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BS 1377-3:2018+A1:2021 BSI Standards Publication Methods of test for soils for civil engineering purposes Part 3; Chemical and electro-chemical testing bsi. BS 1377-3:2018+A1:2021 Publish igand copyright information “The BI copyright notice displayed inthis document indicates when the document was last issued (© The British Standards Institution 2021 Published by BSI Standards Limited 2021, ISBN 978 0539174007 4393020 “The following BSI references relate to the work on this document: Commitee reference B/526/3 Drafts for comment 18/30351283 DC; 21/30435929 DC ‘Amendments/corrigenda issued since publication Date ‘Text alected ‘30 September 2021 AL: see Foreword (© THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED BRITISH STANDARD BRITISH STANDARD BS 1377-3:2018+A1:2021 Contents Foreword 1 Scope 2. Normative references 3 Terms and definitions 4 Determination of the organic matter content 41 Principle 42. Reagents 43° Apparatus 44 Preparation of test specimen 45° Procedure 46 Calculations 47° Testreport 5 Determination of total organic carbon (TOC) 5.1 Principle 5.2 Reagents 53. Apparatus 54 Preparation of test specimen 55 Procedure 56 Calculations 57 ‘test report {6 Determination ofthe mass loss on ignition 6.1 Principle 62. Apparatus 63. Procedure 64 Calculations 65. Testreport 7 Determination of sulfur compounds 71 General 7.2. Sampling, sample storage and sample preparation 7.3. Determination of water-soluble sulfate in soil (WS) 74 fon Chromatography (IC) method for analysis of water extractor groundwater sulfate Table 1 — Example concentration of calibration ranges Table 2 — Fsamnle anion concentrations in calibration standards 75 Inductively coupled plasina stomie emission spectrometer (ICP-AES) method for analysis oF acid or water extract or groundwater sulfate Table 3— The concentration as a 6 of the upper limit ofthe apparatus of the different calibration standards for ICP-AES Table 4 — Example offive calibration standards fr copper, magnesium and sulfur 7.6 Gravimetric method for analysis of acid or water extract or groundwater sulfate 77 on-exchange method for analysis of water extractor groundwater suliate Figure 1 —Constant-head device for use with ion-exchange column Figure 2 — ton-exchange column for sulfate determination 7.8 Determination of groundwater sulfate (GWS) 79 Determination of acid-soluble sulfate (AS) 7.10 Determination of total sulfur (TS) 7A1_ Determination of total reduced sultur (TRS) Figure 3 — Schematic diagram of the apparatus for total reduced sulfur determination Figure 4 — Jones reductor assembly 23 24 Ey 26 28 30 31 32 33 36 37 39 40 (© THE BRITISH STANDARDS INSTITUTION 2021 ~ALLRIGHTS RESERVED 1 i BS 1377-3:20186A1:2021 712 al 382 383 84 on 92 93 10 101 102 103 104 105 106 ul ua 2 43 4 15 12 12a 122 123 4 125 126 127 13 131 132, 133 134 135 136 13.7 14 14a 142 Determination of acid-soluble sulfides (monosuifide sulfur) (MS) Figure § — Apparatus for determination of acid-soluble mono-sulfide (6S) Determination of the carbonate content ‘Types of test method Total carbon analyzer, combustion method - Total inorganic carbon (TIC) Rapid titration method for determination of calcium carbonate content Gravimetric method for determination of calcium carbonate content, Determination of the chloride content General Determination of water-soluble chloride content Determination of acid-soluble chloride content Determination of magnesium - water-soluble magnesium in 2:1 extract Principle ‘Sample preparation Preparation of 2:1 water-soluble extract Determination of magnesium in solution Calculations Test report Determination of total dissolved solids General Apparatus Test procedure Calculations ‘Test report Determination ofthe pH value General Reagents Apparatus Preparation of sample pl determination Quality control Test report Determination of electrical resistivity Principle ‘Tunes of test and limitations, Measurement af resistivity: undisturbed cylindrical samples Figure 6 — Testing undisturbed cylindrical samples Measurement of resistivity: open container method Figure 7 — Design for open container for resistivity tests on saturated coarse soll Figure 8a — Design for reduced size open container for resistivity tests on fine-grain cohesive soil ~ Example ofa small resistivity test cell for use with fine-grained soits Figure &b — Design for reduced size open container for resistivity tests on fine-grain cohesive soil ~ Example ofa reconstituted soil sample trimmed from a Proctor mould Measurement of resistivity: Wenner probe method Figure 9 — Cirewit diagram for resistivity test using Wenner probes Calculations Test report Determination of the redox potential General Apparatus 1 @ THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED BRITISH STANDARD B 45 48 48 49 51 54 55 55 55 61 63 63 64 6 64 65 65 65 65 60. 66 66, 67 67 67 67 68 68 9 69 0 oo 69 ™ 2 ” 76 7 78 82 83 87 88 89 89 90 £ 5 a3 28 2 BRITISH STANDARD Bs 1377-3:2018+A1:2021 143 Reagents 1 144 Procedure on 145. Calculations 3 146 Test report 93 ‘Annex A (informative) Determination of sulfur compounds of 98 bliography Summary of pages ‘This document comprises a front cover, anit a back cover. le front cover, pages Ito VI, pages 1 to 98, an in (© THE BRITISH STANDARDS INSTITUTION 2021 -ALL RIGHTS RESERVED tl BS 1377-3:2018+A1:2021 BRITISH STANDARD Foreword Publishing information ‘This part of BS 1377 is published by BSI Standards Limited, under licence from The British Standards Institution, and came into effect on 31 July 2018. It was prepared by Subcommitee B/526/3, Site investigation and ground testing, under the authority of Technical Committee B/526, Geotechnics. Allist of organizations represented on these committees can be obtained on request to the committee manager. Supersession BS 1377-3:2018+A1:2021 supersedes BS 1377-3:2018, which is withdrawn, Relationship with other publications BS 1377 is published in the following parts: + Part 4: General requirements and sample preparation; + Part2: Classification tests; ‘+ Part 3: Chemical and electrochemical tests; + Part 4: Compaction-related tests; + Part 5: Compressibility, permeability and durability tests; + Part 6: Consolidation and permeability tests in hydraulic cells and with pore pressure ‘measurement; + Part 7:Shear strength tests (total stress); + Part 8: Shear strength tests (effective stress): + Part: In-situ tests Information about this document ‘This part of BS 1377 is intended to be read in conjunction with BS 1377-1 In this part of BS 1377, the tests described in the 1990 edition have been retained. Additional tests have been added to include the recommendations of BRE Special Digest 1 (BRE 2005) [1]. liyomatography and inductively coupled plasma atomic emission spectroscopy. Ihe two point resistivity method has been removed and additional four point tests included, ‘Text introduced or altered by Amendment No. 1isindicated in the text by the tags 3). Gl. Minor editorial changes are not tagged. ‘Amendment A1 introduces the following principal changes; + technical changes to BS 1377-3 to remove an error in the wording and to improve clarity. This publication can be withdrawn, revised, partially superseded or superseded, Information regarding the status of tis publication can be found in the Standards Catalogue on the BSI website at bsigroup.com/standards, or by contacting the Customer Services team. Where websites and webpages have been cited, they are provided for ease of reference and are correct atthe time of publication. The location of a webpage or website, or its contents, cannot be guaranteed. IW © THE BRITISH STANDARDS INSTITUTION 2021 ALL RIGHTS RESERVED BRITISH STANDARD BS 1377-3:2018+A1-2021 Hazard warnings WARNING. Persons using tis British Standard are expected be familiar with normal laboratory practice. This British Standard calls forthe use of substances and/or procedures that canbe injurious to heath if adequate precautions are not taken, lt refers only to technical suitability and does not absolve the user rom legal obligations relating to health and safety at any stage. These include the us of fume cupboards or sim apparatus when using acids and other toxic chemicals. This standard does nat purport to address the safey| problems, fany associated with suse. tis the responsibilty ofthe user to establish appropriate safety and health practices and to ensure compllance with any natlonal regulatory cont tis expected that tests conducted in accordance with this British Standard will be carried out by suitably | rained and experienced staf WARNING. It is dangerous to add water to concentrated aci. Use of this document thas been assumed in the preparation of this part of BS 1377 that the execution of its provisions will be entrusted to appropriately qualified and experienced people, for whose use it has been produced. Presentational conventions ‘The provisions of this standard are presented in roman (ie. upright) type. Its methods are expressed. asa set of instructions, a description, or in sentences in which the principal auxiliary verb is “shall” Commentary, explanation and general informative material is presented in smaller italic type, and does not constitute @ normative clement ‘Where words have alternative spellings, the preferred spelling ofthe Shorter Oxford English Dictionary is used (e.g. “organization” rather than “organisation’). Contractual and legal considerations This publication has been prepared in good faith, however no representation, warranty, assurance or undertaking (express or implied) is or will be made, and no responsibility or liability is or will be accepted by BSI in relation to the adequacy, accuracy, completeness or reasonableness of this publication, All and any such responsibility and liability is expressly disclaimed to the full extent permitted by the law. ‘This publication is provided as is, and is to be used at the recipient's own risk. ‘The recipient is advised to consider seeking professional guidance with respect to its use of this publication. cation is not intended to constitute a contract. Users are responsible for its correct This publ application, Compliance with a British Standard cannot confer immunity from legal obligations. (© THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED. V a 2 B q E 5 ‘HIS PAGE DELIBERATELY LEFT BLANK BRITISH STANDARD BS 1377-3:2018+A1:2021 1 Scope ‘This part of BS 1377 describes test methods for determining the amount of chemical substances in ‘samples of soil and extremely weak and very weak rocks, as defined by BS 5930, and groundwater. NOTE 1 Chemical tests in this part of BS 1377 may be used on her rocks ifrequired. Italso describes test methods for the determination of some electrochemical and resistivity. properties of solid samples. NOTE 2 These tests provide data to assess the potential of the ground and solutes to damage construction ‘materials, including cementitious materials and metels in he ground. They can also be used in assessment of the potential for volume change of the ground due to chemical reaction. Resistivity test results can also be used to assess Insit resistivity results ‘This British Standard is not written for testing samples from contaminated land or for soil quality assessment, Procedures described in this part of BS 1377 are for the determination of the following: a) organic matter content in the material (Clause 4); 1b) total organic carbon (TOC) contentin the material (Clause 5); loss on ignition of the material (Clause 6); 4) sulfur compounds (Clause 7} 1) water-soluble sulfate content ofthe material by 2:1 extraction; 2) sulfate content in groundwater; 3) acid-soluble sulfate content of the material; 4) total sulfur content of the material; 5) total sulfide content (total reduced sulfur) content of the material; 6) acid-soluble sulfide (monosulfides sulfur) content of the material; €) carbonate content of the material (Clause 8); A) chloride content (Clause 9): 1) water-soluble chloride content of the material; 2) acid-soluble chloride content of the material, ‘maguesiui content of he material (Clause 10); 8) water-solub hh) total dissolved solids of the groundwater (Clause 11); i) pH value (Clause 12); J) electrical resistivity of the material (Clause 13); and Kk) redox potential ofthe material (Clause 14), Brief guidance on the detrimental effects of sulfur compounds on engineering works and alternative ‘methods of identifying the specific minerals is given in Annex A. NOTES Good practice in chemical resting requires duplicate specimens to be tested. In each ofthe test methods the measurement of only one value ofthe overal resul Is described, It is recognized that ts necessary in many practical applications to make a numberof tests in order to obtain a representative value and an indication of ‘the reliability ofthe results Guidance on the number of measurements required and the treatment of te results ‘abtained are not provided in this standard. (© THE BRITISH STANDARDS INSTITUTION 2021 -ALLRIGHTS RESERVED 1 BS 1377-3:2018+A1:2021 BRITISH STANDARD 2 Normative references ‘The following documents are referred to in the text in such a way that some or all oftheir content constitutes provisions of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. BS 89, Specification for direct acting indicating electrical measuring instruments and their accessories BS.1377-1:2016, Methods of test for soil for civil engineering purposes - Part 1: General requirements and sample preparation BS 1881-124:2015, Testing concrete ~ Part 124: Methods for analysis of hardened concrete 1885930, Code of practice for ground investigations BS EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods BSENISO 17034, General requirements for the competence of reference material producers BS EN ISO 17892-1, Geotechnical investigation and testing - Laboratory testing of soil ~ Part 1: Determination of water content BS EN ISO 22475-1:2016, Geotechnical investigation and testing - Sampling methods and groundwater ‘measurements Part 1: Technical principles for execution 3. Terms and definitions For the purposes of this part of BS 1377, the terms and definitions given in BS 1377-1 and the following apply. 3.1 titration addition of a solution from a graduated burette to a known volume of a second solution, until the ‘chemical reaction between the two is completed NOTE Ifthe strength ofone of the solutions isknown, that ofthe ather can be calculated from the volume of liquid added, ‘substance which is capable of giving a clear visual indication ofthe completion of a chemical reaction 3.3. pHvalue logarithm to base 10 of the reciprocal ofthe concentration of hydrogen ions in an aqueous solution NOTE — leprovides a measure ofthe acidity or alkalinity ofthe solution on a scale reading from 0 to 14, on which 7 ropresents neutrality. 3.2. indicator | ty (of soil) electrical resistance, in 2 (ohms) per unit length, ofa column of soil of unit area of cross-section 3.4 resisti NOTE inthis parc ofBS 1377, resistivity is expressed in Om (ohm metres) 3.5 redox potential (reduction /oxidation potential) relative measure, expressed in millivolts, the reducing or oxidising capacity of soil, usually increasing with increasing oxygen content 2 © THE BRITISH STANDARDS INSTITUTION 2021 ~ALL RIGHTS RESERVED BRITISH STANDARD BS 1377-3:2018+A1:2021 3.6 3.7 4A 42 42a 422 423 424 425 426 427 42.8 calibration blank sample extract solution used to make solutions NOTE1 For example, water or aca used forthe preparation of extractions prior to analysis: NOTE2 The primary purpose ofa blank isto trace sources of artificially introduced contamination and used to {frcitatecorrectin ofthe final tet sample result stock solution solution with accurately known analyte concentration(s) prepared with an appropriate purity NOTE Stock solutionsare reference materials within the meaning of PD ISO Guide 30. Determination of the organic matter content Principle ‘This procedure covers the determination of the percentage by dry mass of oxidisable organic matter present in a soil NOTE The method, which uses dichromate oxidation, isknown as Walkley and Black's method Soils containing sulfides or chlorides have been found to give high results by this procedure. Methods for checking for the presence of these compounds, and procedutes for their removal before testing ifthey are present, are included ‘The requirements of BS 1377-1, where appropriate, shall apply to this test method. Reagents All reagents shall be of recognized analytical reagent quality, NOTE Where accurately standardized solutions are required it might be more convenient to obtain them ‘already standardized in concentrated form and to dilute tem as necessary in accordance with the manufacturer's Potassium dichromate solution, [e{K,Cr,0,) = 0.167 mol/l]. Dissolve 49.035 g of potassium dichromate in distilled, de-ionized water (BS 1377-1:2016, 6.1) to make 1 | of solution. Ferrous sulfate solution. Dissolve approximately 140 g of ferrous sulfate in sulfuric acid solution [c(H,S0,) = 0.25 mol/l} to make 1 of solution. Add 14 ml of concentrated sulfuric acid to distilled /de- iuuized whit (03 4377-42056, 6.1) wv mabe i Lut sulfa acid solution (3,50) = 025 wal Record the date the solution 1s made on the bottle, This solution is unstable in air Keep ittightly stoppered and standardize against the potassium dichromate solution at least once a week. Sulfuric acid concentrated. Density 1.84 g/ml. Orthophosphoric acid 85% (v/v) solution. Density 1.70 g/ml to 1.75 g/ml. Indicator solution, Dissolve 0.25 g of sodium ciphenylamine sulfonate in 100 mi of distilled /de- ionized water (BS 1377-1:2016, 6.1) water. Hydrochloric acid, 25% (v/v) solution, Add 250 ml of concentrated hydrochloric acid (density 1.18 g/ml) to 500 ml of distilled/de-ionized water (BS 1377-1:2016, 6.1), then make up to 11 with distilled/de-ionized water (BS 1377-1:2016, 6.1) Lead acetate paper. Filter paper that has been dipped in a 10% solution of lead acetate, (© THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED 3 BS 1377-3:2018+A1:2021 BRITISH STANDARD 42.9 43 aaa 432 433 434 435 436 437 438 43.9 43.10 4aat 43.12 4313 438 4315 43.16 43.17 43.18 44 441 442 443 444 Sulfuric acid, [e(H_$0,) = approximately 1 mol/l). Add $3 ml of concentrated sulfuric acid to about 500 ml of distilled/de-ionized water (BS 1377-1:2016, 6.1) water, then make up to 1 with distilled/de-ionized water (BS 1377-1:2016, 6.1). Apparatus Drying oven, capable of maintaining a temperature of (50 £2.5) °C. Balance, readable to 1g. Balance, readable to 0.001 g, 1 volumetric flask Two 25 ml burettes, graduated to 0.1 ml 10 ml pipette and a 1 mi pipette, each fitted with a rubber teat. Two conical flasks, of S00 ml capacity. 200 ml and 20 ml graduated measuring cylinders. Desiceator, (a convenient size is about 200 mm to 250 mm in diameter) containing anhydrous silica ge Glass weighing bottle, approximately 25 mm in diameter, 50 mm high and fitted with a ground glass stopper. ‘Test sieves, 2 mm and 0.425 mm aperture sizes, with receiver. Sample dividers of multiple-slot type (rifle boxes), having widths of opening of 7 mm and 15 mm. Pestle and mortar, ora suitable mechanical crusher, Wash bottle, preferably made of plastics, containing distilled de-ionized water (BS 1377-1:2016, 6.1). Glass boiling tube. Filter funnel, of approximately 100 mm diameter. Filter papers, ofa diameter appropriate to the size of the funnel: medium grade (e.g. Whatman No. 40 @")) and fine grade (eg. Whatman No. 42 @"). Blue litmus paper. Preparation of test specimen Each test specimen shall be prepared for analysis from the laboratory sample as given in 44.2 10.44.11. ‘An initial sample shall be obtained as described in BS 1377-1:2016, 8.3, and ofthe approximate size as specified in BS 1377-1:2016, 8S. ‘The sample shall be dried in the oven to constant mass at (50 #2.5) °C, and cooled to room temperature in the desiccator. The sample shall be weighed to the nearest 0.1% and the mass m, (in g) recorded. "Whatman va rademarkof GE Healthcare, Thisinformation i given for the convenience of usersof this document and doesnot constitute an endorsement by the British Standards Institution of the named product. Equivalent products may be used they canbe shown told to the same results 44 © THEBRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED BRITISH STANDARD BS 1377-3:2018+A1:2021 445 44.6 447 448 449 44.10 44nd 45 45.1 ASAA 4SA2 454.3 4SA4 45.15 45.1.6 45.17 ‘The sample shall be sieved on a 2 mm test sieve (ifappropriate, guarded by a test sieve of larger aperture) and crush retained particles other than stones to pass the 2 mm sieve. NOTE —Iésassumed that any material retained on the 2 mm test sieve wll not contain organic matter. Ifthis is seen not to be true, the pieces of organic matter should be removed by hand, crushed to passa 2 mm test sieve and incorporated inthe fraction passing the seve, ‘The stones shall be rejected, ensuring that no fine material adheres to them, e.g. by brushing. Record the mass of sample passing the 2 mm test sieve (in g) to the nearest 0.1% (m,). Throughout these and subsequent operations take care to ensure that there is no loss of fines. ‘The material shall pass the 2 mm sieve by successive riffling through the 15 mm divider to produce a sample weighing approximately 100 g. ‘This sample shall be pulverized so that it passes the 425 jm sieve. ‘The sample shall be subdivided by rifling on the 7 mm divider to obtain the following test specimens, ‘as appropriate: a) ifsulfides and chlorides are known to be absent, two test specimens each weighing about 5 g: 1b) _ fora check test to determine whether sulfides are presenta specimen of about Sg ©) _ fora check test to determine whether chlorides are present, a specimen of about 50 g: 4d). if sulfides and/or chlorides are present, a specimen of about 50 g. NOTE Throughout this preparation and any subsequent operation mix the material available thoroughly before ‘any division and take care to avotd segregation during rifin. Each specimen shall be placed in a glass weighing bottle and dried in the oven at a temperature of (50 #2.5) °C. The specimens shall be deemed to be dry when the differences in successive weighings, carried out at intervals of 4 h, do not exceed 0.196 of the original mass of the sample. ‘The specimens shall be allowed to cool to room temperature in a desiccator containing dry self-indicating desiccant and each bottle and contents weighed to 0.001 g. Procedure Standardization of ferrous sulfate 10 ml ofthe potassium dichromate solution (4.2.2) shall be added from a burette into a 500 ml conical flask. 20 mi of concentrated sulfuric acid shall be added very carefully, the mixture swirled and allowed to cool for some minutes. 200 ml of distilled/de-ionized water (BS 1377-1:2016, 6.1) shall be added very carefully to the mixture followed by 10 ml of phosphoric acid and 1 ml ofthe indicator, and shaken to mix thoroughly. Ferrous sulfate solution shall be added from the second burette in 0.5 ml increments, and the contents of the flask swirled until the colour of the solution changes from blue to green. A further 0.5 ml of potassium dichromate solution shall be added, changing the colour back to blue. Ferrous sulfate solution shall be added slowly drop by drop with continued swirling until the colour ofthe solution changes from blue to green after the addition ofa single drop. ‘The total volume of ferrous sulfate solution used shall be recorded, x, to the nearest 0.05 ml. (© THE BRITISH STANDARDS INSTITUTION 2021 ~ALL RIGHTS RESERVED 5, BS 1377-3:2018+A1:2021 BRITISH STANDARD 454 4844 4542 Qualitative check for sulfides ‘The presence of sulfides in the soil shall be verified as described in 4.5.2.2 and 4.5.2.3. NOTE A quolitative check might have heen carried out inthe tests for sulfide (see Clause 7, in particular 7.9). ‘The 5 g check sample (which need not be weighed) shall be placed in a boiling tube. 50 ml (approx) of hydrochloric acid (4.2.7) shall be added. This shall be brought to the boil and the presence of hydrogen sulfide checked for by holding in the vapour a piece of filter paper that has been dipped in a 10% solution of lead acetate. This will turn black if hydrogen sulfide is present. NOTE This should be carried out in a fume cupboard Ifthe presence of sulfides is indicated it shall be removed from the test specimen as described in 4.5.3 before proceeding with the analysis for organic matter, otherwise a result that is too high will be obtained. Ifthe presence of sulfides is not indicated, omit the procedure given in 4.5.3. Elimination of sulfides “About 50 g of the soil shall be weighed, after cooling as described in 4.4.10 and 4.4.11, to 0.01 gand placed in a 500 ml conical flask. Sulfuric acid solution [c(H,S0,) = 1.0 mol/l shall be added until no further evolution of hydrogen. sulfide occurs, as determined by testing with lead acetate paper ‘The contents of the conical flask shall be filtered on a medium grade filter paper, taking care to retain all solid particles. This shall be washed several times with hot distilled /de-ionized water (BS 1377-1:2016, 6.1) until the washings do not indicate acidity when tested with blue litmus. ‘The soil retained on the filter paper shall be dried to constant mass at a temperature of (50 2.5) °C and cooled in the desiccator. ‘The soil shall be carefully removed from the filter paper and its mass determined to 0.01 g, ‘The treated sample shall be subdivided as described in 4.4.9, tem a) and each test specimen shall be dried and cooled as described in 44,10 and 44.11. Qualitative check for chlorides ‘The presence of chlorides in the soil shall he verified hy fallowine the nrocedure described in 9.2.3 Ifthe presence of chlorides are indicated they shall be removed from the test specimen as described in 4.5.5 before proceeding with the analysis for organic matter, otherwise a result that is too high will bbe obtained. NOTE 1 Alternatively, che efect of chlorides onthe organic matter determination can be party eliminated by using concentrated sulfuric acid in which silver sulfate has Been dissolved in place ofthe concentrated sulfuric acid specified in 42.4 Ifthe ratio ofcarbon to chloride does not exceed unity, 25 9 of silver sulfate per lee of sulfuric ‘acid wil be suficint to precipitate the chloride. NOre2 Ifthe presence ofboth sulfides and chlorides is indicated, the procedures described in 4.5.3 and 4.5.5 “should both be carried out on the sample of soll used for determination ofthe organic content. Ifthe presence of chlorides is not indicated, omit the procedure given in 4.5.5. Elimination of chlorides About 50 g of the soil shall be weighed, after cooling as described in 4.4.40 and 4.4.11, to 0.01 g, 6 © THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED BRITISH STANDARD BS 1377-3:2018+A1-2021 455.2 45.5.3 455.4 45.5.5 45.5.6 45.6 45.61 45.62 45.63 45.64 45.65 45.66 45.6.7 45.68 46 4641 ‘The soil shall be placed on a mediuim-grade filter paper ina funnel and washed with distilled/de- ionized water (BS 1377-1:2016, 6.1) water: Washing shall continue until no turbidity is observed when a drop ofthe wash water is tested with silver nitrate solution. ‘The soll retained on the filter paper shall be dried to constant mass at a temperature of (50 #2.5) °C and cooled in the desiccator. Al the soil shall be carefully removed from the filter paper and its mass determined to 0.01 g ‘The treated sample shall be subdivided as described in 44.9, item a) and each test specimen shall be dried and cooled as described in 44.10 and 4.4.11. Analysis for organic matter Each weighing bottle containing soil, obtained as described in 4.44, shall be weighed to 0.001 g [Asmall quantity, from 5.0 gto 0.2 g, depending on the organic content (see note), shall be transferred to adry 500 ml conical flask, the weighing bottle reweighed and the mass of soil removed (m,) calculated by difference. NOTE The size ofthe sample or chemical analysis varies with the amount of organic matter present in the soll. ‘Asmuch as 5.9 might be required for soil lw in organic mater, and as litle as 0.2.9 with a very peay sol. Afr ‘a number of determinations have been made experience will ndicate the most suitable size of sample to be taken. Where this isnot so, 1s suggested that a series of samples of varying sizes shouldbe tested. The determmation diving a total of§mto 8 ml of potassium dichromate solution reduced shouldbe taken as the one giving the correct result. 10 mlof the potassium dichromate solution (4.2.2) shall be run from a burette into the conical flask, and 20 mi concentrated sulfuric acid added very carefully from a measuring cylinder. The mixture ‘shall be swirled for about 1 min, and then allowed to stand on a heat-insulating surface for 30 min to allow oxidation of the organic matter to proceed. During this period the flask shall be protected from cold air and draughts. 200 ml of distilled/de-ionized water (BS 1377-1:2016, 6.1) shall be added very carefully to the mixture, followed by 10 ml of orthophosphoric acid and 1 ml of indicator, and the mixture thoroughly shaken, Ifthe indicator is absorbed by the soll a further 1 ml ofthe solution shall be added. Forrous sulfate solution shall be added from the second burette in 0.5 ml increments and the contents of the tlask swirled until the colour of the solution changes from biue to green. ‘A further 0.5 ml of potassium dichromate solution shall be added, changing the colour back to blue. Ferrous sulfate solution shall be added slowly drop by drop with continued swirling until the colour of the solution changes from blue to green after the addition ofa single drop. “The total volume of ferrous sulfate solution used, y, shall be recorded to the nearest 0.05 ml Calculations ‘The total volume V (in ml) of potassium dichromate solution used to oxidise the organic matter in the soil sample shall be calculated from the equation: (© THE BRITISH STANDARDSINSTITUTION 2021 ALL RIGHTSRESERVED 7 BS 1377-3:2018+A1:2021 BRITISH STANDARD 46.2 46.3 46.4 ar V=105) 1- o where 'y isthe total volume of ferrous sulfate solution used (see 45.6.8) (in mi; x isthe total volume of ferrous sulfate solution used inthe standardization test (see4.8.1) (om, “The percentage of the original soil sample passing the 2 mm test sieve shall be calculated from the equation: fraction finer than 2mm= 2100 @ m where ‘m, isthe initia dry mass of sample (In g; ‘m, — Isthemass ofthe sample passing the 2 mm test seve (ing), ‘The percentage of organic matter present in the fraction of the soil specimen finer than 2 mm for each determination shall be calculated from the equation (see note): 0.677 “a 8 percentage organic matter content where is the mass of soil used in the test (In). MOTE ‘The method is based on wet oxidation ofthe organic content ofthe sol, and assumes that sil organic ‘matter contains an average of $8% (m,/m) of carbon. The method employed oxidises approximately 77% ofthe carbon inthe organic matter, and these factors are included in the equacion given. The factors wil give correct result only for soil containing natural organic matter. If duplicate specimens have been tested, and ifthe individual results expressed as a percentage of “organic matter differ by no more than 2%, the mean result shall be calculated. If they differ by more than 296, the test shall be repeated starting with two new representative portions of soil. Test report ‘The test report shall state that the test was carried outin accordance with BD os to /s-s:cvserAiccucs Gp, Wlauise 4 and suai contain Une 1OLI0N riniauion: a) the method of test used: ) the organic matter content present in the soil fraction passing a 2 mm test sieve to the nearest 0.1% ofthe original oven dry mass of soil; ) the perventage by dry mass of the original sample passing the 2 mm test sieve to the nearest 19; 4) if sulfides or chlorides have been identified in the soil; e) the information required by BS 1377-1:2016, 10.1. Determination of total organic carbon (TOC) Principle ‘This procedure covers the determination of the percentage of total organic carbon present in a sample by total carbon analyzer using the combustion method. Total organic carbon, which measures {8 © THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED BRITISH STANDARD S.2 S24 S22 5.23 S24 5.2.5 5.2.6 53 53.4 5.3.2 5.8.8 BS 1377-3:2018+A1:2021 just carbon, is different from organic matter, which includes all the elements (hydrogen, oxygen, nitrogen, etc. that are components of organic compounds. The inorganic carbon, as carbonate, is removed prior to testing for total organic carbon. NOTE Anexample ofa routine method fr the determination of TOC is described using a total carbon analyzer controlled by a computer running appropriate software. The sample s washed with acd prior to analysis to remove inorganic carbon so the result obtained from the instrument is only organic carbon, The sample is heated in a high temperature combustion furnace (typically around 1 050°), through which a carrier gas suchas helium, 15 constantly flowing. Once in the combustion furnace oxygen is introduced to combust the sample. The carrer gas then conveys the combustion products via other furnace tubes containing materials to aid complete combustion and remove halogens, then via a suitable desiccant to remove molsture. The remaining stream of gas passes into a detector (eg infra-red) where carbon dioxide is determined asa function of ime, Carbonate minerals are ubiquitous in natural deposit and will affect che TOC determination, All metal carbonate minerals are unstable ‘and break down in the presence of hydrogen fons available in hydrochloric acd releasing the mineral carbon as. (CO, Most show reaction wih cold dilute hydrochloric aci, but some such as dolomite siderite, magnesite and other less common forms are any vey slowly soluble. The solubilty increases significantly in hot hydrochloric acid Pre-treatment of soil and powdered rack samples with hot hydrochloric acid i essential to remove any carbonate ‘minerals and to ensure that the value of TOC detormined accounts ony for the total organic carbon present. Reagents All reagents shall be of recognized analytical reagent quality. Concentrated hydrochloric acid (density 1.18 g/ml) Hydrochloric acid, 10% (v/v) solution. Dilute 100 ml of concentrated hydrochloric acid (density 1.18 g/ml) to 1 ml with distilled de-ionized water (BS 1377-1:2016, 6.1). High purity gaseous oxygen. Combustion catalyst, as specified by the instrument manufacturer. Certified carbon standards, a range of carbon levels are required to provide a calibration over the required range. Apparatus Drying oven, capable of maintaining a temperature of (50 42.5) °. Balance, veadable to 0.01 g olance, readable to 0.0001 g Conical flask Funnel Desiceator with dry selfindicating desiccant. GF/C glass fibre filters. Filterable crucibles and vacua bath, Beakers. Pasteur pipette Hot plate ‘Test sieves, 2 mm and 425 ym aperture sizes, with receiver. (© THE BRITISH STANDARDS INSTITUTION 2021 ALLRIGHTS RESERVED 9 5 a 5.3.13 5.814 5.3.15 5.3.16 5.4 541 542 5.43 544 545 5.4.6 SAT 548 54.9 7-3:2018+A1:2021 [BRITISH STANDARD Sample dividers of multiple-slot type (riffle boxes), having widths of opening of 7 mm and 15 mm, Pestle and mortar, ora suitable mechanical crusher. Carbon combustion analyzer and associated catalyst. Appropriate pipework and regulator, as required, to convey the gasses to the carbon combustion analyzer. Preparation of test specimen Each test specimen shall be prepared for analysis from the laboratory sample as given in 5.4.2 t0 5.4.10. ‘An initial sample and of approximate size shall be obtained as described in BS 1377-1:2016, 8.3. and cooled to room ‘The sample shall be dried in the oven to constant mass at (50 2.5) * temperature in the desiccator containing dry desiccant. ‘The sample shall be weighed to the nearest 0.1% and the mass recorded, m, (g} ‘The sample shall be sieved on a 2 mm test sieve (if appropriate, guarded by a test sieve of larger aperture) and retained particles other than stones crushed to pass the 2 mm sieve, NOTE Ieisassumed that any material retained on the 2mm test sieve wll not contain organic matter: IF this is seen not tobe true, the pieces of organie matter should be removed by hand, crashed to passa 2 mm test sieve and incorporated inthe fraction passing the sieve. ‘The stones shall be rejected, ensuring that no fine material adheres to them, e.g. by brushing, ‘The mass of sample passing the 2 mm test sieve shall be recorded (in g) to the nearest 0.1% (m,). Throughout these and subsequent operations care shall be taken to ensure that there is no loss of fines. ‘The material passing the 2 mm sieve shall be divided by successive riffling through the 15 mm divider to produce a sample weighing approximately 100 g. “This sample shall be pulverized so that it passes the 425 um test sieve. ach specimen shall be placed in a glass weighing bottle and dried in the oven ata temperature of (50 £25) °C. The specimens shall be deemed to be dry when the differences in successive weighings, carried out at intervals of 4 h, do not exceed 0.1% of the original mass of the sample. ‘The specinen shall be cooled t2 room temperature fn th tattle and contents weighed to 0.001 g, Procedure Determination of test sample mass ‘The glass fibre and filter or filterable cuvette shall be weighed, m, recorded to the nearest 0.001 g. ‘The sample shall be added to the glass fibre filter or into the cuvette and reweighed, m, to the nearest 0.001 g, NOTE. ‘The mass ofthe sample tested depends on the organic carbon content, apparatus used and the manufacturer's recommendations for that apparatus Samples with high organic content, such as peaty material, require lower test mass than for instance material containing high carbonate and low organic carbon. NOTE2 The size ofthe sample for chemical alysis may be reduced when there is @ large amount of organic ‘mater present inthe sol After a number of determinations have been made experience will indicate the most sultable size of sample to be taken. 10. © THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED BRITISH STANDARD BS 1377-3:2018+A1:2021 5.5.2 5.5.24 5.5.2.2 55.2.3 55.24 55.25 55.2.6 5.5.2.7 5.5.4.2 5.543 5.5.44 carbon Removal of inorgar The carbonate content shall be removed from the sample as described in 5,5.2.2 t0 5.5.2.10. The glass fibre filter containing the sample shall be placed into a funnel supported in a conical flask, or the fiterable crucible placed into its vacuum bath, Cold 1096 hycrochloric acid shall be added drop by drop to the sample until each sample is wet, if using fiterable crucibles turn on the vacuum. NOTE This process shouldbe carried ou ina fume cupboard, beneath an extractor hood or similar equipment. ‘The addition of acid might cause the samples to effervesce,ifso, the 10% hydrochloric acid shall be added until no further reaction can be seen, ot {(80 #5) °C] 10% hydrochloric acid shall then be added drop by drop until no reaction canbe seen, Washing with hot concentrated hydrochloric acid (5.2.2) shall be repeated. Each aliquot shall be allowed to drain through the filter or crucible before the next addition is made. ‘The sample shall be washed with six washings of a Pasteur pipette full (approximately 1 ml) of hot {(90 #5) °C] distilled /de-ionized water (BS 1377-1:2016, 6.1). The water shall be allowed to drain through between cach addition. Once the liquid has drained though, fold the filters to ensure no sauuple is lost and placed ima crucible, ‘The crucible shall be placed into the oven at (105 #5) °C for atleast 2 h or until the sample is dry. ‘The crucible shall be removed from the oven and placed in a desiccator with dry self indicating desiccant to cool until ready for analysis. carbon Analysis for total orgat ‘A representative sub sample of suitable mass as recommended by the apparatus manufacturers, shall be placed into a ceramic crucible, and then placed on the auto-sampler of the analyzer. The crucible is mechanically lowered into the combustion furnace and the test shall proceed asin the apparatus ‘manufacturer's recommendations. Calibration nent shall be verified before each batch of analyzes and after ‘The performance of thi each service. ‘The combustion analyzer shall be calibrated using a multi-point calibration of certified carbon standards with different organic carbon contents following the manufacturer's instructions. “The analysis of samples and check standards shall be as per manufacturer's instructions. Procedural blanks shall be run in duplicate. The instrumental software should automatically register that the carbon signal for a procedural blank is below the specified calibration range. If both of these duplicates values exceed this value, remedial action shall be taken to identify and correct it. NOTE.1 This method does not measure soluble organic compounds as they are removed during the acidification ‘and washing procedure. NOTE2 Any chloride or water nt removed by the instrument can corrode analyzer components and/or interfere ith che determination of carbon dioxide (© THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED 11 BS 1377-3:2018+A1:2021 BRITISH STANDARD 5.6 Calculations 5.6.1 The weight of sample prior to acid washing, m, (which is equal to m, ~ m,) shall be input into the apparatus computer data for that sample as required and the results from the instrument are as 1% carbon, Because the acid washing has removed inorganic carbon this will equate to the % total organic carbon present in the dry soil, 5.6.2 ‘The percentage of the original soil sample passing the 2 mm test sieve shall be calculated from the equation: fraction ner than 2mm = 2100 @ my where sm, ‘sth ntl ry mass sample (nh 'm, isthe mass of the sample passing the 2 mm test sieve (ing), 5.7. Test report “The test report shall state that the test was carried out in accordance with B) Bs 1377-3:2018+A1:2021 Gi, Clause S and shall contain the following information: a) the method of test used, BS 1377-3, test 5; b) the apparatus used: ©) the total organic carbon present inthe soil fraction passing a 2 mm test sieve to the nearest 0.1% of the or 4d) the percentage by dry mass of the original sample passing the 2 mm testsieve to the nearest 1%; and ‘on required by BS 1377-1:2016, 10.1 Loven dry mass of soil fe) the informs 6 Determination of the mass loss on ignition 6.1 Principle ‘This clause describes the procedure for determining the proportion by mass that is lost from a soil by ignition at a specified temperature, “The mass loss only relates to the organic content of peat, oreanic sand and materials that do not contain minerals that decompose or delystrate at the test temperature such as clay minerals, calcium ‘carbonate and gypsum. Such minerals might be responsible for the major proportion of the mass loss on ignition, ‘The requirements of BS 1377-1, where appropriate, shall apply to this test method. 6.2 Apparatus Drying oven, capable of maintaining a temperature of (50 #2.5) °C. Balance, readable to 1 g. Balance, readable to 0.001 g. Desiccator, cont ing anhydrous silica gel Test sieves, 2 mm and 425 ym aperture sizes, with receiver. 12. ©THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED | i : i BRITISH STANDARD 6.2.6 6.2.7 6.2.8 6.2.9 63 6.3.1 63.11 63.1.2 63.13 63.14 63.2 63.24 6.3.2.2 63.23 63.24 63.25 63.210 63.244 BS 1377-3:2018+A1:2021 Pestle and mortar, or a suitable mechanical crusher ‘Sample dividers ofthe multiple-slot type (riffle boxes), having widths of opening of 7 mm and 15 mm. Crucible or similar container, of about 30 ml capacity. Electric muffle furnace, capable of maintaining a temperature of (440 #25) °C. Procedure Preparation of crucible Before starting each series of tests, a test shall be carried out on the empty crucible or container as described in 6.3.1.2 to 6.3.14. ‘The crucible shal be placed in the mulfle Furnace, heated to (440 #25) °C, and maintained for 1h. “The crucible shall be removed from the furnace and allowed to coal to room temperature in the desiccator “The crucible shall be weighed to the nearest 0.001 « (m.) Preparation of test specimen Each test specimen shall be prepared for analysis from the laboratory sample as described in 6.3.2.2 to 63.211. (016, 8.3, and of the approximate ‘The initial sample shall be obtained as described in BS 1377, mass as specified in BS 1377-1:2016, Table S. “The sample shall be dried in the oven at (50 £2.5) °C, and cooled to room temperature in the desiccator ‘The sample shall be weighed to the nearest 0.1% and the mass recorded, m, (in g) “The sample shall be sieved on a 2 mm test sieve (if appropriate, guarded by a test sieve of larger aperture), and retained particles other than stones shall be crushed to pass the 2 mm test sieve, Fine material adhering to stones shall be brushed off into the sieve. The stones shall then be rejected, The mass ofthe sample passing the 2 mm test sieve shall be recorded to the nearest 0.1% (m,. Throughout these and subsequent operations care shall be taken to ensure that there is no Ince of fines ‘The material passing the 2 mm sieve shall be divided by suecessive riffing through the 15 mm divider to produce a sample weighing at least 10g ‘This sample shall be pulverized so thatiit passes the 425 um test sieve. ‘The sample shall be subdivided by rffling on the 7 mm divider to obtain test specimens each ‘weighing approximately 5 g. Throughout this and any subsequent operation the material shall be mixed thoroughly before any division and to avoid segregation during riffing Each specimen shall be placed in a prepared crucible and dried in the oven ata temperature of (50 42.5) °C. The specimens shall be deemed to be dry when the differences in successive weighings, carried out at intervals of 4h, do not exceed 0.1% of the original mass of the sample. ‘The specimen shall be allowed to cool to room temperature inthe desiccator and each crucible ‘weighed to 0.001 g (m,). (©THE BRITISH STANDARDS INSTITUTION 2021 -ALLRIGHTS RESERVED 13 BS 1377-3:2018+A1:2021 BRITISH STANDARD 63.3 63.3.1 63.3.2 6333 6.3.3. 64 64d 642 65 TA Tad Ignition of soil Ignite each test specimen as described in 6.3.3.2 t0 6.3.3.4. ‘The crucible with soil oF known weight, shall be placed in the unheated muffle furnace, and then heated to (440 +25) °C, and this temperature shall be maintained for not less than 3 h. NOTE The period required for ignition will vary with te typeof soil and size of sample. ‘The crucible and contents shall be removed from the furnace and allowed to coo! to room temperature in the desiccator, ‘The crucible and contents shall then be weighed to the nearest 0.001 g (m,) Calculations ‘The percentage of the original soil sample passing the 2 mm test sieve shall be calculated from the equation: fraction finer than 2mm = "2100 @ ™ where ‘m, isthe initial dry mass of sample (ing): ‘m, isthe mass ofthe sample passing the 2 mm test sieve (ing). “The mass loss on ignition, LOI, as a percentage of the dry mass of soil passinga 2 mm test sieve shall be calculated from the equation: Lot = "4 1009 © mm, where rm, isthe mass ofthe erucible and oven-dry soll specimen (ing): im, isthe mass ofthe erucible and specimen after ignition (in ); ‘m, isthe mass ofthe crucible (ing), Test report The test report shall state that the test was carried out in accordance with :2018+A1:2021 Gi, Clause 6 and shalll contain the following information: }) the mass loss on ignition as a percentage of the soi fraction passing the 2 mm test sieve, to two significant figures; ) the percentage by dry mass ofthe original sample passing the 2 mm test sieve, to the nearest 1%; and. 5 mm retained fraction consists of inert material such as quartz then the material shall be brushed lean of any adhering particles, which shall be added to the <2 mm fraction, and the inert fragments ‘hall be retained for weighing, Ifthe material consists of weakly cemented grains, they shall be broken down by gentle pounding using a clean agate or ceramic pestle and mortar and re-sieved. If the retained material consists of dried clay, silt, mudstone or siltstone or any material considered to be a potential host for sulfur minerals as identified by a suitably experienced person, it shall be crushed and added to the fraction passing the 2 mm sieve, which is retained for testing. ‘The <2 mm fraction shall be weighed to the nearest 0.1 g and the mass m, shall be recorded in g 16 © THE BRITISH STANDARDS INSTITUTION 2021 ~ ALL RIGHTS RESERVED 2 72.38 72.3.6 7.2.3.7 73.4. H STANDARD BS 1377-3:2018+A1:2021 Fine-grained material The dried fine-grained material shall be broken down using a clean ceramic mortar and rubber pestle, Any gravel size (>2 mm) material shall be removed for examination under‘a binocular microscope. Any fragments of inert material shall be brushed clean of any adhering particles, which shall be added to the disaggregated material and retained for weighing. Ifthe retained material consists of clay, mudstone, silt, siltstone or any material considered to be a potential host for sulfur minerals, as identified by a suitably experienced person, it shall be added to the disaggregated fraction which is retained for testing, ‘The <2 mm fraction shall be weighed to the nearest 0.1 gand the mass m, shall be recorded in g Extremely weak and very weak rock [After drying, samples shall be brushed clean of any loose particles and then broken down into fragments of less than 10 mm using a clean industrial fly press; alternatively, a hammer and steel plate or a steel pestle and mortar or other similar equipment may be used, The material is retained for testing, Care shall be taken when using mechanical crushing devices that samples clo not become heated above 60°C by the pounding action. NOTE For intact rock samples the tests are carried out on m, The fraction finer than 2 mm, m, is 0. Subdividing ‘The material retained for testing shall be mixed thoroughly and subdivided by cone and quartei riffing until a representative sub-sample of between 200 g and 300 gis obtained. Pai ‘The particle size reduction shall be accomplished using a clean tungsten carbide dise shatter mill, ‘or an equivalent type of mill The samples shall be subjected to successive episodes of between 10 and 15 seconds of milling, Longer periods shall be avoided as they might cause alteration to sulfur species, The powdered sample shall be passed through a 212 jm sieve, with any material retained on the 212 jum sieve re-ground and the process repeated. le size reduction Storage of processed material ‘When samples are to be stored before testing, the powdered samples shall be oven dried ata temperature of between 40 °C and 60°C for about 24 hours. The samples shall then be allowed to cool to room temperature ina desiccator with dry desiccant and stored as described in 7.2.2. ‘The method measures the water-soluble sulfate of solid samples. The prepared dry sample is mixed with de-ionized water with a ratio of 2:1 water to solid by mass ratio and the resultant filtered solution is tested for sulfate ions. The results obtained give the sulfate content at the time of sampling only. NOTE The test methods in 24 2.5, 26 and 2.7 may also be used to determine the sulfate content of samples of {groundwater and surface water provided they have been filtered using the method given n 2.2.25 and 7.3.3.6 as required. NOTE 2 Water-soluble sulfate san index value thats used fr the assessment ofthe potentially aggressive sulfate that might be readily leached from soll and rocks. The most common sulfate, hydrated calcium sulfate (CaSO, 2H _aypsum) has a relatively low solubility of about 1 500 mg/ISO, at room temperature. However, other sulfate ‘minerals, particularly those containing magnesium or sodium, have much higher solubility an, hence, pose greater risk to concrete, steet and construction materials Therefore, t might be necessary to test the water extract for (© THE BRITISH STANDARDS INSTITUTION 2021 ALL RIGHTS RESERVED 17 Bs 1377 7.3.2 73.24 73.22 TB22A 73.222 73.23 73.234 73.232 73. 73234 73235 73236 73237 73238 733 7334 5 10181-2021 BRITISH STANDARD cations; such as magnesium (Clause 10}, The total amount of potentialy reactive sulfate is given by the aca:soluble sulfate test in 2.9 Preparation of water: soil extract General ‘The requirements of BS 1377-1:2016, where appropriate, shall apply to this test method. Reagents 70%) for use if water 1n methods only. Nitric acid, analytical grade concentrated nitric acid, 1.42 g/ml (solution samples are to be stored for ICP-AES or gravimetric chemical determinat Hydrochloric acid, analytical grade concentrated hydrochloric acid, 1.19 g/ml (solution = 40%). Used ifsamples need to be stored for ICP-AES or gravimetric chemical determination methods only. Apparatus For test sample preparation prior to water:soll extraction see 7.2.3, Extraction bottle, a 250 ml capacity clean and dry, rigid plastic such as high-density polyethylene (HDPE) container with a water tight screw cap. Glass containers should not be used as they are susceptible to damage from the soil particles during the extraction, Mechanical shaker, a rotary tumbler or mechanical shaker capable of keeping 50 g of soil in suspension in 100 ml of water. Sample bottles, 30 ml to 50 ml capacity sterile polystyrene or polypropylene sample bottles with leak-proof caps. Vacuum fileration unit with filter funnel, flask and filter paper (e.g, Whatman No. 542”), Syringe filter, 0.45 jum membrane syringe filter. pH meter, calibrated, electronic pH meter. Laboratory glassware, including 75 mm diameter watch glass and $0 ml and 25 mi pipettes. Procedure ‘A30 gto 50 g representative portion of the oven-

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