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BRITISH STANDARD Methods of test for Soils for civil engineering purposes Part 3. Chemical and electro-chemical tests BS 1877: Part 3: 1990 Inoorporating ‘Amentiment No. 1 E BS 1377 : Part3: 1990 Issue 2, April 1998 Foreword ‘ThisPartof BS 1377 hasbeen prepared under the direction of the Road Engineering Standards Policy Commins. tina revision of clause $ of BS 1377 : 1975 whichis euperesded by amendment. 8S 1377 was frst published in 1948 and fret appeared in metric form in 1978, 8S 1377 : 1975 which has now been withdrawn fs replaced by the foliowing Parts of BS 1377 : 1900: Part 1. General requirements and sample preparation Port 2. Classification tarts Part. Chemical and alactto-cherica taste ert 4, Compaction-reated tests Part. Compressibiliy, pormenbitty and durability teats art 8. Consolidation and permepbitty tests in hydraulic cells and with pore pressure measurement Part7. Shear strangth teste (total seas) Part 8. Shear strength tests (eftective stress) Part9. In-situ tosts Foference should be made to Part forfurther information ‘bout asch of the Pers. Inthis Part of BS 1277 thotest methods doscribadinthe 1975 ‘dition have been reteined with some modifestion, and tha {oltowing methods of test have been introduced: (8) determinstion of oss on ignition; (0) dotermintion of corbonete coment; (e) determination of chloride content; (G) determination of tral dissolved solids content; (6) determination of electrical resistiviey (1) determination of the redox potential: ‘Sample test form are shown in Appendix A ‘thas boon assumed in the drating of thie British Standard that the execution ofits provisions is erarusted 0 ‘eppropriately qualified end experienced people. Caution. Attention should be given tothe potemtially hazardous nature of certain chemicals by folowing recognized practice and taking the appropriate precautions. “These include the use of a fume cupboard when using ackés ‘nd other texie chemicals ‘Special core and preceutions may benecessary when dealing ‘wath contaminated ground (see DD 175) Compiiance with a Grtish Standard does not of iteaf confer Immunity from legat obligations, Issue 1, April 1996 BS 1377 : Part 3: 1990 A Summary of pages ‘The following table identifies the current issue of each page. Issue 1 indicates that a page has been introduced forthe first time by smensimen. Subset issoe numbers indicate an pasted page Vertical sidelining on replacement pages indicates the most recent changes (amendment, addition, deletion), ase Tore Faae Teaoe Front cover 2 2 original Inside front cover 2 23 original a 1 a 2 b blank 25 original L original 26 original 2 ‘original a7 2 3 original 28 original 4 original 29 original 5 original 30 original 6 original at original 7 original a2 oxiginal 8 2 38 original 8 2 at original 10 2 5 2 u 2 % 2 2 2 aT original 1B 2 8 origina 4 original 9 original 6 2 40 original 16 original 4 original W ‘original 2 oniginal 8 original Inside back cover original 9 original Back cover 2 20 original a original Contents Foreword ‘Commitoes responsible Methods 1 Scope 2. Definitons 3. Determination ofthe organic matter content 31 Gonezal 32 Apporatus 33 Reagents 34 Procedure 35 Caleulations 36 Testreport 4. Determination of the mass oss on ignition 41 Generat 4.2 Apparatus 43 Procedure 44 Calculations 45 Testreport 5 Determination ofthe gulphate content of soil and ‘ground water, 5.1 General [5.2 Preparation of soll and its acid extract {5.3 Preparation of soll end ts water ext ‘5 Preparation of ground water for testing 535 Gravimetric method for analysis of acid or water ‘extract or ground water 56 lon-exchange method for analysis of water ‘extract or ground water 5 Determination ofthe carbonate content 81 General 6.2 Preperation of sample 6.3 Rapid tretion mothod 84 Gravimetric method 7. Determination of the chloride content 7.4 General 7.2 Determination of water-soluble chloride content 73 Determination of acid-soluble chloride contant Pog Inside front cover Back cover 2 2 2 3 14 14 4 6 7 BS 1377 : Part3: 1990 {8 Detormination of total dissolved solids 8.41 General 85 Test roport 9. Determination of the pH value 8.1 General 82 Apparatus 8.3 Reagents 8.4 Preparation oftest specimen ‘95 Eloctrometic method of pH determinstion 3.6 Test report 10. Determination of resistivity 101 General 410.2 Measurement of resistivity: disc electrodes smothod 40.3 Measurement of rasistivty: Wenner probe ‘method 10.4 Measurement of resistivity: open container method 11 Determination of the redox potential 11.41 Gonoral 112 Apparatus 11.3 Reagents 11.4 Procedure 115 Calculations 118 Test report Appendix. A Typical test data and calculation forms Figures 1 Ion-exchange column for sulphate determinstion CConstant-head device for ise with ion-exchange column 3° Circuft diagram forresitivitytestusing Wenner probes 4 Container for resistivity tests on saturated granular soll BRUISES 8 8 0 at BS 1377 : Part3: 1990 Method 1 Scope ‘This Part of BS 1377 describes tost methods for determining the amount of chemica! substances, including organic. -ettar, in samples of soil and ground water. The determination of some electrochemical and corrosivity properties of soil and water semples is also included. NOTE. Th ties ofthe pubestions referred 0 inthis standard ste onthe inside back cover. 2 Definitions For the purposes ofthis ant of BS 1277, the definitions given In BS 1377 : Par t apply together with the following. 2.1 Gitration. The addition of a solution from e graduated ‘uretteto 2 known volume of @ second solution, until the chemical reaction between the two is completed. the strength of one of the solutions is known, thatof the other can bbe celculated from the volume of liquid added. 122 indioator. A substance which is capable of giving a clear Visuslindication ofthe comptotionofe chemical resction na ‘solution Being strated, usually by mesns of ¢ change in ‘colour. 2.3 plivalue, The logarithm to bese 10 ofthe reciprocal ofthe ‘concentration of hydrogen ions in an aqueaus solution t provides a meesurs ofthe acidity or alkalinity of the solution ‘on a scale reading from0 to 14, on which 7 represents ‘euteality. 24 reslathviy (of sail. The electrical resistance, in ohms per Lnitlength, ofa column of soil of unit aree ofeoss section. In ‘this standard resistivity is expressed in ohm metres, NOTE, This ito conform wih ! unas. Te eustomary unit Sem, ‘equsltoootam. 25 redox potential (reduction/oxidation potential) A relative measure, expressad in milivolt, of the reducing oF ‘oxidizing capacity of sol, usually increasing with inereasing ‘oxypen content. 3 Determination of the organic matter content 3.1 General procedure covers the determination ofthe porcentage _by dry mass of organic matter presant ina soll. The mathod, which uses dichromate oxidation, isknown as Walkley and Black's method. tio in enema! acting requires that uplicta should be tasted. In ach ofthe ott methods he ‘specie ‘meaturementof oniyoneveie ofthe overal aes describes his ‘i enony procheal applications to make {ho rolabity ofthe reuts, Gldanon on the tar ot Iorutererts requires and te treatment oft results obtained Deyone the scope ofthe Part ofBS 1977 ‘Soils containing sulphides of chiorides have baen found to ‘ive high results by this procadure. Methods forchecting for the presence ofthese compounds, and proceduras for their removal betore testing if they are prasant, ar included. ‘The requirements of Part 1 of this standard, where ‘appropriate, shal apply to this test method. 32 Apparates 3.2.1. Drying oven, capable of maintaining 8 tempereture of 50+ 25°C. 322 Balance, readable to 1 g 328 Balance, readable t0 0.001 g 3.24 1 volumetric fast. 325 Two25 ml burettes, graduated 60.1 ml. 32.6 10ml pipette and'e 1 mL pipette, each fitted with @ rubber teet. 32.7 Two conical flasks of 600 mL capacity. 32:8 200 mL and #20 ml graduated measuring cylinders. 3.2.9 Desiccator (a conveniant size is about 200 mm to 250 ‘mm in diameter) containing anhydrous silica gol. 32.10 Glass weighing boti, approximately 25 men in diameter, 50 mm high and fitted with a ground gleesstopper. 82.11 Testsieves,2 mm and 42S um apertute sizes, with 32.12 Semple dividers ofthe multiplesiot type (rite boxes). having widths of opening of 7 mm and 16 mm, £32.18 Pestle and mortar, ota suitable mechanical crusher. 3.2.14 Wash bortie, preferably made of plastice, containing distilled water. 8.2.45 Gless boiling tube. 8.2.16 Fitor funnel, of approximately 100 mm diameter. 3.2.17 Filter papers, of a diameter appropriate to the sie of the funnel : medium grade (e.g. Whatman No. 40) and fine ‘arade (e.g. Whatman No. 42). 3.2.18 Blue ftmus paper. 3.3 Reagents 12.3.1. Goneral. All reagents shall be of recognized anatvtical reagent quality NOTE, Where accurately standardaed solutions are required tmey 'bemore convenientta abun thar already rencarded in ancentrateoiorm anda dilutethem as necessaryin accordance win ‘the manutoetutere instrustions. 38.2 Potessium dichromete solution, ({KiCtz0) 0.167 moiN}. Dissolve 49.035 g of potassium dichromate in Is the total volume of ferrous sulphate solution used in the standardization test (see'3 4.1) in mL. 252 calwewthpranag oft oa st ame dering tm rm tse ome ato ton ror n= vee im teil oy mest sore nh mak mateo hese pening th 2 mm tetsive ina 283 cainetbe soca of eave mtr rertin Irtclonctherotepwsia tan en fora desurinaton tam hoon ne ea povenoge organic mater conten S22 won |My is the mass of soil used in the test {in gl. Wort nena onto sr iar cata tees a Smear sta nee este oin Seon een ae eee et nde acinar gem sees Rese te ES estate 28.4 If duplicate specimens have been tested, and ifthe vidual results expressed as a percentage of orgenic mater differ byno morethan? %, calculate the mean cesult. ltthey differ by more than 2 %, repeat the test starting with ‘wo new representative portions of sil. 88 Testraport ‘The test epor shal stata thatthe test was cenried out ‘accordance with clause3 of BS 1377: Pan 3: 1980, and shall contain the following information: (a) the method of test used; (0) the average organic matter content presenti the soit fraction passing a2 mm test sieve to the nearest 0.1 % of the original oven dry mass of soil; (ch the percentage by dry mess ofthe original sample passing the 2 mm test siove tothe nearast 1 %; (d) tt sulphides or chlorides have bean dentifiad inthe sl, this chal bo stato: (6) the information required by 9.1 of BS 1377 : Part 1: 1990. BS 1377 : Parts: 1990 4 Determination of the mass loss on ignition 41 Gononat This cause describes the procedure or determining tho proportion by mass that slot fram asa by ignition ata specified temperature. NOTE. Geod pratcnin chemical toting ecules thet duplicate specimens should beste. In euch ofthe taut metioce the ‘essuromantofaniyonevaive ofthe overall vsutis cenribe. is ‘ecogeizodthattisnecestary ic many pasta eppfeationsto make {number afte inordert> obtain amesavelue end an ingestion ot ‘he relat ofthe reals. Guidecew on ha number of ‘eesurerner's rogues and thereat ofthe eeeuts abainad beyond te ape of hia Par of BS 1377. ‘The mass loss on ignition i related tothe organic content of certain soils, such as sandy soilsthat contain tla orn clay, ‘of chalky material, peats end orgenic clays conteining more ‘than about 10 % orgenie matter. However it should be recognized that, in some sols, factors unrelated ro organic content could be responsible for the major proportion of the mage lose on ignition. ‘The requirements of Part} of this standard, where appropriate, shall apply to this rest method. 42 Apparatus 4.2.1. Orving oven capable of maintaining a temperature of 504 25°C. 422 Balance, readable to 1 9 423 Balance, readable to 0.001 g. 424 Dasiccator, comaining anhydrous silica gel 4.25 Tost sieves, 2 mm and 426 ym sporture sizes, with receiver. 4.26 Posto and mortar, or 8 suitable mochsrioe! crusher 42.7 Sample dividers of the muttipie-siot type (rife boxes), having widthe of opening of7 mm and 15 mm, 42.8 Crucible or similar container, of about 30 mL capacity. 42.8 Elootric mute furnace, copsble of maintaining a temporsture of 40 + 25°C. 43 Procedure 43.1 Preparation of erucible 4.2.1.1 Boforestarting each series oftests, carry outa teston ‘the empty erucble or container as described in 43.1.210 reery ‘43.12 Placa the crucible in the mutfe furnace, heat 10 {440 = 25°C and maitzin the temperature for 1h. 43.13 Remove the crucible from the furnace and allow it to cel to room temperature in the desiccator. 4.3.14 Weigh the erucible tothe noarest 0.001 g (md. BS 1377 : Part3: 1990 43.2 Preperation of test specimen 43.2.1 Prepare each tost specimen for anslysis from the Jaboratory sample as describedin4.3.2.2t0 42.28. ‘48.2 Obtain an initial sampte as described in 7, and of the ‘approximate size specified in 7.5, of BS 1377 : Part: 1990. 432.3 Dry this sample inthe oven at60 + 2.5°C,andeoo!to oom temperature in the devicestor. 4324 Weigh thesampiotothencarest0.1 %andrecord the mans m (ing) 4328 Sievethosampleona2 mmtestsievefifeppropriete, ‘guarded by ates sieve oflargor aperture), and crush retained ‘particles other than stonesto pass the 2 mmtast sieve 43.2.6 Reject the stones ensuring that no fine meter ‘adheres to them, 9. By brushing. Record (in g) the mass of the sample pessing the 2 mm test slave tothe nearest 0.1 % (m,). Toroughourthess and subsequent operations ensure ‘that there is no loss of fines, 43.2.7 Divide the material passing the 2 mm sieve by successive rifling through the 15 mm divider to produce @ ‘sample weighing at lesst 10g. 43.28 Pulverizethis samploso thatit passes the 42S um test 43.29 Subdivide the sample by rifling on the 7 mm divider 10 obtain test specimens each weighing approximately 5g. ‘Throughout this and any subsequent operation mix the ‘material avilable thoroughly before any division ond avoid segregation during rifting 43.2.10 Place eech specimen in a prepared crucible and dry inthe oven atatemperatureof50 + 2.5°C. The specimens are deemed tobe dry when the differences in successive weighings, carried outat intervals of4 h, do notexceed 0:1 % ‘ofthe original mass oftho sample, 43.11 Allowthespecimensto coottoroom tomperaturein ‘tha dasicostor and weigh each erucible to 0,001 g fm ‘432 Jgnition of soil 4.3.3.1 lgrite each ost specimen as described ing3.2.2t0 43x 49.32 Prace the crucible with soit in the unheated muta, furnace, heat to 440 + 25°C, end msintain this temperature {or @ period of not lass than 3h, or until constant mass is achieved. NOTE. The period required for ignition wil vary with the nype of 08 nd ie of vamote 43.33 Remove the crucible end contents from the furnace {nd low to cool to room temperature inthe desievator. 4.334 Weigh the crucibie and contents tothe nearest 0.004 g (ma). 44 Calculations NOTE. Sea form 310) of eppendix A. ‘44.4 Calculate the percentage ofthe origine! sol semple ‘passing the 2 mm tost sieve from the equation: fraction finerthon'2:mm-= 72 x 100, where ‘mis the original dry mess of sample (in ‘mis tho mass of sample passing the 2 mm sieve ting). 442 Cafculeta the mass oss om ignition, LOL asa orcantoge ofthe dry mass of sil passing 22 mm vest sieve fromthe equation: where _mig the mess ofthe crucible and oven-dry soil specimen, tingl: ‘mais the mass of the crucible and specimen after fing: mis the mass ofthe crucible [in gh. 45 Test report The est report shall state thet the test was caried out in ‘accordance with clause 6 of BS 1377 : Part 3: 1990 and shall contain the following information: {} tho method ofrest used; {b) the mass loss on ignition ae a peteantage ofthe si! fraction passing the 2 mm test siave to two significant figures: (c} the percentage by dry mass-of the original sample passing the 2mm test sieve, tothe nearest 1%; [q) the information required by 8:1 of BS 1377: Part 1: 1990. pion 5 Determination of the sulphate content of soll and ground water 5.1 Goneral 5.1.1 Principle, This clouse deseribos procedures for determining the sulphate content of eal and qraund water. The results obtained give the sulphete content atthe time ot sampling oniy. ‘Acid-toluble sulphates include a naturally occurring. ‘sulphetes with rara exceptions. Calcium sulphate, the ‘sulphate salt that is most commonly faund, has low solubility in water. 5:12 Types oftest Procedures are decribed forthe detominaton of the flowing: NOTE. Good rain nhac ting require that ups ‘pecimoe shoud ened nach of bua ose ‘moguedtetn neesayhinanyprctapeeatorst mate at rman rato Spero ‘rari oftntsn rir iocnna ren alu tne inaon ct ‘feraoiny of erat. lcunon sae nar of ‘eauraria oq andth Wester reat tide Styonatne scape tana Fan fone sacar (a) theacidaclubleulphate content toi (also refered {oanthetotal sulphate content for which anacg tract frst prepared (0 82) (0) thewetar soluble supheta content of sol for which a waar wavactia Ft prepared (ee 3): OTE the supra reentin he oi pradonaty the talcum sk, th total saphte contre Setelond nbc aly ave a milacng od persia lng oe Ager to conor snmenreanizod maar rng om the bruce of aes Incans whee ha il eps exons Gb % tie svogonae atten obs wha content ote 2to wersalrnseouidb etre est pate iss onsite preset how ky wl emia {he ndpnace corer fhe aumous nc does rat ran {gl Suphaeconntsn econ ofthe fpurein chs ate ccinirththe gourd wrarasdetrminadin hair erore iret prosnne afar end more hrf phate at {c) the dissolved sulphates in ground weter (08.4). Soils containing sulphides may require special attention. NOTE. Sal conaing wipes. The ald croton manag Surin acne cotont of oso etna cet and sryaalen nen bese anohe een ros (eosnomtob-04 ¥nspnison we prem ESscemeyocdinnthlong tort poaiensadonel saute ‘beproere ofsuhiceis uaesad andthe pane onaaten ot iRelom behavenietona oiconara(e or oamprintacacct refereedoah het iphurcntetahulbe assed oy ihe Iratod pvr 187 he rare heer waco {dino ul ie aclgaoine, npr conerebom mpg {srw ot erarape 80g ¢ means fhe mau of eaphde set and oan bora tngtar ek 1.3 Methods of analysis. Two methods of analysis are eacribed: (a) the grevimatic method for acid antrocta wate cisracte and ground water samples eo 88 (0) the ion-exchange proceaure for water waracts and ground wera samals only (08 88). Inthe gaviretic method barium chloride soltonis added {0 te acd or water extract andthe precipitate of barium suphota i colecte, cried and weighed. The sulphate contentisthoncalulted romthemassofthemateia used intheanayais andthe mana ofbarum eulpbatepresptated. In the fon-exchenge procedure the water axtract orthe ‘sample of ground water is peesed through a resin ion- ‘exchange column and the quantity of anions present it ‘measured by titration ageinsta standardized solution of ‘so6ium hydroxide. This method cannot be used Ifthe eofl or {round water contains anions of other strong etic, such as chlorides, nitratas and phosphates, NOTE. Me pressnce or otherwiae of ntrtrig anions shouldbe Investigated before electing the approprige method. Mere prvence ofother anions prectuces ti use ofthe ion-exchange twathod the supiate conten of sol-wateremtect endl his ‘round water can be determined grovimeticaly ax described mB. BS 1377 : Part3 : 1990 ‘5:14 Anernativecombinations ofprocedures. Theres some ‘lexbiliy inthe selection of the method of anaiysison a given. typeof sulphstes extract. An cid extract from a oil sample is “analysed bythe gravimetric method, but a water extract may ’be analysed either by the gravimetric method or by the ion- ‘exchange method. A sample of ground water may be ‘analysed by either method, 5.2 Preperation of soll and is nei extract ‘The requirements of Part 1 ofthis standard, whore ‘appropriate, shall apply to 521 Apparetue 52.1.1 Apparatus for preperation of test specimen 5.2.1.1.1 Drying oven, capeble of being controlled 10 ‘maintain stemperaturerange of7§ °Ct080 °C, ae wal asthe range 105 *Cto 110°C. 52.1.12 Balance, readabieto 1 g 52.1.1 Balance, readable t0 0.001 g. ‘52.1.1 Desiceator, containing anhydrous silica gel. 5.2.1.1 Test sieves, 2mm end 425 ym aperture sizes, with receiver. 5.2.1.1. Postie and mortar, or aquitable mechenicel crusher. 821.17 Semple dividers of multiple stot type (rifle boxes), having widths of opening of 7 mm and 18 mm. {52.1.1.8 Glass weighing-botte, approximstely 60 renin diameter, 25 mm high and fitted with a ground-gless stopper. 5.2.1.1.8 Red litmus paper. 5.2.1.2 Apparatus for proparing acic-soluble sulphate extract. 52.1.2.1 Two500 mL conical beakers with glans rode and ‘cover glassos. 52.1.22 Etectric hotplate, capable of being controlled 10 boil the contents of the boskere. 2.1.23 Buchner funne|, of abou 100 mm dlametar. 5.2.1.24 Vacuurn filtration fash ofabout 500 ml. capacity, to take the funnels. 52.1.28 Fiter papers. of medium grede (e.g. Whatman No, 40), hardened medium grade (e.g. Whatman No. 640) nd fine ‘grade e.g. Whatman No. 42) 0 ft the funnels. 62.128 Source of vacuum, 6g. efter pump. 5.21.27 Length of rubber veouumn tubing, to fit the vecuumn ‘bump and fier flask. 52.128 Twoglees rods, about 160 mm 0200 mm iongand 3mmto'5mmin diameter. 82.12.98 Wash bottle, preferably made of plastics, containing dated woter 5.2.1.2.10 Glass filtor funnel, about 100 mm diameter. 82.1.2.14 Dropping pipette, 10 mL capactty. 5.2.1.2:12 Ambercoloured glass container, 851377: Part3:: 1990 ‘822 Reagents 522.1 General Allreagents shall bof recognized analytical reagent queity. NOTE. Whar accurately standa-ized solutions are required may bbemore convenient io obain them already standarczed in Concentrated ormandto lute hem ee ceserseryinncordanco wih She manufocurers insvuctions. {5222 Hydrochloric acid, 10 % (vv solution, Dilute 100 mL. of concentrated hydrochloric acid (relative density 1.16) 0 1 Leth ditled water. 82.23 Ditute ammonia soluvion. Diute 500 mL of ammonia {folative density 0.260) to 1 L with distled water. 6.2.24 Sifver nlirale.0.5 % (VV) solution. Dissolve 0.5 g of silver nitrate in 100 ml. of distilled water. Store the solution in an amber-coloured glass container. 6228 Concentrared nitric acid devsity (1.42 girl). $2.26 Distilled water, ofa purty complying with 8.1 of BS 1377 : Pare: 1990. 1.23 Preparation of test specimen ‘52.3.1 Propere each test spacimen for analysis from the laboratory sample as given in8.2321052.3.11. {5232 Obtain aninkial sample as describedin73, andofthe epproximate size specified n 75, of BS 1377 : Part 1: 1990. 523.3 Drythie samploinths oven atatomporsturebetween 178°C and 80°C and allow to coal te room temperature inthe desiccator. NOTE. Sols consininsuiphatesinthe form of gypsum onewererot {ryetiaation esta above to bpelieg omer. 23.4 Weighthasampletothe nosrest0.1% and record the ‘mass m tin). 18235 Sievethesample on a2 mmtestsiove it appropriate, ‘guarded by atest sieve of larger aperture). andcrush panicles ‘other than stones to pass through the sieve. [NOTE Ria stsurnod that any matrilcotainadonthe2 mmtestaleve ‘walnotconaineuphaos. Ths sgeneratytue bu sralnsoiemay {ortnn tp of gypsum leger nan 2 min clarmeter andi euch {ison e gypturn shouldbe removed by hard, crushed to pass 8 ‘nm tes reve ond incorporatedin the ration passing the neve. 82.8 Reject the stones ensuring that ne fine material adheres to them, eg. by brushing. Record (in g) the mass of ‘the sample passing the 2 me teat sieve to the nearest0.1 % (im), Throughout these and subsequent operations ensure ‘thet there i no loss of fines. 8.2.3.7 Divide the material passing the 2 mm sieve by ‘successive riffing through the 15 mm divider to produce a ‘sample weighing approximately 100 9. 62.3.8 Pulvorizethiseomplesothatit assoc the 428 nm tost sieve. Throughout this and any subsequent operation, mix the material thoroughly befora any division and take care to _nvoid segregation during riffing. 8.2.39 Subdivide the sample by successive riffing through ‘tha 7 men divider to obtain test specimens each weighing ‘approximately 10 g Issue 2, April 1996 1523.10 Place exch spacimen in a glass weighing bottle and dry in the oven at a temperature of75 °C. The specimens are ‘deerned t0 be dry when the differences in evocessive ‘woighings atimervals of 4h do not exceed 0.1 % of the ‘specimon mass. 523,11 Allowthe specimenstocoo|t0roomtempersturein the desiccator. 5.24 Propacation of acid extract 5.2.41 Obtain the acid exact forthe determinstion of the ‘otal sulphate content from each ofthe prepared specimens. as givenin5.242105245. . 82.42 Weigh the weighing bottle containing the dried test spocimen to the nearest 0.001 9. 5.2.42 Transfer representative sample ofabout2 ginmaxs {200 nate) to # 500 ml. backer, rewaigh the weighing bosle ‘and calculate the mass (rm) ofthe sample by difference. NOTE. The mass ofsarnpeo use depend. onthe amount of sulphate ‘rework. ideally a tee should b chosen at vl produce & recite f baru eiphate weighing appraximanaly 029. 5.2.46 Add 100 mL of 10 % hydrochloric acidto the sample, taking care frothing occursto ensure that no material islost. NOTE. Matarie comtasiog aulphies wil ralaasa HS 00 ‘tflcation ne tniscanbe detect by kx snel inthasa case there Wadangertnathis procedure wlloverestimatethe wiphave content Decaues of euiphide ondation W thermal concana ephis, sha Gomi otne sin 8360 faakr anche boing Ramove trom the heat eourea and wil ering the el ol {sprinkle the weighed analyte earpleon ta the aid. 5.2.45 Coverthe besker witha cover giass, boll, and simmer ‘Gently for 15 min inafume cupboard. Ringethe underside of the cover glass back inta the beaker. Issue 2, April 1996 BS 1377 : Part3: 1990 4s rie tao ta NOrD nas fered $324 pamitingontpues de yet 1tnra nore mate 24 tengo Be mer riaetbr case ak fete So Tne ripeermemremdesvemtte — sanaettegt hi absence of turbidity when a drop is added to a small sscfenermtetiter Cserhevage wn $228 Teaneinnne gear {he fre and analyse the Sitrate as described in 5:3. 55 ry when the differences in uccessive weighings at Forsots tat ‘conn Intervals of 4h do not exceed 0.1 % of the specimen mass. qanties, eg. certain tropical residual sols, te sesquioxises ‘5.3.26 Allow the specimen to coo! to room temperature it shouldbe preciptata before proceeding wth the sulphate the desiccator. analysis 28 folors, 33.3. Preparation of water extract 8) Add a few drops of nite acid while the suspension 5.3.31 Obtain the2: 1 water-soil extract forthe continues to boi determination of the water-soluble sulphate content from ) Add ammonia soliton slowly (preferably fom a ‘ach ofthe prepared specimens as given inB.3.32t0 53.3.6. tural), with constant tring tote Boling Soluion 543. Weigh aaample of 50.00 gon awetch gles and nil he sesquiordes ara prociptaied and red muss favtie nrc cuenendervemnesontette tuned blue by the liquid. Filter and proceed as described in 52.4.8, 153.33 Add exactly 100 mL of cated water tothe {a voluminous precipitate of sesquoxides forms extraction bot, stopper iighty and plac tin the shaker when ammonia is added to neutralize the ail, sore endagiatafor 16h, sulphate may be entrapped which wil net be removed by 7 weapdcsuseacenous niacnes |” £224 rte wlnnminitaacten wd dy fa ‘stonnd precilationis recommended. Tiss done by ‘rough seule iter paper eg, Whatman No, 6,00 the caret removing the fier paper with the precip ‘and replacing in the orginal beaker, A 10% solution of Soman ivumseentfuye sbelertemnresion Tsctpension trydroehorc cid added and te contents sted unl Santnan be eattugad mata et Seared and 25m. othe Saat the sesquioxdes have gone into the solution (20 ml of | SHPETSNAME gud ume forthe any 10 % hydrochloric acid should be sufi) Bring the 5.3.25 tfthelomexchange method of analysis tobe used conlens othe boll and repeat step) above, {s005 6)itinexsantilthat no adctional waeris added tony 15.3 Prapartion of sot aa is water extract stage andthe sotremeining nthe iter paper not washed. . “Transfer 50 mL of the extract 108 clean chy 250 ml conical | “Tho requicranta of Part tof hie eunderd where nant of art of hie ended beaker snd add distilled water ta maka upto 100 mL. sporoprine 53.3.6 Ifthe gravimetric method of analyse eo be used, 521 Apparatus transter 50 mk offered extract oa 500 mL. conical beer. 83.1.1 Apparatus for poperaton of test specimen-The ‘Add distilled watarto about 300 mL and proceed to. "operstuxrequire forthe preparation of each tert pecan spperatusreqrirs fo the pra 5.4 Preparation of ground water for testing ‘The requirements of Patt of this standard, where 6:21.12 Apparatus for preparing water entect appropriate, shall apply to this wet method. 2121 General The apparatutlisiedin§ 21221063125 5.4.41 Apparatus ‘srequiredin addon othe ime ited in8.2.12, 843.1 Filaton funnel and send, ‘$.B.1.2.2 Mechanical shaker or stirrer, capabie of keeping S0gofsoiincontinuou suapension in 00 mi of wate S12 Fw papert a camotertsukthe fun, 83.123 Extraction bottle, of approximately 250 mt. A122 Thvee00 ml glass cont capacty. 53124 75mm dlarater watch glass. 54:14 T0250 mi conice! beakers. $3425 50ml anda? mL piper ‘SA48 100 ml glass measuring eytinder. {83.2 Preparation of test specimen S418 s0 ml pee, 532.1 Preparecscntestspecimentor enslysistromthesol 54.1.7 Wesh bottle, praterebly made of plastics, containing sample as described inS.3.22t0 8328, ied water, 8222 Prepare esemple of material passing the 2 mmtast_ 542 Procedure sieve, ox described in6.2.32t052.38. 54.2.1 Froma.sampie of atleast 00 ml of ground water 5:23 Divide the rater! passing the 2m sive by Propare two testeamples as givenin S22 1054.24. ‘successive fling through the 15 mim divider to produce a ‘somple weighing epproximately 60 9. BS 1377 : Part3: 1990 5.422 Fittarthe weterthrough e suitablefiter paper such: ‘Whatman No. 4¢ intoaciean ftsk, to remove any particles ‘suspension. BAS tthe gravimetric method of analysis (see .5)is10 be used, traneter 50 ra ofthe filtered water to each of wo clean, ‘ry $00 mL conical beakers, and add approximately 100 mL of distilled water 10 each. 5424 Ktheion-exchange method of analysis sae 5.8)is to ‘be used, tranefer exactly 100 ml. of the filtered waterto each ‘oftwo clean dry 250 nL conical beakers, 5.5 Gravimatrie mathod for analysis of eckd or water extract (or ground water ‘The roquirements of Part 1 of this standard, where ‘ppropriete, shall apply to this test method. 55.1 Apparatus 55.1.1 Theopporstus ietod inB.6.1.2t08.5.14s required in addition to the tems listed in 52.1 oF 8.2.1 0F 5.4. 65:12 Exher: (a) a sintered sila fhoring erucibie of porosity grade No. 4 and about 35 mm diameter and 40 mm high: or (©) anigattion crucibveabout 3 mm diameter and40 mm high, capable of maintaining a constant mass when hhestod to 800 # 50°C. 85.13 A suitable means of igniting the precipitate, preferably an electric muff furnace capable of reaching and ‘maintaining 900 #: 60°C. Atornatively e Bunsen bumar or Siilar burner, tripod and suitable pipectay triangle may be used. 55.14 Bafance, resdsble to 0.001 9. 55.15 Sluelitmus poper 552 Resgents 85.21 Gonoral. Tha reagent lirted in §.6.22is required, in ‘ndciton to thooe listed in 5.22. All reagents shall be of ‘recognized analytical reagent quality. (NOTE. Whare accurtalysundardized solutions are required it may ‘bemore convenient i claain thom already standurdzed in ‘oncaerstedTorm ancto cine them es necessary in accorsance with {hemanutecure’s netrucione. 5.5.2.2 Barium chloride, § % (mV) solution. Dissotve 50g ‘of barium chloride in 1 L of water. Fiter before use if necessary, 553 Test procedure - 55.8.1 Analyse each fitrat Semple obtained from the acid ‘exrrect procedure deseribedin$.2.4, or fromthe water extract ‘provedure describedin5.3.3(see5 3.26), orfromthe ground ‘water sample propared ac described in 6.4.2 (s00 5.4.2.4), 5 deccribed inB532t0 553.8. 55.3.2 Testthe solution with litmus paper and f necessary ‘make slightly aid by the addition of 20 drops of hydroehoric acid, 55.23 Dilute 10 300 mL if necessary), bring the solution to the boll and add 10 mL barium chioride solution drop by ‘drop with constant stirring. Continue bol¥ing gently unti the precipitate is property formed. Issue 2, April 1996 ‘55.3.4 Allowtha solution ostand atjustbelow boiling point {for at least 30 min, then teave to cool to room temperature. {8.5.3.5 Transferthe liquid and precipitate of barium sulphste ‘with extreme care toa previously ignited and weighed ‘sintered silica fiter crucible using suction. Alternatively ‘transfer the precipitate with extreme care toa sutabte fiter ‘Paper, e.g. Whatman No. 42, in the glass filter funnel and fiver. In either cage wash the precipitate several times with ‘hot cistilod water until the washings are free rom chloride es cated by absence of turbidity when a drop is tested with the solution of evar nitrate. 55.2.6 Hasinteredsitica ter crucible is used removeit from ‘the fter flask aad dry at 105 °C to 110°C for approximately 20 min and gredually reise the temperature to 800°C, either inan olsewie muffle furnace or by other suitable means untit no further loss in macs occurs. {55.327 If the precipita is fitered through a fee paper, ‘vonsfer the titer paper end precipitate toa previouslyignited ‘and weighed crucible. I en electric mutfe furnace is used, place the crucible andcontantsin it atroomtemparature and ‘gredually caine the temperoture to red heat, Ife Bunsen or ‘other burner is used first dry the fitter paper and precipitate ‘slowly over 2 emall flame, taking care to char the filter paper slowly rather than to allow ito inflame, otherwise some of ‘the precipitate may be lost. Ignition for about 15 min atred hoatis ueuelly eufficientin either casa. 5.5.3.8 Following 58.3.6 or 8.5.8.7 coo! the crucible to room, ‘temperature inthe desiccator and waigh Ito the nearest 0.001 9, Calculate the mass ofthe precipitate (ma) from tha ‘increase in the recorded mass ofthe erucible, 8.54 Calculations NOTE 1. Traditionally sulphate contonts are exprossadin terms of ‘80, apd this isthe mathod that has therefore been adooted here, i itis desired to express sulphates in trra of SO, the resuts, in terms of §0,, ia the relevant equations given inthis clause should be mutipied by 1.2. NOTE 2. See form 3 () of Annex A. 5.5.1 Soil samples ‘554.1. Calculatethe percentage ofthe original soileample ‘passing the 2 mm test sieve from the equation: ‘fraction finer than 2 mm = 22 x 100 om where ‘mis the mass of the fraction passing the 2 mm sieve (in gh: ‘mis the initial dry mess of sample fin g). 5.8.4.12 Forthe acid exact procedure, calculate the percentage of total sulphstes (as SO,)in the frection of the sol! sample finer than 2 mm for each determination from the equation: eam 80,=—= (%) where _myisthe moss of each test specimen used (in gh: ‘mia the mass of ignited precipitate (ng). {more than one specimen hes been tested end the individual ‘results differ by no more than 0.2 % {80,),calculatethe mean ‘osu. fthey differ by more then 0.2 %, repeat the test ‘starting with two new analytical portions ofthe sol 10 Issue 2, April 1996 5.8.4.4.3 For the water extract procedure, the sulphate Cente can be expresaed eer inten of he of supa tha enc (a £039 fiat | below orn tere cf parsonage trateesoubie suiphato the S01 semper Bk asin J, Method 1. Caleuate the sulphate content in gf ofthe 2:1 waterisol extract from: Concentration of ‘ere mss the mabe ofits redpate 6) Methed 2 Calas to suphato corte as 2 percentage of the soil from: xquation: ‘Water-soluble sulphate content (as SO3) = 1.372m, (%) ‘Where m, is the mass of ignted precipitate (in ). {individual results differ by no more than 0.2 % of 0.2 g/L ($04) cakeuate the mean fesut they dite more than aoc 2g repeal he ot staring wth orem ‘analyical portions ofthe sol. ‘542 Ground water semples. For each determination calculate the sulphate content (as $0) ofthe ground wetor (in ‘ot from the equation: $803 = 688m, ‘individual rautscitfer by no more than 0.2 gf. (S03), calcutta the mean reauit. they differ by more than 0.2 of, ‘Tepamttha test aring with two new 50 mL samples of fired ground wane, SS Tost report 6.58.1 Soil samples. The test report shel tata thatthe test ‘was carried out in accordance with 5 of BS 1377 : Part’ +1980 and eal contain the fflowing informati (ah the method of test weed: b) the acid-soluble sulphate content (if determined) to Breneares: 01 ag G0) othe ovenay mas fol pasting onan est sve, ¢) the water-sotubie ether to the nearest 0.1 tboth ae 80). (d} the percentage by dry mass of the original sample passing 2 um tetova, to tho naaret 3%; {0} th information required by 8:10 BS 1377 100. {8552 Ground wate camo. hates rapt shal tate that the eat wa cried out in coordunce with 68 08S 1377 Part 3: 190 aed hal contain te towing information (a) the method of tet ured; (0) thoavarage sulphata content ofthe sample a ground war othe nearest O01 pl: (c) she iformation ruled by 8.1 of 1377: Par: ‘90. 56 torraxchange method for aosyaa of water extract or rovnd water ‘The roquirmont of Par 1 ofthis sandra where -pproprista, shall apply to this test method. NOTE halon nchenge methodcanot be ued eo ground ‘watarcontann onions of strong acide, nuh ne chlorides nitrate and ‘Paonphetas (we note 3-13) 5O1 Apparatus ‘content if determined) ‘Gt orto the nearest 0.01 % at BS 1377: Part3: 1990 5.6.1.1 General Tho epporatue ered in 6.6.1.2 10 6.6.1.6 is ‘required in adition ro the itamsilsted in B3.1 or 54.1, 5.612 Glass ion-exchange column, fined with 8 ewan-nack ‘outlet (208 figure 1). ‘5.81.3 Water resorvotr, incorporating a constant head ‘device (optional). Atypical design is shown in igure 2. 5.1.4 Two800 mL conical beakers. 5.6.15 250 ml beaker. 5.6.16 50-ml burerte and buratt scand. 5.6.1.7 Ambercofoured glass container. 8.02 Reagents ‘5.82.1 Goneral Alleagentsshallbe of recognized analytical reagent quality. NOTE. Where accurately standardized solutions are aquired Renoy ‘be more convenient obtain ham aes eandardead in ‘concentrated form and uta them ae neceasary in aocordance wit ‘he manutacturer instructions. 5.8.22 A strongly acidic cation-exchange resin. ‘5.82.3 Hydrochloric acid solution (e(HCH = approximately 4 ‘moV/L), Dilute 260 mL of concentrated hydrochloric acta {Genaity 1.18 g/ml) t0 1 L with distilled water. 5.624 Sodium hydroxide solution, (e(NaOH = ‘epproximstely 0.1 mol/L). Dissolve about 2g of sodium ‘hydroxide (see note 1)in500 mL of dstitted water. Determine ins exect concentration (2) by titration againet the potassium hydrogen phuhalate solution (see 6.6.28) using phenolphthalain or thymol biue as indicstor (aoe note 2) Keep the solution in an airtight container. [NOTE 1. Sodium hvdronie is stronghy caustic: care should therefore ‘be tatan to void contactwith the stin and aye protection required. NOTE 2. Wetandarced acide avalabi, e.g. preparedasdenribedio ‘£33 thie may be uted inetand ofthe potassium probate. -Arteraatvay key be more convenient to obtain a ready ‘Standardised solution of sodium hydroxide and prepare Kin ‘ctordanes wht the manufacturers Inervcions 5.6.28 Potessium hydrogen phthalate solution, Fe{KHC.H

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