,

•0.

zjz.: tl

T,i

?

ii;

•s\

*

*

f--

3.

—r — •— --i

ii

5

'*>,"*T

—- (Scrtc/t/zetf JAsn1 Mefaf— J — j ——— *

—— 2 'Cor*

trnw-flto/ff

*w«*uAbw — «f- — ——

il1 3 * ' . 1 4 3 7

254 ?6J 15(12 33* 940

FIG. 4

'w riii yanjs'G L 'Hrsrttiut tiandatd are <.'\f*fi<k athniM ifal dttcrmuwumtxikc voltduvtXoni stun•. !.•*/< andtfcnsl. ofmfanftmcm of sur* rtfias. are ennreiy thinr ,,»

is suhftn to neauiM ji any tmr r>r /A rfspotiittiie itthmtai cfltnms:iff and majr jr wmtd ntrvfyf vw»n astf-ctf rt/At-f tfopprtncd of H.'/W'axw >'OKr tnminrnt) are tn\ncJ either tor mmnn & ihu, uandiira ew far addaww'

• jnd sfifu/i/ /v add'ruea to lS7\\f Hfaaguarters Your ttimmfrai HV// rnwf care*u/ fdrsideraiim a: a meninf a! theT tn'finiijj wmmitife n^icfl irt/ mav J/rrnJ //" tew fct-i.lAai \-our spwye .tuiie nor rKt;\cd j fair Htar\r\s you ihiHt.j,r .ie*.\ */ii^»n ifltae AST *•! Committee \"i Standards Wl 6 Race Si f . a nia fa

D-l flR300695

Designation: 0 4318 - $4

Standard Test Method forLIQUID LIMIT, PLASTIC LIMIT, AND PLASTICITY INDEX OFSOILS1

njjftl i* niuni under itw ii\«J drupniuon D43t* the numta immediateK folio* mj the dni(nitian indicates ihe >ear of. jj>>f»t»t>n « m thr cue of trttyon. Uw ytir oTtwcMuon \ number m parentricsn indicate! itw >ar of last reappfo\aJ_

*! indicate. an nhtonai ttunir unct the Ust rcviuonor mpproval.

t -scope 1.1.3 The procedure for calculating the plas-l This tesi method covers the determination ticity index is given in Section 19.

-r'Kliqutd limit, plastic limit. *nd the plasticity 1-2 The liquid limit and plastic limn of soilsP.W of was M defined in Section 3. (along with the shrinkage limit) are often coilec-

t . l TUQ procedures for preparing test spec- ti vely referred lo as the Atterberg limits in rec-.».ns and two procedures for performing the ognition of their formation by Swedish soil sci-... id limit are provided as follows: «*»*• A- Atterberg. These limits distinguish the

Multipoint test using * wet preparation boundaries of the several consistency sates ofprocedure, described ia Sections 10.1. U, P»a«ic soils.aoa* 12. 1.3 As used in this tea method, soil is any

/* Multipoint left usinc a dry preparation natural aggregation of mineral or organic matt-procedure. described in Sections 10.2. 11. rials.mUturesof$uehmaterials.oramrkialmix-aixj 12. tures of aggregates and natural mineral and or- "

< One-point tea using a w« preparation pro- pnk particles. Jcedure. described in Scctkxu 13, U. and 1.4 The multipoint liquid Emit procedure is15. somewhat more time consuming than the one- , --,

/; One-point test using a dry preparation pro- point procedure when both are performed bycedure, described in Sections 13, M, and experienced operators. However, the one-point J15. , procedure requires the operator to judge when

The procedure to be used shall be specified by the test specimen is approximately at its liquid -jiV requesting authority. If no procedure is spec- limit. In cases where this is not done reliably, the

Procedure A shall be used multipoint procedure is as fast as the one-pointprocedure and provides additional precision due

1— Prior to u*e adoiKioa of ibis tea method, to the information obtained from additional ]****** wjpwfiod aa ,P"t * «j* trials. It is particularly recommended that thefor perfonntnt the liquid Umrt test. The , • • , u j . _ -tool s not considered u be u xruraie *s the multipoint procedure be used by inexperienced

' uxrt described ia 6.2 sura ft does not controi the operators.-nn of ihe s»Hn Use liquid limit cup, However, there 1,5 The correlations on which the calculationsvmf dtta which mdiatc tfa« mjicaJJy ihe bquid of lhe one.pojnl procedure are based may not be

is sliritUv increased when the fiat tool is used ... , . ., . ,.--M of Secured tool. ^ for wrtain SP'1*' such «* or anjc ™l* or

soils from a marine environment. The liquidi 2 The plastic limit test procedure is de-

_ __- . £ i i __j »e TV.. ~],«. ' Thn tca'iwihod u under ih« junjdietiofl of ASTM Com-in Sections 16. 17. and 18. The piasuc J'TIH icn is performed on material prepared for SutxQmmitt«r ois.03oa Teirure. Piuuciry *«J Denary Ow"x liquid Umit test. In effect, there are two w™1**.0 *- _^_ ., IMJ . "_ . "

_; . - , Currcni etfiiion tppn)v«J Oct 26. 1914 Published DecemberP'-MTdures for preparing test specimens lor ine ,qi4 ontuuihpuWuh«Ji»D 4311-13 Ua P«TX>OUI ediuon;" i-tic limit lest.

D-U: flR300696

L

<SIf> 04318

limit of" these soils should ihercforc.be deicr- D r>5.; Terms and Svmhols Reijiing 10 So,,mined b\ ihe muinpomi procedure (Procedure and Rock Mechanics4M. - . D 124! Specification for Mau'nals lor Sod

t.6 The liquid and pfasiiclimits of man> soils Aggregate Subbase. Base, and Surfr^thai ha^e been allowed 10 drv before testing ma> Courses'he con$iderabl) different from values obtained D 2216 Method for Lahoraior> Deierminaiioeon undned samples. If the liquid and plastic of Water (Moisiurc) Content of Soil. Rod.limits of soils are used 10 correlate or estimate and Soil-Aggregate Mixtures4the engineering behavior of soils in iheir nat.ural D 22-iO Test Method for Rubber Property-moist slate, samples should not be permitted 10 Duromeier Hardness'drv before testing unless dau on d_ned samples D 2-437 Test Method for Classification of Safeare specificallj desired. for Engineering Purposes*

1.7 The composition and concentration of D -488 Practice for Description and Identifi.soluble salts in a soil affect the values of the cation of Soils (Visual-Manual Procedure;*liquid and pUstic limits as welt as the water D3282 Practice for Classification of Soils tadcontent values of soils (s« Method D22I6). Sotl-Agtrefaie Mixtures for Highway Cot-Special consideration should therefore be given struciion Purposes4to soils from a marine environment or other E 11 Specification for Wire-Cloth Sieves fasources where high soluble salt concentrations Testing Purposes*may be present The degree to which ihe salts E 319 Methods of Testing Single-Ann Bat-presem in these soils air diluted or concentrated ances*must be given consideration if meaningful results E 898 Method of Testing Top-Loading. Q.are to be obtained reel-Reading Laboniorv Scales and Bat

1.8 Since the tests described herein are per* ances*formed only on that portion of a soil which passes .the 425-um (No. «Q) sieve, the relative contri- 3- D™****bution of this portion of the soil to the properties 3.1 Atterberg limits—originally, seven "limaof the sample as a whole must be considered of consistency" of fine-grained soils were define!when using these tests to evaluate the properties by AJben Atterberg. In current engineering usage.of a soil. the term usualh refers onl> to the liquid link

3,9 The values staled in acceptable metric plastic limil. and in some references, theunits are to be regarded as the standard. The age limit.values given in parentheses are for information 3.2 consistency—the relative ease withonly, a soil can be deformed.

1.10 This standard mav invoke hazardous 3.3 liquid limit fLL}—lhe water content, nmaterials, operations, 'and equipment. This percent, of a soil ai the arbilrarily defined bouaistandard does not purport to address ail of ihe ar> between the liquid and plastic states. Tt»safeiy'probiems associated with its use ft is the waier content is defined as the water content*responsibility of whoever uses this standard 10 which a pat of soil placed in a standard cup aitconsult and establish appropriate safetv and cut by a groove of standard dimensions will flothealth practices and determine the applicat>i/ny together at the base of ihe groove for a disuaaof reg:i/a!or\-limitations prior to use. of 13 mm ('/: in,) uhen subjected to 25 shod*

from the cup being dropped 10 mm io a staadjd1. Applicable Documents liquid limil apparatus operated at a rate of!2J ASTMStandards i J V" - ;>« per.second, -CIO: :Methods for Reducing Field Samples of ". . - . . - - -

Agpregaie to Testing Six? " " - ; ,,>< v5n/j™ . v0icuo:D 75 Practice for Sampling Aggregates ' innwi a** of TH Sianjjrdi. vob CM o:. 0* 03.D 420 Recommended Practice for Invesugat- w?8 ,_ . _... . , ,,.,,,,.,,_ ,. _ , , _ , , _e^, ' Innsuii S,fl. Of 4$7U Siaiutanii. VolCUOS

mg and Sampling Soil and Rock for Enp- > <*/,mi a,*t oUSJUSiow'di. v0i 0001neenng Purpos«* - * m* &»>* & 57W Siawa, v<ji \t o:

D-15 SR300697

\..i» :~7heundnunedtfwar«renfihofioiUuhtf 4,3 The plasncit} index is calcujated as the.....a nmn is considered to be : =0.: kPa to :s JBII. difference between ihe liquid limn andlhe plastic• -i piti\nt limn f?£j—the water content, in l|m11-

vrccrit. of a soil at ihc boundary between the . „. ._ ...:.o<uc and bntile states. The water content at 5' Significance «d tw(UN boundary is the *ater conient at which a soil 5.1 This lesl method is used as an integral pan.an no longer be deformed by rolling into 3.2 of ***»! engineering classification systems to-m ('/» m.l in diameter threads without crum- characterize iherme-irainedfractionsofsoilstsec.hn?. Test Method 0 2487 and Practice D 32821 and' 5 plaan soil—a soil which has a range of K> specify the fine-grained fraction of construe-

»..tcr conient o\er which it exhibits plasticity lion materials (see Specification D 1241). The.iui *hich will retain its shape on drying. liquid limit, plastic limit, and plasticity index of

J fr ptaancay index W>—the range of water soils are also used extensively, either individual!)...mem o\er which a soil behaves plastically, or together with other soil properties to correlateNumerically, it is the difference between the liq- with engineering behavior such as compressibil-uiJ limit and the plastic limit «y- permeability, compacubility. shrink-swell.3" liquidity m<fev—the ratio, expressed as a and shear strength.

.vrcenute, of (/> the natural water conient of a 5.2 The liquid and plastic limits of a soil canMI! minus its plastic limit, to (2) its plasticity be used with the natural water content of the soiltmjex. to express its relative consistency or liquidity3.8 dBiriry number fA)—the ratio of (/) the index and can be used with ihe percentage finer

-touchy inde\ of a soil to (2} the percenl by than :-jim size to determine its activity number.wc;|hiofpanicks having an equivalent diameter 5.3 The one-point liquid limit procedure ismatter than 0.002 mm. frequently used for routine classification pur-

poses. When greater precision is required, as4. Snauur; *f MetM when used for the acceptance of a material or for4,1 The sampfe is processed to remove any correiaiion with other test data, the multipoint 1

material retained on a 425-um (No. 40) sieve, procedure should be used. ,.]The liquid limit is determined by performing 5.4 These methods are sometimes used tomah in which a portion of the sample a spread evaluate the weathering characteristics of clay- pm a brass cup. divided in two by a grooving tool, shak materials. When subjected to repeated w«- .'md then allowed to How together from the ting and drying cycles, the liquid limits of these L ]shocks caused by repeatedly dropping the cup ia materials tend to increase. The amount of in-j sundard mechanical devke. The multipoint crease is considered to be a measure of a shale's 11liquid limit. Procedures A and B. requires three susceptibility to weathering. I jor more trials over a range of water contents to 5.5 Toe liquid limit of a soil containing sub-tc performed and ihe data from ihe trials plotted »™u"»l amounts of organic matter decreases dra-or calculated to make a relationship from which matically when the soil is oven-dried before test-the liquid limit is determined. TV one-point in*. Comparison of the liquid limit of a samplel.quid Umit. Procedures C and D. uses the dau before and after oven-drying can therefore befrom two trials at one water content multiplied used as a qualitative measure of organic matterX a correction factor to determine the liquid content of a soil.'imu.4 2 The plastic limit is determined by alter- 6- *??«*»

pressing tofcthcr and rolling ir.x a 3.2 6.1 Liquid Limit Device— A mechanical de-("6 in.) diameter thread a small portion of vice consisting of a brass cup suspended from asoil unu.1 its water content is reduced to a carriage designed lo control its drop onto a hard

pi-mi at which the thread crumbles and is no rubber base. A drawing showing the essentiallunger able 10 be pressed together and rerolled, features of ihc device and the critical dimensionsThe water content of the soil at this siagc is is given in Fig. 1. The design of ihe device mayfc&oned as the plastic limit vary provided that the essential functions are

fiR3Q0698

*|h 04318

pre$crvttJ_.Th? do ice ma> be opcruu'd either b> rnusi noi diiK-; ;roni tnov ohuineJ usinga hand crank or b\ an elccinc motor - ----- manuaj|j operated J^MCC6.! I £JH'— The base shall he hard rubber 6.2 f-'fut 0'"-r>.'.\f T»t<i — A grooMne lool ha.

having a D Duromeier hardness ol'KO 10 0. and mp dimensions shown in Fig, 2. Thtf tool iJu.a resilience such that an 8-mm ( Vi*.-in. ) diameter be made of plastic or noncorrodmg metal. TVpolished steel ball. *hen dropped from a height design of irk- lool mav \ar> aslongasiheessenu,of 25- cm (9.84 in.} will have an average rebound dimensions are maintained. The tool ma>, fa-of at least 80 % but no more than 90 i. The tests need not. incorporate ihe gaee for adiusting fashall be conducted on ihc finished base with feei height of drop of ihe liquid limit deMcc.attached. 6.5 G'um'— A metal pgc block for adjusting6.1.2 Feet — The base shall be supported b\ the height of drop of ihe cup. hating the dimes

; rubber feet designed to provide isolation of the sions shown m F;c. _V The design of the toot nu[. j base from the work surface and having an A vary provided the gaae will rest secure!} on tit

Durometer hardness no greater than 60 as mea- base without being susceptible to rocking, aicsured on the finished feet attached to the base. the edge *hich contacts (he cup dunng adju

jjj| 6.1.3 Cup— The cup shall be brass and have a mem is straight, ai least 10 mm C«in.)»idettouU weight, including cup hanger, of 1 85 to 2 1 5 g. » iihout bevel or radius.

6.1.4 Cam—The cam shall raise the cup 6.4 Con/Jimr*— Small corrosion-resiiUir--| smoothly and continuously to its maximum containers with smit-fining lids for wiier conferEH height. over a distance of at least 1 80* of cam specimens. Aluminum or stainless steel cam 2L:kiJ rotation. The pieftiieU cam motion is a uni- cm <1 in.) high b> 5 cm (2 in.) in diameter*

formlv accelerated lift cun-e. The design of the appropriate.cam and follower combination shall be such that 6.5 Balatht- — A balance readable ro at katthere is no upward or downward velocit) of the 0.0 1 g and ha> ing an accuracy of 0.03 g withbcup when the cam follower leaves the cam. three standard de\ laiions within the range of tot

.VOTI 3— The cam and follower design m Fig. t is Within anv I >g range, a difference between re»for umfonniy Kcelented (parabolic) motion after con- ings shall be accurate vMihm 0.01 g (Notes 4 UKuci and assures thai the cup has no veiocm ai drop 5 ).off Oihcr cam designs aiso provide (his feaiurc andma> be used. How w. if ihe cam-follower lift patwrn SoTE T5" Mtfl/lods E 8"s and E 3i° for M «is not known, zero velocity at drop off can be assured pianation of lerms relating 10 balance peflormance.by carefully filing or machining the cam and follower Non ?— For lr^u«n" "«- a lop-ioadmg t>pc tiso that the cup height rtmajns constani over the last :0 ance *llh automatic load indication, readable to 0.0to 45' of cam rotauon S- an^ *i3vin? an mdfx of precision isundard dfManoc

of 0.003 or better is rnosi suiuble for ihis mrthoc6.1.5 Carriage—- The cup carnage shall be However, nonauiomauc indicating tquaJ-arra

consmicted in a wa> that allows convenient hut "l bafancn and wmc small tquaJ arm IQP pansecure adjustment of ihe heighi of drop of the laving «adab.lui««d Kns.inii.es <ri 00:g „ •te

j~ „ ,„ _, , , „ provide ihe required accurarv »hen used *iih a weafecup to 10 mm (0.394 in.). The cup hanger shaJI ^ of ASTM CTaiS 4 ,sal(0na| Bureau of Sundtrtbe attached 10 the carriage by means of a pin Class P> or better. Ordinan. commerciaJ and dassrooa:which allows removal of the cup and cup hanger t>pe bajances such as beam baJances art no( sutiaAfor cleaning and inspecuon. for thls mcihod

6.1.6 Optional \ioior Drive— As an aJtcrna- 6.6 Sivrasc Container— A container m whktlive to the hand crank shov/n m Fig. i . ihe device to store the prepared soil specimen that will orma\ be equipped *tth a motor to turn ihc cam. contaminate the specimen man> wa\.and wbxSSuch a motor musi lurn the cam at 2 ±0.1 proems moisture loss, A porcelain, glass, omoluiions per second, and must be isolated pbstic dish aboui I I.J cm (41: m i in diamCTfrom the rest of the device b> rubber mounts or and a plastic bag laree enough 10 endow the dtffin some other wa> that prevents vibration from and he folded o\cr is adequate.the moior being transmuted 10 the resi of the " 6." (Jn>unj o/^tj Plait' — A ground glass plttapparatus, It musi be equipped with an ON-OFF ai leasi i'O cm 1 11 in ) squair b> I cm 1 5i IB.switch and a means of con\eriientl\ posiiioning thick for mixing soil and rolling plastic iifflsthe cam for heighi of drop adjustments. The threadsresults obtajned using a moEor-dmen device 6.S Spuiitfc— \ ipaiuto or pil! knife ha \ingi

I

flR300699D-l? - - - : - " • . • ~: " - - -

< 04318

_,,u jrvui ^ cm i i m ' wide b> about ifl cm 8 3 V^herc dau from this test method are 10. n * .,*n£ In addition, a spaiula ha\msL a blade be used t'or correlation w-ith other laboratory or-s-ut 2 j cm 11 in i «.idc and 15 cm (6 in.) long field test data, use the same matenal as used forj*. fwn tound useful for inttiai mixing of sam- these tests where possible. _ . .'ic* . 8.4 Obtain a representative pcnion from then o j iy A 20-3 cm (S m.J diameter. 425- total sample sufficient to provide 150 lo 200 g of

..m (No 40) sie\c conforming to ihc require- maienal passing the 425-um {No. 40) sieve. Free-icnts oi' Specification E 11 an3 having a nm at flowing samples ma\ he reduced by the methods.j*t 5 cm E2 m.i abo^e the mesh. A 2-mm (No. of quartering or splitting- Cohesive samples shall"i sie\e meeting the same requirements mav be mixed thorough!} m a pan with a spatula, orvo be needed, scoop and a representative portion scooped from« 10 Hi/Wi &v;/i". or similar container for the total mass b> making one or more sweep*

controlled amounts of water to soil and with a scoop through the mixed mass.tines from coarse panicles.

f- 11 Dntny 0\cn—A thermostatically con-.roHed oven, preferably of the forced-draft type. 9- Calibration of Apparatus.upable of continuously maintaining a tempera- 9.1 Inspection of H 'earLjreontO±5"Cthroughouiihedrytngcnamber. 9.1.1 Liquid Limit Device— Determine thatI he oven shall be equipped with a thermometer the liquid limit device is clean and in good work-.4 suitable range and accuracy for monitoring ing order. The following specific points should•x en temperature. _ be checked:6,12 Washing Pan—A round, fiat-bottomed 9.1.1.1 Hew of Base—The spot on the base

run at least T.6 cm (3 in.) deep, slightly larger at where the cup makes contact should be worn no;iie bottom than a 20.3*cm(&-in.}diameter sieve, greater than 10 mm (H in.) in diameter. If the

6,13 Rod {optional*—A metal or plastic rod wear spot is greater than this, the base can be 1," tube 3.2 mm Ci iiu in diameter and about 10 machined to remove the worn spot provided the j. m (4 m.) long for judging the size of plastic limit resurfacing does not make the base thinner thantreads, specified in 6.! and the other dimensional rela-

tionships are maintained. 1-, Miteriih 9.1.1.2 Wear of Cup—The cup must be re- I J

7,1 A supply of distilled or demineralized wa- placed when the grooving tool has worn a de-ter, prwson in the cup 0.1 mm (0.004 in.) deep or <-i

when the edge of the cup has been reduced to | IS. Sampling ' ha]f iu Ongjaal thickness. Verify that the cup is ' '8,1 Samples may be taken from any location firmly attached to the cup hanger.

that satisfies testing needs. However. Methods 9.1.1.3 Wear of Cup Hanger— Verify that uheC 702, and Practice D 75, and Recommended cup hanger pivot does not bind and is not »ornPracucc D420 should be used as guides for se- to an extent that allows more than 3-mm (''i-in.)Itfcung and preserving samples from various side-to-side movement of the lowest point on thei^pcs of sampling operations. Samples which will nm<V prepared using the wet preparation procedure. 9.1.1.4 H Vor of Cam—The cam shall, not beso 1. must be kepi at their natural water content worn 10 an extent that the cup drops before theprior to preparation, cup hanger (cam follower) loses contact with ihe

£.2 Where sampling operations have pre- cam. ... _ .v?rved the natural stratification of a sample, the 9.1.2 Gfijo'vi'ng Tools—Inspect grooving toolsanous sirata must be kept separated and tesas for *ear on a frequent and regular basis. Ther ribrmed on ihc panicular stratum of interest rapidu> oCwear depends on the matenal from•.ah as little contamination as possible from *hich the 100! is made and the types of soils•trier sirau. VVhcre a mixture of materials will being tested. Sandy soils cause rapid wear of"v used in construction, combine the \arrous grooving lools. therefore, when testing these ma-jmponents in such proportions that the result- tenals. tools, should be inspected mort frequeniNjnt sample represents the actual construction than for other soils. \n> tool *ith a up

flR300700

r

W D4318

of Ihe up of the grooving tool musi be 7-9 10 8.1 Adjust the water contcni of ihe soil to nnngit tomm. a consistenc> lhai would require 25 to 35 blo*s

Son 6—The width of the tip of grooving toois is of ln liquid limit device to close ihe groot?comememly checied using a pocket-sued measuring (Note 8). If. during mixing, a small percentage ofmagnifier equipped with a millimetre scale. Magmfien material is encountered that would be retainedof this l>pe arc available from most laboraton. juppl) «-.<?«,„ ,nj m. ,- . .._ .L.companies. The depth of the tip of grooving tools can 0,n a *2S+m °' *>J Slcve; remove lhfsc Pbe checked using ihe depth measuring feature of vernier cles b> hand- " possible. If tl is impractical localipers. remove ihe coarser material by hand, removt9.2 .idjuvmentnt'tMx/ntifDrop-Mjuxthe sma11 P««niages (less than about 15^) tf

heigh! of drop of ihe cup so that the point on the ?«»' ma*enal > *«*."« lnc SP 111ctip thai conies in contact with the base rises w 1*25b * ''r1"1 *>° 40> MCVC W|W a P*61**a height of 10 ±0.2 mm. See Fig. 4 for proper f«»«»h«"nr rubber stopper, or olherconvea.location of the me relative to the cup during *m **** Prided Ihe operation does not da-adjusunenL *** nci* * <**«* nwenal that wouldM _ , . , __ . , ~ . . wuined if the washing method described •NOTC 7— A tfoov-enjcnt procedure fcrtdjuan* the i« i •»-_-„„-, tf 1.™ B---.,.... nf « _aeigln of drop * as follows: place a piece of *MUnf '«•'-*<« "««• " *«!» percentaies of cotni

a«tenaJ are encouniered dunnf rmung. or « •taea»of!heenpltiJiAcrpi\«c.Thea4 «f Aeiapr coosideted imprKtical to remove the comer«w> from uWc^hurrtbouldbbeci the 901 oatke nuteriaJbj the met hods just described, wash tfc

-todiup ie*«al ti«a wii mirfc ihe comaci ipot Anich pwude* found during mixing areme cup wtlie device and iwii tae CUB* wMil dw cop sbeUs. or other fiigile panicles, do not crash tfaoeii laned *o its aaurnum he«ht Slide die acifht pit panides to make them paa«425-tim-(No.4Q|•oder tfttf cup from the fi md ob«nT wjwiter ite ^ ^ itmo%« b> hand or b> washing. Raceo|rcainactstlwcuportheiape.SeeFft.4.Jf!beitpe .1. • _j -i - .». « j- t __ andcuparc both conticiJI the beifhi ofdrop^ »«« m'wd «»'««»*« noragc dish, cox-er to pipproximiteiy conect tf ooc adjust the cup until n- venl toss of moisture, and allow to stand for mmuJtaneous contact is nude. Check adjustment by least 16 h /overnight). After toe standing periodturning the crank ai 2 icvoluiioM per second while and jmmedi3tely before starting the test, thor-holding the jage m position agatna the upe and cup. Miinu,, «„,:. ,k- ,«;iIf a ringing or clicking sourrf is hard without the cup OU^J> remnt Thc Ml1-nsin| from the gage, the adjustment is correct. If no NOTE S — The time laien lo adequaieJj mix a trinngjniisheardoriftheeupnsesfronj the gage, readjust will vaiy greailx. depending on ine plastiat> and initaline height of drop. If ihe cup rocks on the gage dunnf water content. Initial mixing limes of more Uian 30 —this checking operation, the cam follower pivot ii ex- in ma> be needed for sitff. fat days.cnsivef> worn and the worn parts should be replaced. ._ . _ _ , / * . „ • u , ..„; D«_, -jAlways remove upe after eomplaion of adjustment 'O-1-2 Samples CotuamngMattnai Xetaii*operauon. on a 425-pm fa'o. 40) Sieve:

10.1.2.1 Select a sufficient quantity of soil *MULTIPOINT LJQU1D IJMTT-PROCEDl RES Mlufaj waier comem to provide ,50 "lo 2QQ g rf

A maleriaJpaswngthe425-jim{No.40)sieve.Plicr10. Pr«p*r«rion of Test Specimens in a P3" Pf d/sh ™d add su cient wafer to cow,-,..._ _ , . , the soil. Allow to soak until all lumps haw10. 1 H e, Prcparanon-Etw where the dry taRened and fines no Iongtfr adhefe lo

method of specmien prepanuion is specif.ed surfacesoflhecorasepartides(NoIe9}.(10.2). prepare specirnens for test as descnbed inthe following sections. - - ;-. - Norr 9— In some cam. ihe cations of saiii presea

10 I 1 Samfl/cs Passing ihc 42 f -urn f.\o. 40 in UP water. . , . _ , . the soil and signincanU> aJter the test results should upb> v,suaJ and manual procedures wa,fr UJfdsm j , afld washmg opcraupttit is determined lhai the sample has little or no UnJea it is known thai such cauons are not present amaienaJ retained on a 425-um (No. 40} sie\e, the up water, distilled or dcmtneralned atcr shouldprepare a specimen of 1 50 to 200 g bv mixing be used- As * S*n*ral ™'*- wr conu.n.np more thu, . . . , ,. „ , „ . _• „, '_. . . 100 mt/L of dissolved solids should not be used fcrthoroughly with distilled or demmeralized water wash]nj oper,,]0ns.on the gJass plaic using the spatula. If desired.soak soil in a storage dish with small amount of 10.1.2.2 When thf sample contains a laijcvar/v •« «fkft»Ti tK»(r.;i k*f«r- »K. nv<* -*• -.;•;«- percentage of material retained on the 425-uJD

D-19 flR30470!

043 18

\4> 4i" -.icvtf rvruirm the lolloping ^ashine diiiillcJ or Jcmineniii^oJ "-JUT or N ji•pcotion in increments, ashing no more than the mixture to dry at ri\jm tern pen; u re• Kg 1 1 Ibi ot matenal at one time. Place the mivmg on the glass plate The soil should be at „-» Sunn NQ, -Jyisieve in the boitom of iheclean water content that will result m closure of tru-;un Pour the soil water mixture onto the sieve, groove. in 25 to 35 blows Return the mixed sosH gravel or coarse sand panicles are present, nnse to the mixing dish, cover to prevent loss o.f mois-js manv of these as possible with small quantities turc. and allow to stand for at least I ti h. After•r water from a wash bottle. and discard. Alter- the standing period, and immediateK before•umelv. pour the soil water mixture over a 2- starting the test, remix the soil thoroughly.•nmiNo IQi sieve nested atop ihe 425-um (No. 10,2 Dr\ • Pwparaitiw-01 sieve, nn« the fine matenal through and 10.2,1 Select suiTicieni soil to provide 150 tc'cmove the 2-mm (No. 10) sieve. After washing 200 g 6F material passing the 425-um (No. 40,:nd removing as much of ihe coarser matenal as sieve after prixressing. Dn the sample at rootr(••ossible. add sutTicieni waTcr to ihc pan to bnng temperature or in an oven at a temperature no:the level loabout 1 3 mm (•: in.) above the surface exceeding 60*C until the soil clods will puhenzeot the -125-um (No, 40> sieve. Agitate the slum readilv. Disaggregation is expedited if the sample**> stimnj with the fingers while raising and is noi allowed to completelv dry. However, thelowering the ste\e m the pan and swirling the soil should have a dr> appearance when pulver-tuspension so that fine matenaJ is washed from ized. Puhenze the sample m a mortar with athe coarser particles. Disaggregate fine soil lumps rubber tipped pestai or in some other wa> tha::hat have not slaked b> gently rubbing them over does not cause breakdown of individual grainsthe sieve »ith the fingertips. Complete the wash- When the coarse panicles found during puNen-mg operation by raising the sieve above the water anon are concretions, shells, or other fragileourface and rinsing the material retained with a panicles, do not crush these pankies to makesmall amount of dean water. Discard material them pass a 42 5 -urn (No. 40) sieve, but removeretained on the 425-um < No. 40) sieve. by hand or other suitable means, such as washing10.1.2.3 Reduce theater content of the ma- 10.2.2 Separate the sample on a 42i-ura (No pi

lenal passing the 425-um (No. 40) sieve until it 40) sieve, shaking the sieve by hand to assureapproaches the liquid limit. Reduction of water thorough separation of the finer fraction. Return ^content mav be accomplished by one or a com- the material retained on the 425-tira (No. 40*Innation of the following methods: (a) exposing sieve to the pulverizing apparatus and repeat the fji he air currents at ordinary room temperature, pulverizing and sieving operations as many times Mi />} exposing to warm air currents from a source as necessary to assure that all finer material has<-uch as an elcctnc hair dryer, (c) filtering in a been disaggregated and matenal retained on theSuckner Funnei or using filter candles, id) de- 425-um (No. 40) sieve consists only of individual |~j..anting clear water from surface of suspension, sand or gravel grains. [ Jor (<r) draining in a colander or piaster of pans 10.2.3 Place material remaining on the 425-Jish lined with high rctentivity. high wet-strength um (No. 40) sieve after the final pulverizing initer paper." If a piaster of pans dish is used. taJte operations in a dish and soak in a small amount '.-are that the dish ne\«r becomes sufficiently of water. Stir the soil water mixture and pourturned that it fails to actively absorb water into over the 425-u.m (No. 40) sieve, catching theis surface, Thoroughlv dry dishes between uses, water and an> suspended fines m the washingDunng evaporation and cooling, stir the sample pan. Pour this suspension into a dish containingiitenenoughtoprevemoverdrymgofihe fringes the dry soil previouslv sieved through the 425-jnd soil pinnacles on the surface of the mixture um iN\> 40 1 sieve. Discard matenal retained orfor soil samples containing soluble salts, use a ihe 425-u.m l No 40) sieve.•nctfiod of «.jter reduction such as j or b thai IQ.2.4 Adjust the water content as necessary•.<!! noj eliminate the soluble sails from the test b> dning as descnbed m 10, l.-.j or b> mi vine• ivamen _ on thegJass plate, using the .spatula uhile addtnc

in ! 2.-1 Thoroufhh mix the matenal passing increments of distilled or Jemincrjlized water,-iQ) sieve on ihe glass piaie using ______

- spaiuia, Adjust the water content of ihe mix- . s -^ s njtef 15Bfc lh"7:<m"7-ri«re, if necessarv bv adding small increments of pr^cnwii>ta*:i.>r>

\flR300702

r

<f 0 4318

until ihc soil is at a water content" that will resuli operation and repeat I t . I 10. 11,3 If the soilin closure of the groove m 25 lo J5 blows. - slides on the surface of the cup. repeat ll.j

l0.2.,> = Pui soil m the storage dish..cover 10 through 11.3 at a higher water conient. If. afterprevent loss of moisture and allow to stand for several trials ai successive^ higher water con-at feast 16 h. After the standing period, and tents, the soil pal continues to slide in the cup orimmediate!) before starting the test, thoroughly if the number of blows required to close theremix the soil (Note 8). groove is always less than 25. record that the

liquid limit could not be determined, and reportM. Procedure . . . .: .,.- _the soil as nonplastic without performing the

II. I Place a portion of the prepared soil in plastic limit test.the cup of the liquid limit device at the point 11.5 Record the number of drops. A', requiredwhere ihe cup rests on the base, squeeze it down. 10 close the groove. Remove a slice of soil ap»and spread it into the cup to a depth of about 10 proximatcly the width of the spatula, extendingmm at its deepest point, tapering to form an from edge to edge of the soil cake at right anglesaprxoximately horizontal surface. Take care to 40 the groove and including that portion of theeliminate air bubbles from the soil pat but form groove jn which the soil flowed together, piace »the pat with as few strokes as possible. Heap the a weighed container, and cover. - -unused soil on the glass plate and cover with the J I.* Return the soil remaining in the cup atinverted storage dish or a wet towd. the glass plate. Wash and dry the cup and froo*

11.2 Form a groove in the soil pat by drawing ing tool and reanach the cup to the carnage mthe tool, beveled edge forward, through the soil preparation for the neit trial. -*ron a line joining the highest point to the lowest 11.7 Remix the endre soil specimen on lacpoint on the rim of the cup. When cntting the (lass plate adding distilled water to increase thegroove, bold the grooving tool against the surface water content of the soil and decrease the numberof the cup and draw in an arc. maintaining the of blows required to dose the groove. Repeattool perpendicular to the surface of the cup I I.I through 11.6 for at ieast two additional triad-throughout its movement. See Fig. S. In soils producing successively lower numbers of blowswhere a groove cannot be made in one stroke to close the groove. One of the trials shall be forwithout tearing the soil, cut the groove with a closure requiring 25 to 35 blows, one for closureseveral strokesof the grooving tool. Alternatively between 20 and 30 Wows, and one trial for acut the groove to slightly less than required di- closure requinng 15 to 25 blows. -•:mensions with a spatula and use the grooving 11.8 Determine the water content. H \.ofthe'tool to bnng the groove to final dimensions, soil specimen from each trial in accordance with'Exercise extreme care to prevent sliding the soil Method D 2216.. Make all weighings on the same.pat relative lo ihe surface of the cup. _ _ ..balance... Initial weighings should be perforrDed-

11,J_ Venfv that no crumbs of soil are present immediately after completion of the test. If the''on the base or ihe underside of the cup. Lift and test is to be inicrrupted for more than about !5'drop the cup bv turning the crank at a rale of 1.9 min. the specimens already obtained should betto 1,1 drops per second until the two halves of weighed at the lime of the interruption. -Tthe soil pat come in contact at the bottom of the _*groove aJongj distance_o_H3i_mmI'/iJrU.. See 12. Calculations .____ . -~Fig-£ ..-.-....----.' ....... 12.1 plot the relationship between Ihe waterNOTE 10—Use the end of the grooving tool. Fig. 1 content. H\. and the corresponding number of

or a scale to venfv thai the groove has dosed 13 mm drops. .V. of the cup on a srmilogarithmic graph(''Ini)l with the water content as ordinates on the arith-

11.4 Venfv thai an air bubble has not caused meiical scale, and the number of drops as abscis-prematurr dosing of the groove by observing that sas o_n..the loganthmic scale. Draw the bestboth sides of the groove have flowed together straight line through ihe three or more plotted'with approximately the same shape. If a bubble points. -----.has caused premature closing of the groove, re-. 12-2 Take the water content corresponding to"*form" the soili in the cup. adding a srflall amount the intersection of the line with the 25-dropof soil to make up for that lost in ihe grooving abscissa as ihe liquid limit of the soil. Computa-"

D_21 fl-R300703•J't

QJP 04318

al methods mav be substituted for the graph- liquid limn values is greater than one percentagemcih&j for fitting a strat|hrtme to the data point, repeat the test.: determining the liquid limit. PLASTIC LIMIT

LIQL1D LIMIT—PROCEDURES . . _,^ „C \NO D 16. Preparation of Tesi Specimen

. _ 16.1 Select a 20-g portion of soil from thel.t Prepannon of Test Specimens matcn2] prepareaibr ihe liquid lirnifiett. either

11 1 Prepare the specimen m the same man- after ihe second mixing before the test, or from•„•• is described in Section !0, except thai ai the soil remaining after completion of the test.- vmg, adjust the water content to a consisiencv Reduce the waier conteni of ihe sot! to a consisi-^uinng 20 to 30 drops of ihe liquid limit cup ency at which ti can be rolled without sticking to.. lose the groove. the hands b> spreading and, mixing continuous!;.

on the glass plate. The drying process may be14. Procedure accelerated bv exposing the soil to the air current

4 I Proceed as described in II.I through frorn an electnc fan. or by blotting with paperi * except thai the number of blows required to that does not add any fiber to the soil, such as*•><? the groove shall be 20 to 30. If kss than 20 hard surface paper toweling or high wet strength•T more than 30 Wows are required, adjust the filter paper..ijwr conient of the soil and repeat the proce-'ure, _. ___ _____ 17. Procedure,4.2 Immediately after removing a water n.j From ihe 20-g mass, select a portion of" --- - - - -

.orient specimen as described in 11.5. reform L5 ro :.o g. Form the test specimen into anTI_ soil in the cup. adding a small amount of eii_pjoidal mass. RoU this mass between the palm... .1 to make up for that tost in the grooving and „ gn|ers j $* ground-glass plate with just»jtcr content sampling operations. Repeat 11.2 sufficient pressure to roll the mass into a thread-.trough 11.5. and. if the second dosing of the Of uniform diameter throughout its length (Note ngroove requires the same number of drops or no 12). The thread shall be fanner deformed on•nme than two drops difference, secure another jj nroke so thai its diameter is continuously ' •**jter conient specimen. Otherwise, remix the reduced and its length extended until the diam-.ntire specimen and repeat. ner reaches 3.2 ±0.5 mm (0.125 ±.020 in.). |")van 11— Excess** drying or iMd«quate mixiot taking no more than 2 min (Note 13). The j

*ill cauie the number of btaw* to vary. amount of band or finger pressure required will14.3 Determine water contents of specimens vary greatly, according to the soil. Fragile soils of

.v described in 11.1. low plasticity are best rolled under the outer edge Iof the palm or at the base of the thumb. • , J

15, CiJcoIaiioos NorE l2—\ oonn»I rate of roilinf for most joib15J Determine the liquid limit for each water should be SO us 90 strokes per roinutf. counuot » }

,*mem specimen using one of the following sroke is ooecomplne motion of the hand forwird and ,back to the starting position. This, rate of rollint nuy.cuations, havc w decreascd for ^ ( 1 ^

i NOTE 13—A 3.2-mm CVm.l djametet rod or tubeor is useful for frequent comparison *ith the ioil thread

to isceruin when the thread has reached the properLL m MH\J diamcier. especiail> for inexperienced operators.

tfK _ __ 17.1.1 _\Micn the diameter of ihe thread be-- ihe number of blows causing closure of the comes 3.2 rrirh". break ihe thread into sevcrajirooveai water content. pieces. Squeeze ihe pieces together, knead be-

= waier content, and twern the thumb and first finger of each hand.- a factor gjven m Table 1 reform into an ellipsoidal mass, and reroll. Con-

The liquid limit is the avenge of the two tnal tmue this ajiernaie rolling to a thread 3.2 mm inuid limit values, diameter, gathering together, kneading and re--, * 2 If the difference between the two tnal rolling, until ihc thread crumbles under the pres-

D-22

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*j)in 04318

until the soil is ai a water eomem thai will result operation and repeat 1 1 . 1 to 115. If ihe soilin closure of the groove in 25 to 35 blows. -- slid on the surface of the cup. repeal i i . i10.2.5 Put soil in the sioragc dish, cover to through 11.3 at a higher water conient. If. after

prevent loss of moisture and allow to siand for several trials at successively higher waier con-ai least 16 h. After the standing period, and lents. Ihc soil pat continues to slide in the cup orimmediately before starting the lest, thoroughly if the number of blows required to close theremix ihe soil (Note 8). groove is alwa\$. less than 25. record that the

liquid limit could not be determined, and reportIJ. Procedure thf ^ as nonp[astic without performing ihe

II.I Place a portion of the prepared soil in plastic limit lest.the cup of the liquid limit device at ihe poinj 11.5 Record the number of drops. A, requiredwhere the cup rests on the base, squeeze it down, to close the groove. Remove a slice of soil ap.and spread it into the cup to a depth of about 10 pro\imaie!v the width of the spatuJa. exiendinfmm at ifs deepest point tapering to form an from edge to edge of the soil cake at right anglesapproximately horizontal surface. Take care to to the groove and including that portion of theeliminate air bubbles from the soil pat but form groove in which the soil flowed together, place tothe pat with as few strokes as possible. Heap the a weighed container, and cover.unused soil on the glass piate and cover with tbe H.6 Return the soil remaining in the cup toinverted storage dish or a wet towel the glass plate. Wash and dr> the cup and poo*

11.2 Form a groove in the soil pat by drawing ing loo! and rextuch the cwp lo the carriafe •the tool beveled edge forward, through the soil preparation for the next trial.on a line joining the highest point to the lowest 11.7 Remix the entire toil specimen on thepoint on ihe rim of the cap. When cutting the glass plate adding distilled water to increase thegroove, hold the grooving tool again* the surface water content of the soil and decrease the numberof the cup and draw in an arc. maintaining tbe of blows required to do* the groove. Repottool perpendicular lo tbe surface of the cup II.1 through 11.6 for at least two additional triabthroughout its movement. See Fig. 5. In soil* producing successively lower numbers of blowwhere a groove cannot be made in one stroke to ctose the groove. One of the trials shall be fcrwithout tearing the soil, cut tbe groove with a closure requiring 25 to 35 Wows, one for closuresevend strokes of the grooving toot. Alternatively, between 20 and 30 blows, and one trial for acut the groove to slightly less than required di- closure requiring 15 lo 25 blows.rnensions with a spatuJa and use the grooving 11.8 Determine ihe water content, W\.ofthetool to bring the groove to finaJ dimensions, soil specimen from each tnal in accordance withExercise extreme care to prevent sliding the soil Method D 2216. Make all weighings on ihe samepat relative to ihe surface of the cup. balance. Initial weighings shouid be performed

11.3 Verify that no crumbs of soil are present immediate!) after completion of the lest. If theon the base or the underside of the cup. Lift and test is to be interrupted for more than aboul 15drop the cup by turning the crank at a rale of 1.9 min. ihc specimens already obtained should beto 2.1 drops per second until the rwo halves of weighed at the time of the interruption.the soil pat come in contact at the bottom of thegroove along a distance of 13 mm (lh in.}. See 12. CalculationsFig- 6- - - . . . - - . ----- j-> | pj0[ (he relationship between the waterNOTE 10—Use the end of the grooving tool. Fig. 2. conient. H\. and ihe corresponding number of

or a scaJe to verify thai tbe groove has dosed 13 mm drops. x of the cup on a semi logarithmic grapb(l/'inj . ,_ with the waier conieni as ordinaieson thearitb-

i 1.4 Verify that an air bubble has not caused mcncal scale, and the number of drops as abscis-premaiure closing of the groove by observing [hat sas on the logarithmic scale. Draw the bestboth sides of the groove have flowed togeiher straighi line through the three or more ploncdwith approximately the same shape. If a bubble, points.has caused premature closing of the groove, re- 12,2 .TaW ihc waier content corresponding to"form the soil injfie cup. adding a small amount the intersection of the line with the 25-dropof soil 10 make up for that lost in the grooving abscissa as the liquid limit of the soil. Compuu-

D-23 flR30(j705

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.ii meincd1- mav be suKiuuicd for the graph- liquid limn \alucs is greater ihan one percentagemetJuxJ lor lining a straight line to the dau pomi. repeal the test.determining the liquid limit. Acnr ixtrrrltfA^iiiw Lli>i( i

T UQUD LIMIT-PROCEDl RES ^ „C AND O 16. Preparation of Test Specimca

_ . , _ _ , 16.1 Select a 2G-g portion of soil from theit Preparation of Test Specimens • , , *. .. ,- -.,- . ,' ¥ ^ matenal prepared for lhe liquid bmii lest, eiiheri ' Prepare ihe specimen in lhe same man- after the second mixing before the test, or from

, as described m Section 10. except that at ihe soil remaining after completion of lhe tesi.mj. adjust ihe uatcr content to a consistency Reduce ihc water content of the soil to a consist-

.. .nnng lO to 30 drops of the liquid limit cup er,cy at which it can be rolled without sticking 10.lose the groove. the hands by spreading and mixing continuously

on the glass plate. The drying process may bel-i Procedure accelerated by exposing the soil to the air current

-i I Proceed as described in 11.1 through from an electric fan. or by blotting with paper* except that the number of blows required to lnai does not add any fiber to the soil, such as-< the groove shall be 20 to 30. If less than 20 hard surface paper toweling or high wet strength

• more than 30 blows are required, adjust the filter paper.-wicr content of the soil and repeat the proce-•„•»*. 17. Procedure-0 Immediately after removing a water ,?.! From the"2vH mass, select a portion of•lent specimen tt described m 11.5. reform jj to 2.0 g. Form the ten specimen into an

-, so3 in the cup. adding a small amount of effipsoidal man. Roll this mass between tbe palm. to make up for that ton m the tromine and or fingers and the jround laa plate with just*,tercoa*m sampling operation*. Repeat 11.2 sufficient pressure to roU tbe mass into a threadtrough 113. and. if the second dosinj of the of am bro diameter throogrwuttetentth (Noteshin* requires the same number of drops or no 12J. The thread shall be further deformed on n-%•« than two drops difference, secure another g 5 ^ w t itt dimeter is continuously Ittjtcr content specimen. Otherwise, remix the fortd and its length extended until the diarn ! , mire specimen and repeat. e{a jf ^ $3 ±0,5 mm (0.125 ±.020 in.).\ort ii—Exeeutve dnini or inadequate raixint taking no more than 2 min (Note 13). Tbe [*)

»iK CIUK the number of bte*s 10 v«y. _moum ^ „ fia|ftr 3 required will I j14,3 Determine w»:er contents of specimens vary greatly, according to the soil Fragile soils of

- Jescnbed in 11.3. low plasticity are best rolled under the outer edgeof the palm or at the base of the thumb, ' ]

15. CikrlitioM Non 12—A aomwi me of roffiDg tof mo« «ib i*15.1 Determine the liquid limit for each water should be SO to 90 mokes per minute, counong a

.oment sxcirnen using one of the followini iuoke»OMa3mptetemoik»ofUieb»odfoiwinlti»d ,back to the suruni poouoa. This rale of roflioc may

. 13—A 3.2-mra (H-in.) diameier red or rubeLL - «-A —j or 3 useful for frequent comparison with tbe soil thread

to isctnain *hen the thread has reached the properLL « A'(K'o diameter. especnUy for ineipericDCod operaion-

*r^rr 17.1.1 When the diameter of the thread be-\ * thenumberofblowscausingclosureofihe coroes 3.2 mm. break the thread into several

groove at water content. pieces. 5q-ieere ihe pieces together, knead be-11 » w iercomcnt. ind r>«n ihe thumb and first finger of each hand,*• * a factor pven in Table !. reform into in ellipsoidal mass, tad reroU. Con-

* he liquid limit is ;he average of ihe iwo inal unue this iliernate rolling to a thread 3.2 mm inVnnd limn values. diameier. gathering together, kneading and re-

s'1' I If ihe difference between the two tnal rolling, until the thread crumbles under the pres-

-4R3Q0706

(ked;

sure required for rolling and the soil can no 18. Calculationslonger be rolled into a 3,2-mm diameter thread lgi , Compute the average of the two **.(See Fig. 7). It has no significance if the thread comcms. If the difference between the two «breaks into threads of shorter length. Roll each comenis is greater than two percentage pointof these shorter threads to 3 2 mm m diameter. fepeat lne tesj_ Thc plastic Jiniil is a fThe only requirement for continuing the test is ^ ,wo water contents.that they are able to be reformed into an ellip-soidal mass and rolled out again. The operator PLASTICITY INDEX

,_ shall at no time attempt to produce failure atexactly 3.2 mm diameter by allowing the thread 19. Calculations

. to reach 3,2 mm. then reducing the rate of rolling jg.j Calculate the plasticity index as foUanor the hand pressure, or both, while continuing Pi - LL- PL

r •-: the rolling without further deformation until thejm • thread falls apart It is permissible, however, to *"nerc:m reduxrtlwtottlanwuirtofde&nMtionforfceWy LL - the liquid limit.

pfcsiksotk by making the raitiaJ diameter of the «•"« the plastic bmttB ellipsoidal ™*f« nearer to the required 12-mm Botn LLtnd PLsn whole numbers. If cat

final diameter. If cnimWing occun when Ihe *** ***utd Umit * P***1* fin"t could MI kthread has a diameter pester than 3.2 mm. this determined, or if the plastic limit is equal to*sh be owsideTtdtiatisfiKWry end point, pro- abater than the liquid feus. report tbe ** 4

D vided the nil has been previously rolled into a •ooptasuc. NP.•I thread 3 J ram ia diameter. Crumbling of the .

thread will manifest itself differently with the 20. Beponvarious types of soil Some foils &U apart ia »« , „ L <• „ - - rnumerous smaOaareptions of parbctei. others J. Repon tBefoltowing information:may form an outside tubular tover that sum ^ '! **""* ^ mformatKm. -splitting at botn"eSdTTSr inii.g progresses f° Any spcaal s men selecuon pn»toward the middle, and finally, the thread falls us£*Jcil » removal of and ^ fmm "apan in many small piaty particles. Fat clay soils lul?f° ple* , .,.,.,,.require much pressure to deform the thread. 20.1.3 Report sample as airdned if the swprparticularly as they approach the pla5tic limit. waLaird"f? or du,nng P P 00-With ihese soUs. tbe thread breaks into a series . 20' J'4 Iim«- P^c lirart- andof barrel-shaped segments about 3 J to 9.5 mm !!>'.in*x to the "earcst(H to '* in } in length Un* thc percenl dcsi?natlon-

17.2 Gather the portions of the crumbled ^ limit tests could noi be perform or .thread togeiher and place in a weighed container. [he PJf 1C iimit IS «P**° °rImmediately cover the container. h u'd I'™1- reP?rt thc »rf »

1 7.3 Select another 1 .5 to 2.0 g portion of soil 20' ' "5,from the originaJ 20* specimen and repeat the pfc ™"n °the 425*"(C40

"k . .

operations described in I7.l"a«d 17.2 until the J?"''* ^ **ich ''q,U'dcontainer nasal least 6 g of soil. ' " "" °m '**

17.4 Repeat 17.1 through 17.3 to make an-other container holding at least 6 g of soil. De-termine the water content, in percent, of the soil 21. Precision and Bias^ J TT* IV"0"*1!" ** 21.1 No imerlabonion testing programMethod D 2216. Make all wrings on the same ^ ^ con£Jucled usmg IBI mctia

. . . determine_mu!nlaboraiory precision.NOTI 14— The intent of performing two plastic ^ f c U'uhm larxsraton precision of

limn maJ when ihe conasjency in the lesi results can ai one laboratory on two soils using Procedure Abe confirmed by other meani for lhe liquid limit isshowri m Table 2.

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Thi\ uandard M fuf'/tfi n> 'r>/j/<>n a: ax\ nmff>\ the rnponsthlf tefhmcal nomminfc ana muxt tv reviewed nf. tii,- \farsotijif tin (e*ued I'ltht" 'tjpprrni-d ,\t +nhe'a+n tnur tomrnmn ore mwtetf fiifif t'o' 'ftiiiiin of tfitt siandara •>' i.'r jddmoralstijndjrdi and ifi"ii,J~fo atlawntJ W .tST\l HtaJijuartff) Yi'ur wnmewi •»(// rrcetv? rcrc'.i! toniidrraiinn ji s W .TII? u' sktrr^pttniihlfteehan.u. mmmiiitV *>kich ivu ma\ atirnd Ifyoujffiihai \pur comments ha\t not nrtinvt a lair hnjr.nv urnmai.f\vur I'jntj iw»fl to if\f 4ST\f Ci)'>"Hifi?ei>n Standard*. 1916 Race S/, Ptiiladctpntc. fa

D-31- AR3007I3

Agency Cincinnati OH 45268

Research and Development

Test Method

Organic Carbon, Total(low level)(UV promoted, persulfateoxidation)—Method 41 5.2

1. Scope and Application detector. The detector signal aintegrated and displayed as the

1.1 This method covers th. concentration of purgeibl. organicdetermination of total organic carbon carbon.n dr.nk.ng water and other waters jh. sample is then transferred to asubject to the limitations tn 1,3 and quartz ultraviolet reaction coil where5-1- tht nonpurgeable organtcs are, » _. . . ,. subjected to int.ns. ultraviolet12 Th,s instrument is des,gn.d for i()uminatlon in m- „„,„«.. rf lhea two-step operation to d.stmgu.sh ^ p.rsuifat«>.ag.nt. Thtbetween Purgeabl. and nonpurgtabtt nonpurfle7b,« M conv.r»d to CO

1.3 This method is applicable only to co» to th* '•J'Ction syst.m and intoth. carbonaceous matter which » th« dawctor Th« signal .1 integrated,either soluble or has a panel, siz. of *«•<*» th* P"'S«abl. organic carbon0.2 mm or less. valu«- and splayed as th.

conc.ntration of total organic carbon.1.4 The applicable range is from -approximately 50 ^g/L to 10 mg/L "*'Higher conctntratrons may b. 3 , Totaf anic csrt>on measurvidetermined by sample d.lutwn. ^ [h)J procedure IS tht sum of the2. Summary of Method Purgeabl. organ.c carbon and th.

' J ^ . . , nonpurgeable organic carbon asA sample is combined with 1 mL of -I-*;MH ;« •» 9 a«H t -a,,-, . kd . ufTlinOQ ITT iJ.A aMU ,O-acidified persulfate reagent andplaced in a sparger. Th. sample is 3.2 Purgeable organic carbon is th.purged with helium which transfers organic carbon maner that isinorganic COj and purgeable organics transferred to the gas phase when theto a C03 scrubber The COZ is sample is purged with helium andremoved with at least 99 9% which passes through the CO*efficiency with a 2.5-mmute purge. scrubber The definition is instrument-The purgeable argamcs proceed condition dependent.through a reduction system where thegas stream is joined by hydrogen and 3.3 Nonpurgeable organic carbon ispassed over a nickel catalyst which defined as that which remains afterconverts the purg^a^ie organic carbon removal of the purgeable organicto methane. The methane >s carbon from the sample containingmeasured by a flame icnizaiton acidified persulfate reagent and which

4IS1 J Dac 1382

i

4R3007II}

r

is converted to COs under the ' when analyzing samples w'nh easily carbonate 'Oicaroonate SIOCK solutioninstrument conditions. purgeable organics so as to minimize in a 100 ml volumetric flask and

losses. dilute to tfi« mark with reagent3.4 Th« system blank is th« value disuHed water f7.1).obtained in 8.2 for an irradiated, /• Reagents ,rrecir culated reagent distilled water 8. ProCdduro **'samp,a 7.1 Reagent Distilled Water:

Distilled water used in preparation of. 8.1 Allow at least 30 minutes4. Sampltf Handling and standards and. for dilution of samples warm-up time, Leave instrument'Preservation should be ultra-pure to reduce th. console on continuously when in dairy

magnitude of th* blank. Carbon use. except for the ultraviolet light4.1 Sampling and storage of dioxide-free, double distilled water is source, which should be turned offsamples must be done in glass ' recommended. The water should be when not in use for more than a fewbottles. Caution: Do not leave any distilled from permanganate or be hours.headspace in the sample bottle as obtained from a system involvingthis may contribute to loss of distillation and carbon treatment. The 8.2 Adjust all gas flows,purgeable organics. reagent distilled water value must be temperatures and cycle times to

compared to a system blank manufacturer's specifications. Perform4.2 Because of the possibility of determined on a recirculated distilled the "System Cleanup and Calibration"oxidation or bacterial decomposition of water sample. The total organic procedure in the manufacturer'ssome components of aqueous carbon value of the reagent distilled specifications each day. Recirculate asamples, the lapse of time between water should be less than 60 j/g/L. sample of irradiated distilled watercollection of samples and start of _Purgeable organic carbon values of until two consecutive readings within

" fhaFysis should be kepi to i minimum, the reagent distilled water should be '0% of each other are obtained.Also, wimples should be tcept cool less than 4 g/L. Record th. last value for the system(4°CJ and protected from sunlight and blank. This value is a function of theatmospheric oxygen. 7.2 Ptxasiium hydrog.n phthalat., total instrument operation and should

Stock solution. SCO mg csrbon/titer: not vary significantly from previous4.3 When analysis cannot b* Dissont 1.063 g of potassium runs. Reasons for significant changesperform** within two hours from time hydrogen phthal»t. (Primary Standard in the value should be identified.af sampling, the sample should b« - Grade) in reagent distilled water (7.1)acidified to pH 2 with HjSCU. Note: and dilute to 1 Hter *-3 Check the effectiveness of thc«C! should not be used because it is - CO* scrubber by analyzing theconverted to chlorine during the 7.3 Potassium hydrogen phthsists (2 - carbonate-bicarbonate standardanalysis. This causes damage to tht mg/L): Pipet 4 mL of potassium «olution(7J). Add 1 mC of acidifiedinstrument hydrogen phthalate stock solution pert ultaie reagent (7.6) to SO mL of

(7.2) into • one Kter volumetric flask , th. solution. Transfer 10 mL of th*a. lnt«rf»r*nc*s ' * and diluM to the mark with magent • «o!ution>wtth-rMgcnt to the first«. M ... . _ , dbtffiMt water (7.1). sparger and start the analysis cyde.B.I w • ssfnpw is nomogeniMd to No response or a very minor reading,reduce the size of the paniculate 7.4 Potassium hy*agen pMhaiat* (S should bt obuirwd from this solution.matter, the homogenizing may cause mg/U Pipet 1 mL of potassiumtoss of purgeable organic cartoon, thus hydrogen phthalate stock solution . 4 AC« 1yieiding .n ——— sly tow n*uK,. ,7.2. into - 100 mL vo.urn.trc ««k *£*?6 Aooaratus I"? , " '? *£ T. r**g™1t «««* *•»' <7- 1 ' blank- standardsB. Apparatus dtthltad ^ an6.1 Apparatus for blending or 75 potassium hydrogen phthalate fl c r.,:... th.homogenizing samples: A household (TO mfl/L): Plpet 2 m^of po(assrurn i-*?allbrale theblender or similar device that will hydrogen phthalate stock solution wwws.reduce particles in the sample to less (7 2, jnto a too mL volurnetr,c flask 3.5, j Run the reagent distilled waterthan 0 2 mm. and di|ute to the mark wjth reagem (7 , } and g 0 mg/(_ SIanaard ,7 4).

6.2 Apparatus for Total Organic d'St"led waief (71)' - - Transfer 10 mL of the solut.on-wnh-Carbon: The essent.a. components for 7>6 Aodtfied Persulfate Reagam: :"«*« ISZ 'lrSt SPaf9er *""the apparatus used in this method P|ace 100 mL of reagent distilled anaiyzer cycieare: A sparge assembly, flow water {7 t) in a comamer Add 5 g of ignore the meter reading for the firstswitching valves, a pyrolys.s furnace. potassium persulfate, Add 5 g {3 mL) CVC|equanz ultraviolet reactor coil, reducing Of concentrated (85%) phosphoriccolumn, flame lomzatton detector. acid Transfer a second 10 mL of theelectrometer and integrator. This solution-with-reagent to the firstmethod is based on the Dohrmann 7.7 Carbonate-bicarbonate, stock sparger and start the analysis cycleEnvirotech DC-54 Carbon Analyzer. solution, 1000 mg carbon/liter: PlaceOiher instruments having similar 0 3500 g of sodium bicarbonate and Record the meter reading (see 9 1} ofperformance characteristics may be 0 4418 g of sodium carbonate m a the final carbon value for each of theused. -" " ~ : 100 mL volumetric flask. Dissolve with reagent distilled water (7 1 1 and the

reagent distilled water (7.1) and dilute standard (7 4).6-3 Sampling Devices: Any ,0 tne m3rkapparatus that will reliably transfer If the meter reading is more than 25%10 mL of sample to the sparger. A 50 7.8 Carbonate-bicarbonate, standard above or below The calculated value ofmL glass syringe is recommended solution 50 mg/L. Place 5 ml of the standard 7,4. reanalyze tne standard

QIC. 1382 - 415.2-2

flR3007!5D-33 -. "-- -- "-

Committee O- 1 9. Task GroupTransfer a SKond 10 mL of the 19.06.02.03 (Chairman R. J. Joyceisolution-wtth.r.ag.nt to the first January 1 978.sparger and start th. analyzw cycle , _ . , _ « ._2. Operating Instruction OohrmennR.cord th* m«« reading <SM 9. 1 J of Envirotech. 3420 Scon Boulevard.the final carbon value for tach of th. Santa Clara, California 95050.standards 7.3 and 7.5.

of conc.n.r*ion us forand '

h« Uwtrt. o( the X/Ashould b. asonain* Conf*rtnct' AWWA'

from a knowl*dg. erf th* rang, ofainc«ntra(K>nt «xp«t«d from th.samples Standards for lower rangescan b. prepared by diluting standards7 2. 7 3. and 7 4

8.7 Analyze th. samples. Transf.r10 mL of sample with reagent 10 th*first sparger and start the analysis

4152-3 OfC, 1392

e>

and then begin 8 5 I again, If th. analyzer cyclem«ttr r«*dmg Isee i 1) ts within 25%o* the calculated value, continue to 'fl00'" tne "fw '«*ng for the firstn*xt step Th. calculated value is cvcl*<fefinedMS.S2. __ - Transfer • second 10 mL of theS.5,2 Calculate the factor for the solution-with-r.agent to th. first .deviate of th. inttrum.nl reading sparg.r and start th. anaVzer cycle($«•§ 1) for th. standard (7.4) from _, ,_ , , , „ . , ,h. calculated value by: "•«* *• ™ttf '••*"« ts" 9A°'th. final carbon value for each of thestandard reading - samples.calculated value 5PACTOR g Ca|cu|ationacalculated value

9.1 The values are read off the finalwhere th. calculated value >s [hit digital readout m pg/L The systemvalue obtained t* using (h* weight of blank reading obtained in 8 2 must 5epotassium hydros*" phtMiate and subtracted from alt reagent distilleddoes not include the carbon water, standard and sample readings.contributed by the reagent distilledwat*r|7.l]wnh whehtt has bean 10. Precision and Accuracydiluted.

10.1 In a single laboratory (MERL).8.5.3 Calculate tht adjusted reading using raw river water, centnfugedbv' river water, drinking water, an'd th.calculated value * (ROW - (FACTOR X effluent from a carbon column whichROW)) i ADJUSTED READING. had concentrations of 3.11, 3.10.where ROW * mtan reagent distilled 1 79. and 0.07 mg/L total organicwater (7,1) value. carton respectively, th. standard

deviations from ten replicates were9.3.4 Push in CAUBRATi button =013. ±0.03. r002. and ±0.02after READY light comes on and mg/L respectively.adjust the SPAN control to theADJUSTED READING calculated in 10.2 In a Single laboratory (MERL).S.S.3. _ using potassium hydrogen phthalate

in distilled water ai concentrations of«.* AnaJyze the standards 7.3 and 7.5 5.0 and 1 .0 mg/L total organic carbon.« oroV to check the linearity of the recoveries were 80% and 9 1 %.instrument at toast once each day: respectively.Transfer 10 mL of the »Jutwn*wrtn* Bibliography _ |

firit Spif9-r ** **** 1. Proposed Standard Method far JPurgeabte and NonpurgeaWe Organic

D-3-4AR3007I6

c

METHOD 9030 ^

* SULFIDES

1.0 Scope and Application

1.1 Method 9030 is used to measure the concentration of total anddissolved sulfides in drinking, surface and saline waters, and domestic andindustrial wastes. The method does not measure acid-Insoluble sulfides;copper sulfide is the only common acid-insoluble sulfide. Method 9030 issuitable for measuring sulfide in concentrations above 1 mg/1.

_2.J) Summary of Method

._,_:_ 2.1 Excess iodine is added to a sample which may or may not have beentreated with zinc acetate to produce zinc sulfide. The iodine oxidizes thesulfide to sulfur under acidic conditions. The excess Iodine is back-titratedwith sodium thiosulfate or phenylarslne oxide.

__ „_fc_, .. -,.- -,- f Ipt:/" ' -: ' ,',',. ..'• i:.

3.0 Interferences3.1 Reduced sulfur compounds that decompose in acid, such as sulfite,

thiosulfate and hydrosulflte, «ay yield erratic results. Also, volatileIodine-consuming substances will give high results. :-.. -: -•••--

3.2 Samples aust be taken with a »lnim» of aeration in order to avoidvolatilization of sulfides and reaction with oxygen which My convert sulfideto unmeasurable forms. •- -

3.3 If the sample is not preserved with zinc acetate, analysis muststart immediately.

4.0 Apparatus and Materials

4.1 Ordinary laboratory glassware.

5.0 Reagents

5.1 Hydrochloric acid, HC1, 6 N.

5.2 Phenylarsine oxide 0.0250 N: Commercially available.

5.3 Starch indicator: Commercially available.

D--35 .,-. flR30Q7M

2 /MISCELLANEOUS ANALYTICAL METHUOS

5.4 Potassium iodide, KI crystals.

5.5 Amylose indicator.

5.6 Standard iodine solution, 0.0250 N: Dissolve 20 to 25 g Kl in alittle water in a liter volumetric flask and add 3,2 g iodine. Allow todissolve. Dilute to 1 liter and standardize against 0.0250 N sodiumthiosulfate or phenylarsine oxide using a starch indicator, as follows.

5.6.1 Dissolve approximately 2 g (+1 g) Kl crystals in 100 to150 ml distilled water.

5.6.2 Add 20 ml of the iodine solution to be standardized anddilute to 300 ml.

5.6.3 Titrate with 0.0250 H phenylarsine oxide (PAD) until a palestraw color occurs.

5.6.4 Add a small amount of amylose indicator and wait until ahomogeneous blue color develops.

5.6.5 Continue titration drop by drop until the color disappears.

5.6.6 Run in duplicate.

5.6.7 Calculate normality by the following equation:Hi « «1 PAO x 0.02502 20

6.0 Sample Collection, Preservation, and Handling

6.1 All samples must have been collected using a sampling plan that Jaddresses the considerations discussed in Section One of this manual.

6.2 Aqueous samples must be preserved with zinc acetate or the analysis 1must be started immediately. . J

7.0 Procedure

7.1 Unprecipitated sample

7.1.1 Place a known amount of standard iodine solution into a500-ml flask. The amount should exceed the amount of sulfide expected.

7.1.2 Add distilled water, if necessary, to bring the volume toapproximately 20 ml.

D-36—— SIT3007I8

I

9030 /3

7.1.3 Add 2 ml of 6 N HCK

7.1.4 Pipet 200 ml of sample into the flask, keeping the tip ofthe pipet below the surface of the sample.

7.1.5 If the iodine color disappears, add more iodine untilthe color remains. Record the total number of ml of the standard iodineused In performing steps 7.1.1 and 7.1.5.

7.1.6 Titrate with reducing -solution (0.0250 N sodium thiosulfate- of 0.0250 N phenylarsine oxide solution) using the starch indicator until

the blue color disappears. Record,the number of ml used.

7.2 Precipitated samples

- zz_i_7.2.1 Add the reagents to the sample in the original bottle.Perform steps 7.1.1t 7.1*3, 7.1.5, and 7.1*6.

7.3 Oewatered samplesr 7.3.1 Return tne glass-fiber filter paper that contains the sample

§to the original bottle. Add 200 "1 of distilled water. Perfora steps7.1.1, 7.1.3. _7.1.5,_md 7.1.6.

- 7.3.2 The calculations (Section 7.4) should be based on theoriginal sample put through the filter.7.4 Calculations. One ml of 0.0250 N standard Iodine solution reacts

with 0.4 mg of sulfide present in the titration vessel. Thus, the followingequation should be used to calculate sulfide concentration:

mg/1 sulfide » 400(A-B)/ml sample

where:A * ml of 0.0250 N standard iodine solutionB = ml of 0.0250 N standard reducing sodium thiosulfate or

phenylarslne oxide solution.

8.0 Quality Control

8.1 All quality control data should be maintained and available foreasy reference or inspection.

f 8.2 Calibration curves must be composed of a minimum of a blank andv three standards. A calibration curve should be made for every hour of

continuous sample analysis.

fl"R300719D-37 -_- — - - - - - - -

4 / MISCELLANEOUS ANALYTICAL METHODS

8.3 Dilute samples if they are more concentrated than the higheststandard or if tney fall on the plateau of a calibration curve.

8.4 Employ a minimum of one blank per sample batch to determine ifcontamination has occurred.

8.5 Analyze check standards after approximately every 15 samples.

8.6 Run one duplicate sample for every 10 samples. A duplicate sampleis a sample brought through the whole sample preparation process.

8.7 Spiked samples or standard reference materials shall be periodicallyemployed to ensure that correct procedures are being followed and that ai!equipment is operating properly.

nii

SR300720

Reprinted from Analytical Chemistry, 1964, 56, 2602.Copyright © 19iW by the American Chemical Society and reprinted by permission of the copyright owner.

rAnalysis of Groundwater Contamination by a New Surface StaticTrapping/Mass Spectrometry Technique

Sir: Th» OOOUDOO ••tibod of walytinc for ocjauk

removta inter sample and th«n u»t a procedure such as purge M- !*• wirw wtrt daafMd by hutmf to th* Curia point underand trap foUowed by GC/MS analysis (/). Th« approach, vacuum. A Mtled culture tube was wed to itore and transportwhen u^uaraconnaittucemod^U very expensive. Jejrire to wid too the field, fa icefield, tte ««.«« pl

It i. widely resized that organic compound, in sub- gPJ-g . ^surface water can m.grate into bedrock aa weU as_ undergo Mmplei were ^ md trjiniported to t iaboratoryvertical migration to the earth s surface (2). The quantities for 5 . Tne loading on the wires was followed by removingof these compounds at the surface are often too low for direct duplicate samples at 1-day intervals. Three unexposed wiresdetection; however, a trapping procedure provides a viable transported to and from the field were used as blanks.approach. Mass Spectrometry Analysis, The adsorbed compoundsRecently, we developed a technique using a static collection were desorbed with a Fisher Curie-point pyrolyzer {1.5 kW, 1.1

device for surface geochemicalYiploration for petroleum (3). MHz} in MrieB with an £*tranuclear Laboratories SpectrELThe static collection device consisted of a ferromagnetic wire t ™*01* ma? «?«««»«»«/- Lo*-«ergv electron ionizationto which charcoal had been glued with an inorganic cement. (15 **> w? w minimize frapnentat.cn, A scan rate of 1200_, . , ,. ^ • • «e «e j LI- amu/« and a scan range of 10-240 amu were used in all analvsea.The wire was placed m a support in a 25-35 cm deep hole in D& n ected Ona DEC 1123 computer and stored on disk.the aoii and covered by an aluminum can and the dirt back- Identification of individual species was made based on molecularfilled. After equilibrating with the volatiles from petroleum weight and isotope distribution. Since a major portion of theoccurrences for about 1 week, tbe wires were removed and compounds in the study contained chlorine, high confidence istransported to the laboratory for analysis by Curie-point placed on the identifications.pyrolysis/mass spectrometry in conjunction with pattern Theproceasof mapping fluies of single or groups of compoundsrecognition. The ferromagnetic wire served as a heat source w" completely computerized. The sample sites on a map wereto desorb the adsorbed compounds when placed in the high fim <*Wt™4 " X-Y coordinates. The X-Y dau were thenfrequencv field of the Curie-point pyrolyzer. In this paper mer«ed w'th f*1? mf3 IP«tf"1 P"k ion oun,t3' A file w«

j • L. j L. .L *• •* • /»»c * T." • i. i constructed which was subsequenuy run through a plotting routinewede^nbedhowthestaUctraPpmg/MStechn,quehasalso to ^ thfi flui ma for ^nd.PThe * {been guccessfuUy appbed to the 3Urface detection of low levels procediires were done on the DEC 1123 computer while digitizingof tetrachloroethylene and other contaminates in groundwater. ^id map construction were done on a DEC 1091 mainframe

EXPERIMENTAL SECTION computer. All data were transferred between two computers on. * „, . , - . - , - , «•„„, a °ard line utilizing the NIH transfer program CLINK.

Sampling Site. A site of known tetracmoroethylene (PCE) .contamination at an industrial site near Denver, CO, was used RESULTS AND DISCUSSIONfor the study. The PCE and other chemicals had been introduced ~ T L A " . _ - . - r.t. j* jc_into the groundwat-r (averaging 13.4 m bebw surface) bv **page . The «?t«n»ation of the groundwater occurred fromfrom a waste storage reservoir which had been used in the 1960s. leakage of a waste storage pond. Figure 2 Hlustrates anA number of shallow wells had been drilled in the area to assess idealized cross section of the pond and sampling locations.groundwater movement and PCE contamination. . __T : . . The depth of tbe water table averaged 13.4 m. Movement ofSample Collector. A 358 °C Curie-point wire was used as the the groundwater is to the northeast. SoiJ is predominantly

support for the static collector. The static trap was prepared by day. The sampling scheme was chosen 'o traverse .the sus-AR30072r50/0 c 1984 Anw.can Qwm,&ai Socwiy

_-- a

ANALYTICAL.CHEMISTRY. VOL. se. NO 13. NOVEMBER 1934 * 3903

c>tell

500

1. Schematic of trapping device.

pUnt

7* pond #£-*»V t " 7 —*—————r~T"-: - ,^=^--*-T "••:• --:'- :'nJft*;4lJ—!——!__t.* t-.«.<Hw*g?P-^ .,..___ . __" 'S**'1 o^wct-d*™~Wjt«r Ublc ll 44" ~"~~ " " _7 Tr ?1 "*

it4l*f fnovcfn^nt

Rgur* 2. Id«alz«d crou section of pond and umpiog sit«: •,monitoring w*te.

S3

«S

j*ri?Lki »• . _.wHte p»«»

mm KIIII1. Typical mass spvcaun of cplactad gas-*, Flgun 4. T-fracMcio«thyian» surfao* flux data: x, sampto tocattom;

hactwd ar«a. PCE plum*; O. monitoring w«te.

t w*rte *M« »'•«« PM« ,--Tr. '——'lit MIKT KIIII J

11

Tabl« I. CampaQads Identified by Trapping/MS Analysis ————————————————————————— '. ———— '.for a Dtavtr XadustrUl SiU Table II. Compound* Identified by Static Trappio(/MS

aad la W.ll Water by GC/MSbtoxto* dichlorob*nz«n«

chloroform trapping abovt well 23179 well 23179 GC/MStrim«thylben»o« jon concn,

pn-nol naphthaltnt count* ppbtnchlofotthyUn* carbon t*tr»ch!orid*

_____ t<tracfalMO«thyltn« ________________________ dichloroethylene 12" toluene (m/z 92) 1052 toluene <2

pect*d t«t to w«t edge as well as the north edge of the »ylen« lm/» 106) 853 fyien* ^ 3conttminated jroundwater plume A total of 25 samples were trichloro,thylene 352 tnSowib>-len. ~"dtaken on spacings ranging from 30.6 to 6L m. (m,r 130JFigure 3 shows a typical mass spectrum of the trapped uirachloroeihylene 616 tetrachloro*th>!ene 75.2

vapcrs from $it« 3. The major compound in this spectrum (mis 164)is PCE, The molecular ions plus major fragment ions are chloroform* chloruinrm 3440present, clearly defining the" PCE. Table I summarizes the carbon mrachloride lio __ carbon tetrachlonde <3compounds which were observed in the 25 samples. Figure "" " ' "" 'z4 shows the flui data for PCE using the m • z 164 peak. 'Other compounds interfered with -n ; $3- and J5, .;denufica-The fluxes for PCE in the area studied ranged from 0 to tion could not bjynade. _ _^ _ _ ________ .

U 300 ion counts. Although absolute concentrations are notgiven, ion counts for each site are proportional to the surface . .Table II. The_major difference in compounds identifiedfluxes. The decrease in ion counts was sharp on the plume between the two methods for well '23179 is the absence of_edges. For eiample, site 28 had -ISO counts while the adjacent chloroform using the static trapping mech'od. Even at 15sample 27. had 10 171 ion counts. lhe chloroform molecular ions fragment with the loss of "!A qualitative comparison of the data obtained from :he amu to m. : 8X_85. and 5*7." So molecular »>ns were observe

autic trapping technique above well 23179 to the GCMS. .... for. . chloro_fprri)._ Mapy of the other tragped compounds,purge and trap dnalv-sis uf water from welt 23179 is shown in . primarily from soil bar1""1'"'"'* h:>v* major peaks. In the "i, ;.

SR3007221

r

2804

83-87 range and therefore make identification based on isotope Registry No. C, 7440-44-0; tetrachioroethylene, 127-18-4;distribution in the fragment ions difficult in some samples. water. 7732-18-5.In samples from other sites, the isotope distribution for the T ,.-0 AT>TTT>E> of-rer*

, or, ac Jo— .. L " j L «i_ rt_ till tKA 1 UfvCi \^l i CtlJm/z 83, 85, and 8* were not obscured by the presence of othercompounds, therefore allowing for the identification of the <1> Jf™ M' J'; Erdm«nn' °- 6-; a***'*** J- "• *<*' &** ««.chloroform. Figure 3 clearly shows the m/z 83, 85, and 87 (2) s no. A. Packard, e M tv»f»--fl«s<xr /mwr (U s. aw/ SL-V jpeaks in the proper ratios. All other chlorinated compounds 1982- *° 82-*5.

j • ••• - r .L. - i- L r j (31 Vo<xn«fls. K. J.. Hiekey. J C,. Kluaman. fl W "tnteorativB Gas G«o.occurred m regions of the spectrum where no background micat r hfnque ,£ Patrole,m Exptor.Mn-: A,Se," g Sinterference was observed. - - ~ Sociaty M««itng. s«arti«. WA. 1983.This study clearly .shows that the approach of using the jf{ S f'u' o': Thcr-bT' L.**™*"??**?*? 1979. r2' 12A .. „ .. , -. ..,, o. \ .a ,, KK - " . « - • - . <5) Ksftt'- *•• H': Cn**wn»tt. W.; D«>oan. John. Jr.; UOOy, B, A.; Taylor. G.static collection device with Py-MS offers a cost efficient new K,; w«nti«r. G. An*t, o»m ista. 55. 2210,

approach to the analysis of low level vapors originating fromsoil and groundwater contamination. Most compounds were Kent J, Voorhees"identified with a high degree of confidence. However, the i?S ; Hic]ceypotential use of the collection device followed by analysis with _ ,-,,-. J Konald W. Klusmantandem mass spectrometry or GC/MS would add another ?«f "?™tkof ^ ^ Geochem.Gtrydimension to the analyses and should increase the compound Co orado School of Minesidentification confidence to that of the standard GC/MS well Ooiden' 0™*° S0401water analysis (5). These avenue* are presently being ex*plored. __ - RECEIVED for review May 3,1984. Accepted July 2, 1984.

D.-4 flR300723

Presented at the NWWA/API Conference entitled'Petroleum Hydrocarbons and Organic Chemicals in Ground Water: Prevention, Detection, Restoration'

November 5-7, 1984Houston, Texas

Migration Rates of Voiatilesfrom Buried Hydrocarbon Sources through Soil Media

By Ramon E. BisquePETREX

4565 Highway 93 NorthGolden, Colorado

Truce volattles from gasoline, dieset fuel, and crude oil samples introduced at depth in undisturbed soil media were collected atthe surface to determine upward migration rates. Soil media varied from tight clay containing ten percent free water f 100 C) to drycoUuvial materials. In sllcases trace emanations were detectable at the surface within hours from depths of three meters. Numerousindividual compunds from the$e mixtures were identified and monitored.

The tests demonstrate an effective method for detecting and identifying leaks of hydrocarbons from buried sources. Leaks canbe located by gndding the suspect area with collectors and comparing relative flux rates. Appropriate grid spacing depends on thedepth and volume of the leaks.

One liter of these three test substances introduced at 3 meters depth continues to be detectable at the surface two months afterplacement. The trace volatile; were collected on activated charcoal and analysis accomplished by Curie point mass spectrometry.

The collection-detection system used in the tests describedin thi» paper hag bctn uied in one hundred and wventycommercial aurvtyi for oil mud fax exploration in 25 states.Tract volatilw nachinc th* surftc* from deep oil and gasaccumulation* w«re collected on activated charcoal glued to aCurie point wire placed in * small vial just below the soilsurface. The macs spectra, of these volatile* were computer-analyzed by multivariate statistics and used as a signature or"fingerprint" for differentiating hydrocarbon sources.(Bltqu*, RE. 1983, Klusman. R.W. and Voorhees. K.J. 1983.)Although these surveys hxv* demonstrated the potential ofthis approach and provide voluminous data relating tovariation of hydrocarbon "fingerprints", from geologicallyburied sources, they provide no hint of migration rates. Figure 1. Hydrocarbons wer« introduced at depth via

In anticipation of broad application in detecting buried three inch augered holes after backgroundleaks of hydrocarbons and other volatiles, the tests described (lux was monitored (or ten days.herein were performed to establish a time frame for upwardmigration and provide data on which to base samplingtechniques.

Background readings in and around th* test area were The hydrocarbon fluids were introduced to the bottom oftaken for ten days pnor to tests and throughout the test penod. the hole through a plastic hose, ihe hose was allowed to drainFor th* particular compounds observed, background levels thoroughly from a few inches above the bottom and backvaned from a few tens of ion counts per day to two or three „. filling began, as the hose was slowly lifted, Collectors had beenhundred ion counts. Lower background levels values were placed along radii outtothree_meters from thehole Theseweremesauredindryporouscoiluvialmaterialandthehigherlevels removed periodically and subjected, to mass spsctrometncin a well developed soil horizon over a sedimentary sandstone analysis to follow the build up and attenuation of hydrocarbonIn contrast local readings at ihe surface after introduction of flux at the surface.hvdrocarfaons at depth went as hi^h as several tens i>f Theshapeof the curves showing oui!d-up and attenuationthousands of ion counts per day. of total flux were essentially the same for all the tests. Presence

Gasoline, diesel fuel and a crude oil were tested separately. of the an amply was readily apparent withinjhe first twemy-each from a depth of three meters. Clean holes were power four hour_ period, peak flux .resulted on the third day anddrilled with a three inch auger and sealed until the attenuation was rapid into day five. iFIg '2hydrocarbon samples were introduced. Collectors were placed The 'stain" of molecules in the soil was still detectablearound the holes pnor to drilling and several removed after :he after 60 days. Relative ratios of the component molecules, thedrill in« procedure to detect any changes in background levels. "fingerprint", permits differentiation of the three types of• Fiif. It hydrocarbon sources.

. . • AR3QQ72U2-42' ' ' "•

g ._

lli!UN

Surface anamolies mapped over deep petroleumaccumulations are confined to limited areas that are not

i u_r iMte «a BWI M consistent with models incorporating spherical diffusionfronts. This effect has been observed and discussed by otherswho have examined results of geocbemical methods forpetroleum exploration (Davidson, M. J., 1982),

In summary results of controlled field testa are consistentwith interpretations made from geochemical explorationsurveys and also demonstrate that volatiles from shallow

_____________________ _. _ hydrocarbon sources reach the surface in a matter of hours or-Si?, i r J i s i minutes. Because of strong vertical migration these volatiles'riMiTc./-!.. *"*VmM provide a means of locating leaks and /or guiding drilling

programs designed to retrieve samples for detailed chemicalFigure 2. Build-up and attenuation of volatiles from

gasoline through a sand column and Referencesthrough undisturbed wet clay soil. ,. „., _ ... , .. , ., . ,rtnn . VTe ,7. -,_ * *. ,c » * Klusman, R. W. and Voorhees, K. J., 1983. A NewSee also appended figures (Fig. 4 and 5), r, , .. „ A , .-, , , _, .a a ' Development m Petroleum Exploration Technology. Mines

__.„ .,..,„„_..----.-. - •—-- = — - • Magazine, Vol. 73, No. 3, p. 6-10.

Usually six to ten compounds of these mixtures need be 2) £isque' E" 1983' New G«ochemical Technique Used indetermined to derive a diagnostic fingerprint or signature (U., ™ Denver *****' Western Oil Reporter, June, 1983, p. 23.mass spectrum). The technique developed by Kinsman and 3} Davidson.M. J.. 1962. Toward A General Theory of VerticalVoorhees collects these compounds on activated charcoal. Migration. OH and Gas Journal, June, pp. 288-300.•naiyiss them simultaneously by mass spectrometry andidentifies the source by quantitatively oomparinc tbe Appends*

Th« gwxMtry of th«s« teats wewld indicate thatasorfac* i~«-" ..........•rid spuing of UM collectors woold havt to bt iaaa than U»holt depth (depth of leak) to iiunz* detection of th« anamoly.This requirement ia much leu stringent for a source that wouldberepleni*hedasintheca»eof*continuous]eak. In the lattersituation a plume would develop and concentrations near the•ource would be considerably higher.

Theshape and extent of theplume would beinfluenced by _ground water movement. In the absence of ground water thedepth of unco nsolida ted soil material might also be influentialif the source provided enough fluid to reach bedrock. In thelatter case, pooling or flow on the bedrock surface can occur. Ineither case, grid sampling and comparison of relative flux rateswill provides map indicating the location of the source and thedirection of flow. Drilling costs can be reduced significantlyand in some cases eliminated. - --- .._.__.— Figure 4. Relative flux build-up and attenuation for

The strong vertical migration effectobserved in thesetests . selected gasoline components (See Fig 2(Fig. 3) is consistent with observations in oil and gas of paper)exploration.

Figure 3, Hypothetical diffusion pattern (below) andmeasured surface (lux anomaly (above)demonstrating the "vertical migration"etfect_ .. ^ - Figure 5. Relative flux build-up and atlenuauon for selected crude:

components. (Seefig 2o( paper)

BR300725D-43

r ' "."".. _.____._..,-,. . ,:: r. -- APPENDIX E

flR300726(

SAMPLE TAP

UNITED STATES ENVmONMENTAL PROTECTION AGENCY

NATIONAL ENFORCEMENT INVESTIGATIONS CENTERBunding 53, Bex 25227, DWTVW F«d«fil C«nter

(tower, Colorado S0225

?/EPA

.!-«. 4

n

Project Code

cnj

Station No. Month.'Oay.'Year Time Designate:Corr-o Grab

Station Location

CO o•=: < v :» •«• - w;

. '•* ** ;*•! -* CO

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s_i;v; :: BRS0.072?

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Scrap. N rw

INORGANICS TRAIT1C REPORTCD Cue Hunter,

Sampling Office:

! (Phon-1

'Begin!

J) SAMPLE CONCENTRATION____ Chech OM|

Mcdiiwi CeecMtn© SAMPLE MATRIX

Witet

Shipping Infernwtioii:

Cut Shipped

!0 Sample Description. \ (*, M*rk Volum« L«V«J' c '5! ")r'*> T OnS*mpleBottl«

n«s M*3i* —— ~i*i ' Amrr.;' 3 . 3

" " " 1 Cysni

MATCHES c?c:A::;r SAMPLE sr

flR300729E-3

&\ • }!fc?jpfMg'jaJji-gy ?iifi© Cue Number:

Sample Site Name/Coda:

© Regional Office: _. —Sampling Personnel

• M-JTSC'

-Phone-Sampling Oat*:

ts*5*Ji) *cfi3'

Q Shipping Infonnatioai

Name of Camer

Date Shipped

A^b£ Number

© SAMPLEC(C

LowCM*rfii

© SAMPLE N(Check CWaterSoU/S

l6S&gg*gMfeni8g««a- KJJ K ju* £•*! ;' *•) J 1 ?? yH3Bi ^ ^ ft ONCENTRATION © Ship To:heck One]

roncentrataonim Concentration

Arm:IATRIX mmm imm m^ __ __ ^>n«) _Transerediment Ship To:

© For each sample collected tpof container* used and mark von each bottle.

Number ofContainers

Water(Extractable)Water(VGA)

Soil/SedixnentWater(E*t.'VOA)

Other

•

© Sample Description

__ Surface Water __ Mixed Media

__ G:ounc Vt'dter __ Sobds

•_ , Special Handling Instructions'«- ; »?**Tf £-•*•• *. (fieri "jtZil iO.iJt Id'.i.'-1-

*cify number *$&•• »"' .^ * - **?otuzne level fe~ T jjjj Z '• * *"5

Bw few i?!Approximate K& S-V v.?'

P *- :'"B B/ :".'« ? -33

•* - •-»> . "\

' '• ' *,

> , .© Sample Location

E--4 — -

flR300730

U.S. ENVIRONMENTAL PROTECTION AGENCYCLP Sample Management OfficeP.O. Box II8 - Alexandria, Virginia 22313Phone: 7D3/.5V-249Q - F7S/.557-2<t90

SPECIAL ANALYTICAL SERVICEPACKING LIST

(phone)

t.'""*.

3.*.3.6.7.S.9.10.11.12.13.1«.15.16.

*7-IS.19.

20.

5AS Number

Sampling Office: Sampling Dated): Ship Tot For Lab Use Only

Sampling Contact: 0*t« Shipped* °*te **"*'« R«'d:

Sit* Name/Cod*! , w : IUc«iv*diyr-Attm •'- •'•:. -———————

Sample Swnpte DtKrtotlon Sample OmfitionNumbers - 1** Analysis, Matrix, Concentration Receipt at Lab

For Lab Us* Only

White - SMO Copy, Yellow - Region Copy, Pink - Lab Copy for return to SMO, Cold - Lab Copy

AR30073i

FIELD CHECKLISTBriefing with Project Coordinator

SIGNATURE OF AUDITOR _______________ DATE OF AUDIT.PROJECT COORDINATOR _______________ ..PROJECT NO. _PROJECT LOCATIONTYPE OF INVESTIGATION(authority, agency)

'es_ No_ N/A_ 1. Was a project plan prepared? If yes, what itemsare addressed in the plan?

Yes_ No_ N/A_ 2. Were additional instructions given to project par-ticipants (i.e., changes in project plan)? If yes,describe these changes.

Yes_ Ho_ N/A _ 3. Is there a written list of sampling locations anddescriptions? If yes, describe where documents are.

Yes_ No_ N/A_ 4. Is there a map of sampling locations? If yes, whereis the map?

Yes_ No_ N/A_ 5. Do the investigators follow a system of accountabledocuments? If yes, what documents are"accountable?

flR300732

Yes_ No_ N/A_ 6. Is there a list of accountable field documentschecked out to the project coordinator? If yes,who checked them out and where is this documented?

Yes_ No_ N/A_ 7. Is the transfer of field documents (sample tags,chain-of-custody records, logbooks, etc.) from theproject coordinator to the field participants docu-mented? If yes, where is the transfer documented?

r"

E—7 flR300733

FIELD CHECKLISTField Observations

Yes_ No_ N/A_ 1. Was permission granted to enter and inspect thefacility? (Required if RCRA inspection)

Yes_ No_ N/A_ 2. Is permission to enter the facility documented? Ifyes, where is it documented?

Yes_ No_ N/A_ 3. Were split samples offered to the facility? If yes,was the offer accepted or declined?

Yes_ No_ N/A_ 4. Is the offering of split samples recorded? If yes,where is it recorded?

Yes_ No_ N/A_ 5. If the offer to split samples was accepted, werethe split samples collected? If yes, how were theyidentified?

Yes_ No_ N/A_ 6, Are the number, frequency and types of field mea-surements and observations taken as specified in theproject plan or a's directed by the project coordinator?If yes, where are they recorded?

Yes_ No_ N/A_ 7. Are samples collected in the types of containersspecified for each type of analysis? If no, whatkind of sample containers were used?

E_ •i

.(feetf

N/A__ _ 8. . Are samples preserved as required? If no or N/Aexplain. ' '

Yes_ No_ N/A_ 9. Are the number, frequency and types of samples col-lected as specified in the project plan or as direc-ted by the project coordinator? If no, explain whynot?

r1 Yes— No— N/A— 10- Are samples packed for preservation when required

(i.e., packed in ice, etc.)? If no or N/A, explain

*'

Yt$ 'k N/A H- Is *»»Ple custody MlnUlntd at all times? How?

flR300735

FIELD CHECKLISTDocument Control

Yes_ No_ N/A_ 1. Have all unused and voided accountable documentsbeen returned to the coordinator by the teammembers?

Yes_ No_ N/A_ 2. Were any accountable documents lost or destroyed?If yes, have document numbers of all lost ordestroyed accountable documents been recorded andwhere are they recorded?

Yes_ No_ N/A_ 3. Are all samples identified with sample tags? If no,how are samples identified?

Yes_ No_ N/A_ 4. Are all sample tags completed (e.g., station no.,location, date, time, analyses, signatures of sam-plers, type, preservatives, etc.)? If yes, describetypes of information recorded.———————————————— '1

Yes_ No_ N/A_ 5. Are all samples collected listed on a chain-of-custody record? If yes, describe the type ofchain-of-custody record used and what informationis recorded.

Yes_ No_ N/A_ 6. If used, are the sample tag numbers recorded on thechain-of-custody documents?

SR300736

Yes_ No_ N/A_ 7. Does information on sample tags and Chafn-of-Custody ''Records match?

Yes_ No_ N/A_ 8. Does the Chain-of-Custody Record indicate the methodof sample shipment?

Yes _ No_ N/A_ 9. Is the Chain-of-Custody Record included with thesamples in the shipping container?

Yes_ No_ N/A__ 10. If used, do the sample traffic reports agree with.____. ._..;,,..», .the (ample tags?

Yes No_ N/A__ 11. If required, has a receipt for camples been providedto the facility (required by ftCRA)? Describewhere offer of a receipt Is documented.

Yes No N/A 12. If.used, are. blank samples identified?

Yes_ No_ N/A_ 13. If collected, are duplicate samples identified onsample tags and Chain-of-Custody Records?

Yes No N/A 14— If used, are.spiked samples identified?

fBR300737

Yes_ No_ N/A_ 15. Are logbooks signed by the individual who checkedout the logbook from the project coordinator?

Yes_ No_ N/A_ 16. Are logbooks dated upon receipt from the projectcoordinator?

Yes_ No_ N/A_ 17. Are logbooks project-specific (by logbook or bypage)?

Yes_ No_ N/A_ 18. Are logbook entries dated and identified by author?

Yes_ No_ N/A_ 19. Is the facility's approval or disapproval to takephotographs noted in a logbook?

Yes_ Ho_ N/A_ 20. Are photographs documented in logbooks (e.g., time,date, description of subject, photographer, etc.)? --,

Yes_ No_ N/A_ 22. Are sample tag numbers recorded? If yes, describewhere they are recorded.

5-12 BR300738

nYis_ No_ N/A_ 21. If film from a self-developing camera is used, are

photos matched'with logbook documentation? i

Yes_ No_ N/A_ 23. Are calibration of.pH meters, conductivity meters,etc., documented? If yes, describe where this isdocumented.

Yes_ No_ N/A_ 24. Are amendments.to the project plan documented? Ifyes, describe where the amendments are documented.

rL

flR3007{39

FIELD CHECKLISTDebriefing with Project Coordinator

Yes_ No_ N/A_ 1. Was a debriefing held with project coordinatorand/or other participants?

Yes_ No_ N/A_ 2. Were any recommendations made to the project par-ticipants during the debriefing? If yes, listrecommendations.

t^ ^ -j>

i

E"14 SR30071iO

«

DOCUMENT AUDIT CHECKLIST

PROJECT NO. DATE OF AUDITPROJECT LOCATION _____________ SIGNATURE OF AUDITORFILE LOCATION

Yes_ No_ 1. Have individual files been assembled (field in-vestigation, laboratory, other)?Comments:

Yts_ No__ 2. ... Is tach file Inventoried?CoMtnts:

Yes_ No_ 3. Is there a list of accountable documents?Comments:

Yes No 4. Are all accountable documents present or accounted~~ ~~ for?

Comments:

Yes.__ No__-- 5. _ Is a document numbering system used?Comments:

flR3007'l*l

Yes_ No_ 6. Has each document been assigned a document controlnumber?Comments:

Yes_ No_ 7. Are all documents listed on the inventory accountedfor?Comments:

Yes_ No_ 8. Are there any documents in the file which are noton the inventory?Comments:___

Yes_ No_ 9. Is the file stored in a secure area?Comments: 0

Yts_ No_ 10. Are there any project documents which have beendeclared confidential? nComments:

Yes_ No_ 11. Are confidential documents stored in a s.ecurearea separate from other project documents?Comments: . ;•

L

si-

Yes_ No_ 12. Is access _to confidential files restricted?Comments:

Yes No 13. Have confidential documents been marked or stamped~ ,_._ . Confidential11? ...____.. ....

Comments:

Y«*__ N0— 14- I$ confidential information Inventoried?Comaents:

Yes_ No_ 15. Is confidential information numbered for documentcontrol?Comments:

Yes No 16. Have any documents been claimed confidential under~~ "~ - • • T$CA?Comments:

E_17 flR3007ii3

TRANSMITTAL RECORDFor UM of thl* form, mm Aft 34O-1S;th« proponent «9«ncy iiTAGO.

1. SECURITY CLASSIFICATION 2. SHIPMENT NO,ORIGINAL

(fterf)3. TITLE/FILE IDENTIFICATION AS OF DATE SHIPMENT DATE

t> lire T»nt-YE AR MONTH DAY YEAR MONTH

07DAY

14-UTHORITY FOR SHIPMENT 7. NUMBER OF RECORDS TRANSMITTED

S. PERSC(] J TO CONTACT (Nome and telephone) S. REQUIREMENT CONTROL SYMBOL CAR 335-15)

10. TYPE OF MEDIA TRANSMITTED

HARD COPY PUNCHED CARDS CASSETTESMICROFILM PHOTO FICHE

11. NUMBER OF BOXES/PACKAGES 12. NUMBER OF ITEMS

13. _ METHOD OF SHIPMENT

COURIER FIRST CLASS PARCEL POSTEXPRESS MAIL REGISTERED

14. SHIPPED TO 16. SHIPPED

j_2T u T e ' „ ,end nrfurn copy (o tender)

14a TYPED NAME AND TITLE OP RECEIVER ISc. TYPED NAME AND TITLE OF SENDER

*b. SIGNATUE OF RECEIVER ANfc DATE ISb. SIGNATURE OF SENDER . /

16. SPECIAL INSTRUCTIONS

17 T»Pb COMPONENT USED fFor magnetically recorded data!

18. REMARKS

DA FORM 200, APR 83 EDITION OF FEB ?s WILL BE USED UNTIL EXHAUSTED fruj.opo: