INTERNATIONAL ISO STANDARD 10701 Fist edition 1994-04-01 Stee! and iron — Determination of sulfur content — Methylene blue spectrophotometric method Aciers et fontes — Dosage du soufre — Méthode spectrophotometrique au bleu de méttylene Refaronse numbar Iso 10701-18946) CopmrigMt bythe Intcational Urganivation Por Standardizstion Sal fou 04 1219 200ISO 10701:1994(E) Foreword ISO ithe Intemational Organization for Standardization) is a worldwide federation of national standards bodios {ISO membor Sodiosl. The werk of preparing Intematonal Standards is normally cadied out through ISO echnical cemmitiess. Each mamber bozy interested in a subject for Which @ technical commitise has been establishec hes the right to be renreserted on thet committee. Intemational organizations, gevernmental ard navgovernrental, “n lisison with ISO, also take part in the work. ISO collaborates closely with the International Electotechnical Commission {IEC) on all matters of elecrotechnical stanaardization. Draft International Standarde adopted by the technical commitices are circulated to the memaer hadies tor voting. Publication as an Intematiorat Stancard requires approval by at least 75 % of tie member bodies cesting avote, Interra-ional Standard ISO 10701 was prepared by Technical Committee ISOAIC 17, Steel, Subcormittes SC 1, Methods of determination of cherrical compostion. Annexas A, 14 B of this International Standard ara for informasion only. © Isc 104 Al ighis ‘esarvad. Unless otherwise spectied, no partof this publeation may be reprocuced Or utlizaa in any form er by ary means, slazecnic or mechanical, cluding pretocepying ond ricrfihn, without parmigsen h writing trem tha publisher, Internasonal Cagenization for Sancerdzstion Casa Pastae 55 + GF-I7IT Gereve 20 * Saitrerland Printod in Sweerland CopmrigMt by the Intentional Urganization Por Standardizstion Sal dou D4 126-28 200INTERNATIONAL STANDARD © iSO 1$0 1070" }994(E) Steel and iron — Determination of sulfur content — Methylene blue spectrophotometric method 1 Scope ‘This In‘erretional Standard specifies a methylene ble spectrophatometric method for the determination of sufur in steel and iron, ‘The method is applicable to sulfur contents between 0,000 3% (nvm! and 0,010 % (rm). However, niobium, silicon, tantalum and titanium intertere in ihe determination of sulfu: Depending on the concentration of the interfering el- ements, the application ranges and test porton masses given in table! apply. Table 1 oma wae comantafivcimareina | 7%, | apptaton sume vote Be (yn) % Ons) dmeoe pete ra | 20 | ae | 20 | om | Om 2 Normative references The following standards contain provisions whch, through ‘eferance in this text, constitule provisions of this Intemational Standard. At the time of publi- cation, the editions indiceted were valid. Alt standards are subject to revision, and rarties to agreements based on this International Standard are encouraged to investigate the possibility of apo'ying the most re- cent editions of the standards indicated below. Memwers of IEC anc ISO mantain regsters of cur rertly valid International Standerds, Copmright bythe International Urganization Por Standardizstion Sal dou D4 126-28 200 IS 977-2:1989, Selection and preparation of samples and fest pieces of wrought steels — Part Z: Sampies jor ihe determinaticn of the chernical composition. ISO 385-1:1984, Laboratory glassware — Bureties — Part 1: General sequirements, 1S0 648:1977, Laboratory Glassware — One-mark pipettes. ISO 1082:1983. Laboratory glassware — One-mark volumetric flasks. ISO 3698-1987, Veter for analyticar laboratory use — Specification and test methods. SC 5725:1986, Precision of test methods — Deter miation of repeatability and reproducibility for standard test method by inter-leboratory tests. 3 Principle Dissolution of 9 test potion in a mixture of hyerachloric and nitric acids. Eveporation with perchloric acid until white fumes appear ta remove hydrochloric and nitric acids. Dissolutien of the salts in hydrochioric acid, Evolution of hyérogen sulfide by reducing with a mixture of hyéroiodic and hygophosphorous acids in @ nitrogen atmosphere, dstilation, and absorption into zinc acetats solution. Formation of methylene blue by reacting with NN-dimethy-p-phenylanedianine and iron(|lit_ sol ution. Spectiaphotometric messirement st a wavelength of about 665 nm.4. Reagents During the enalysis, unless othanwise stated, use only reagents of recognized analytical arade with a ver low sulfur content, and only freshly prepared grade 2 water a8 spectiiad in ISO 3696, 4.1 Hydrochloric acid, » about +,19 gir 4.2 Hydrochloric acid, p about 1,19 giml, diluted 1415. 4.3 Perchlorie acid, p about 1,64 gil 4.4 Hydrobromic acid, p about 1,43 giml 4.5 Mixture of hydrochloric and nitric acids. Mix one volume of hydrochloric acid (#11 ard one volume ef ritric acid, p about 1,40 g/ml Propare immodistely before use. 46 Reducing reagent solution, Transfer 20¢ mI of hydriodie acid [about 87 % tra/ml] and 80ml of hypophesphorous acid about 50 % (miml] into the purifying apparatus (see figure). Purge with nitrogen (4.12) at a flowrate of 100 milimin for 10 min, to mix the acds and expel air from the system, Switch on the electric heating mentla. Hezt to boling and bol gently for about 120 min at @ temperature of about 118 “C in a current of nitrogen. When curification is completed {see 103), switch off the elactric hesting mentla, Then cool the solution and keep it ina brown battle, 4.7 Absorbing solution. Dissove 89 of zinc acemte dihydrate [ICH,COO),2n.2H,0] in 400 mi of weter. Add 200 mi af sodium hydroxide soluticn, 30 g/l, and 70 g of am: amonium chloride, and then dilute te 1090 ml with water. 48 tron, 10 gil solution. Weigh, to the nearest 0.01 a, 1.009 of pure iron which is free irom sulfur as sulfate. Transfer to 2 300 mi beaker, cover with a watch glsss, dissolve by heating with an addition of 20 mi of tydiachloric ace, (p about 1,19 girl, diluted 1+) and boi! gently for about 10 asin, Then edd 2 ml of nitric acd (p about CopmrigMt bythe Intcnational Organization Por Standardization Sal dou D4 126-28 200 eso 41,40 frei) drop by diop to oxidize iron, Remove the oxities of nitragen by boiling, and ccol to oor tem perature. Transfer to a 200 ml onemark valumetic flask, dilute to the mark with wetat and mix. 49° Iron{li chloride, solution. Dissove 1g of ironllil) chloride hexahydrate (FeCl.6H,01 in about 40 mi of water. Add 10 mi of hydrochioric acid (4.1) and cilute to 100 mi with weter. 4.10. N.N-dimethyl-p-phenylenedi in hydrochlaric acid medium. Dissove 0,5 g of A.N-dimethylep-pherylened amine chloride [NH,C.H,NICHe), 2HCI] 1m about 100 mi of ‘water, Add 230 ml of hydrochloric acid (2.1)ana dilute to 500 “rl with water. 4.11 Sulfur, standard solution. A.A1A Stock solution, corresponding to 1g of $ per titre. Weigh, to the nearest 0,000 1 g, 5435 2g of pot asslum suitete [minimum assey: 99,5 % im/ml), ore viously dried at 110°C for 2h and cooled to room temperature in a desiccator. Dissolve in water, trans- fer to.8 1 060 ml ene-mark volumettie flask quantitat- ively, dilute to the mark and mix. 1 mil of this stock solution contains 1 mg of S. 4412 Standard solution A, ccrraspending to 10 mg of $ per litre Transfer 10, ml of the stack solutian (4.11.1) 10 a 1 £00 mil one-mark volumetric flask, dilute te the mark with water and rnix, 1 ml of this standard solution contains 10 ug of S. 4.11.3 Standard solution B, coresconding to 1 mg of § per lite Transfer 10,0 ml of the standard solution (4.11.21 to 3 100 mi one-mark volumetric task, ditte to tha mark with weler and ins. Prepare the solution immediately hefore use. 1 mi of this standard solution contains 1 4g of S. 4.12 Nitrogen.ah TN || syarozan tte rap | | eeene2sem Couniesirtacecndaneee : ar eaivclen Be cmiond i wtregen /harrometar valet Taree-neck Flask capacity 506 mt! Figure 1 — Example of an apparatus for p sation of the reducing mixture Copmright bythe International Urganization Por Standardizstion Sal dou D4 126-28 200(SO 10707:1994(E) eso 5 Apparatus When the apparatus is used for the first Ume, oF after a long porad of disuse, blank tests shall bo carried out All volumetric glassware shall be close A, in escerd ——_<@Patitvely until stale low blank va uas are obtained ance with ISO 386-1, ISO 648 or ISO 1042, as appro- priete. 5.1.1 Decompostiion flask, ebout 300 ml in vor ume. Ordinary laboratory apparatus, and 5.1.2. Reflux condenser, about 199 mm m length. 5.13 Gas washing bottle, about 150 ml in volume. 5.1. Apparatus for reduction and distillation 5.1.4 Absorption flask, one-mark volumetric flask of capacity 20 ref or 100 mi Assemble tha apparatus for reduction and distillation as show" in figure2, Closerfitting grouréglass jcints «3.2. Speetrephotometes, equipped to measure shall be used, aboorbanco at a wavelongth of about 666 nm, Dimensions in millmaves 5 90 v0 ftv To conerser ! LL. yl 3 g| oze witee i = e os ites tune wuage 908 9 [pag] Aosoraton ase {capactiys 2) or 20 ml? Wastingbotte Deesnpasitien Haske apaciry: 300 mi Figure 2 — Example of an epparatus for reduction and distillation CopmrigMt bythe Intcational Urganization Por Standardization Sal dou D4 126-28 200Carry out sampling in accordance with ISO 377-2 or appropriate national standards for sies! and ron, 7 ‘Procedure WARNING — Perchloric acid vapour may cause explesions In the presence of ammonia, nitrous fumes or organic matter in general. 7.1 Test portion Weigh, to the nearest 1 mg, the mass given below 38 a functon of the expected sulfur content: @ sullur coments from 0,000.9 % (wim) 10 0,001 0 % (whl, mass of test portion about 1.00 9g; 9) sulfur contents from 0,001 0 % (n/m to. 0,010 % (n/n), mass cf test porticn about 0160 ¢. 1.2 Blank test Im parallel with the determination and following the same procedure, carry outa blank test using the same quantites of all the reagents, It is recommended that the blank value does not exceed 0,7 ug af sultur for sulfur contents up 10 0,001 % tain), of 1,5 yg of suk fur for sulfur contents from 0,001 % (vin to 0,010 % fev. 7.3 Determination 7.2.1 Preparation of the test solution Pace the test portion (7.1) in a decomgosttion flask 21.1), Add. 16 my! of the mikture of nydrachloric and nitre acids (4.5). After stancing at room tempersture for about 30 rin, heat gently until solvent ection Then, using a pipette, add §,0 ml of perchloric cid 14.3) and 1,0 ral of iron solution {4.8}, reat and evan- orai@ unil white fumes appear. After cooling, add 5 ml of hydrochlore acid 14.1}, (See clause © for a possible modification of this procedure.) Heat again and evaporate to furning on a hotplate at a tempera ture of about 260 °C, Then continus to evaporate until free from white fumes of perchloric acid and dry After cooling, sdd 10 ml of hydrochloric acid (4.*), haat to dissolve the salts and cool to room tempera- ture, Copmright bythe International Urganization Por Standardizstion Sal dou D4 126-28 200 Add 20 ml of the reducing reagent solution (4.6) to the Gecomposition flask (6 1.1} and allow to stand for 40 min, Pour 30 mt of water into the gas washing cottle (6.13). Place the appropriate volume of sbsorting solution (4.71 in an absorption vessel (5.1.4, eccording to tho oxpoctod sulfur content to be determined, as fallews: a Zor sulfur contents Jess than 0,001 0 % {eu/n), in- sroduce 10 ml of the absorbing solution (4.7} into @ 20 ml aasorpton flask; by for sulfur contents from 0,001 0 % im/n) to 0,010 % (n/n), introduce 50‘ of the absorbing solution t4.7] into a 100 ml absorption flask. With water flowing through the rethxx condenser .1.21, connect the decompostion flask (5.1.11 con taining the test solution. Pass nitrogen (4.12) through the apparatus at a flowrete of 100 mllmin, es shown in figure 2. Heat the test solution to a temperature of 114°C to 118 °C for 30 mn. This will notmaty be achieved by setting the hotplate temperature to about 250 °C {sce 19.2). Evolved gases ate convoyed by tho nitrogen carrier gas through the gas washing bottle 5.1.3} to the absorption vessel. 7.33 Golour development 7.33.1 For sulfur contents up to 0,001 0 % (min) Disconnect the 20 ml absorption flask (6.1.4) and the gas inlat tube from the eppsratus. Keaping the tip ct the tube in the absorbing solution, acd 1,0ml ct hycrechloric acid (4.2) from she upper and of the tube by using a micropipette to wash the inside surface of the tube. followed Sy rinsing with 1 ml of water. Remove the gas inlet tube. gently swirl the 20 mi ab- sorption fiask, and allow to stand for 20 -rin at 25 °C in a thermostat. Then edd 2,0 ml of N,N-dimethyl ppphenylenedismine solution (4.10; to the absorption flask 15.1.4) and shake gently, Immedistely add 2,4 ml of irontli) chloride solution 4.9}, and shake vigorously for t min, Dilute to the mark with water and mix. Allow to stand for 16 rin. 7.33.2 Forsulfur contents from 0,001 0% [r/m) to 0,010 % (n/m) Disconnect the 100 mi absorption flask (6.1.4) and the 928 inlet tubs from the epperstus. Keaping the tie of the tube in the absorbing solution, add 1,0 ml of hydrochloric acid (4.2) trom the Upper end of the tubeby using a micropipette to wash the inside surface of the tube, followed by rinsing with 1 ml or Zml of water. Remove the ges inet tubs, gently swit the 100 ml absorption flask, and alow to stand for 20 min at 25°C in a thermostat. Then add 10,0 ml of NJ-dimethy-p-phenylanediamna solution (4.10) to the absorption flask (6.1.4) and sheke gently. Im- mediately add 2,0 ml ef ron(lll) chloride solution (4.9), and shake vigorously for 1 min. Dilute to the mack wita water and mix Allow to stand for 16 rin. 7.34 Spectrophotometric measurement 7.34.1 For aulfur contents up to 0,001 0 % (min) Cary out the speetrophotametric measuremants with a call of { cm optical path langth 2: ¢ wavelength of about S65 nm, after adjusting the spectraphotometar (6.2) to zero ageinst water 7.34.2 For sulfur contents from 0,001 0 % bn) t0-0,010 % (rn/m) Carry out the spectrophotomatric measurements with a cell of 1 cm eptical path length at ¢ wavelength of about S65 nm, efter adjusting the spectrophotometer (5.2) to zero ageinst water. 7.4 Establishing the calibration graph 7.4.1 Preparation of cailbration solutions Introduce 1,6 mi of iron solution {4.8} into a series of Six decomposition flasks (6.1.1) and add the respec- tive volumes of sulfur standard solution (4.71) which, are given in table 2. Then aeld 15 ml of the mixture of hydrochioric and nitric acids (4.5), and 5,0 ml of perchloric acid 14.2), heat and evaporate to fuming. Proceed as described in the secand paragraph of 7.3.1 trom “After cooling, add ..” to the end cf 7.3.3. Copmriait bythe Intcnational Urganization Por Standardization Sal dou D4 126-28 200 Table 2 YVoruno of | Volume of itor | mtr | Comapond- ssutur | scaned | standard | ine mos ot solution A | solution B sulfur una. | eis weiwmi | 1 a ee : 0.001 0 ” ° - 10 16 - 3,0 30 = 50 56 - 16 75 = wo | 199 rr) = D ant 09 ote 05 - 5 10 - 0 20 - 0 30 7 0 50 = 0 1} Zero member, 7.42 Spectrophotometrie measurement 7.42.1 For sulfur contents up to 0,008 0 % (min) Cary out the spactrophotometrc measurements with a cell of 1 em optical path length at ¢ wavelength of about 665 nm, after adjusting the spectrophotemeter (6.2) to zero agains: the zero member (see table 2) 7.42.2 For sulfur contents from 0,001 D % jm} to 0,010 % (m/nh Carry out the spactrophotometric measurements with 2 coll of 1 cm optical path length at « wavelength of about 886 nm, after adjusting the spectrophotometer {6.2 to zero agains: the zero mamber tsee table 2). 7.43 Plotting the calibration graph Prepars the calibration graph by plotting the absorbance agdinst the sulfur concentrations, ex preased in micrograme per 20 ml fee 73.2.1] or por 100 mi of the enlour-ceveloped solution (see 7.3.3.2)8 Expression of reculte 8.1 Method of calculation Corvart tha absothance measwed in 7.3.4 into the corresponding mass, expressed in micrograms of sulfur, in tha colourdevelaped tast solution (see. 7.3.3.1 or 7.2.3.2) by using the calmratior graph (s8e 7.4.3), Tho sulfur contont, ws, axaraseed ea 2 percentage by mass, is given by the equatian 1, 100 Wig = long. — gg) X [ee = (3 — go) « 10°m where gy is the rmass, expressed in micrograms, of sulfur in the blank test solution; msi he mass, oxproscad ir micrograms, of sulfur in the test solution: m Ig she mass, in grams, of the test portion a. 8.2 Precision A planned trial of this methed was carried out by 11 or 13 laboratories, at 18 lavale of eulfur, each labore- tory making three determinations (see notes 1 and 21 of sulfur content at each level. ‘The test samples used are listed in table A1 The results ootcined were treated statistically in ac cordance with ISO 5725, The deta obtained showed 2 logarithmic relationship between sufur content and repeatability |r) or reproducibility (R and X,} of the test resus (see note 3h as summarized in table. The graphical reoresen- tetion of the figures is shown in figura 8.1 Copmright bythe International Urganization Por Standardizstion Sal dou D4 126-28 200 Table 3 Sut | repeauity | foproduaty we - 2 fe pone | aac | com | onoott 200s | oven | 20m 28 | 0000 14 none | oave17 | som37 | ooos 2 gore | omc? | comer | noe: noise | oaeca7 | coor | ogae 51 20100 | oor | coma | ogoe 74 NOTES 1. Tveo of the three determinations were coried aut under opsstabilty concitiors as detined in ISO 5728, 1. ane op- erator, samme apperetus, icentica operaticg conditions, same. calteation, anda minimum pariad of time. 2. The third determination was caviad out at a different time (on a different day) by te same ope'ator as in note 1 above, using the same apparatus wah ¢ new calibration, 3. From the resutt obtained on day 1. the reseatabilty ‘ob and reproducibility (Rj were calculated using the procecure specified ir ISO 8726, From the first result obtained an day 1 and the result obtzined on day 2, the withinsaborarany reproducibility 1R,) was calovted. 9 Special casa For a test portion eontaming selenium, the Srd io 8th tines of the 2nd paragraph of 7.31 should he changed to “After cooling, add 5 mt of hydrachlotic acid (4.1) and 5 ml of hydrobromic acid 14.4). Heat again. and evaporate unt white fumes appear and until absok utely dry, on a hoiplata et 2 temoereture of about 300°C." 10 Notes on procedure 10.1 Due to the extraordinary sensitivity of the method, it is important to eliminate sulfur es a con- tamination source. In prectice, it may be useful to brovide a room for this type of analys's, It the analyst chooses 1 "un twa reagent blanks, the lower one usually ie the eorrect ono, Spuricus contamination by sulfur nas been observed when new flasks. scrupulously ¢ eaned with aqua regia, were used. lis essential thet all semple treetrmants be carred out in scrupulously clesn lateratery stmosphere, ie, free from sulfurie acid fumes and any vapours or dusts containing sulfur or sulfur compounds,ate hiehiante To keep the euifur blank values low and constant (e.9, + =0,80 ug and ¢=0,15 ug of sulfur, special care should be given to the selection of all acids used, out it does not recessitete a purficetion procedure by distillation, 102 Chemically, the redusticn of sulfate to hydro gen sulfide is a difficult rection. To ensure 3 com- late recovery of sulfur, the reaction conditions shall be clesely controled. The optimum reducing tem perature is 114°C to 118 °C. If the reducing solution is excessively diluted by the sample solution, the boiing point is decreased and the reduction kinetics: are sowed appraciebly. At temperatures above 420°C, the acid mixture shows signs of decompo: sition of hypophosahorous acid and an incraasad for- mation of phosphine. The required temperature of the hotplate shall be es- tablished by 2 proliminary blank test with e ther memeter dipped ir tho heated solution. 403 To check the affectiveness of the purification, ‘connect the hydrogen sulfide trap (see figure 1) con- taining 10 mr of the absorbing solution (4.7) ard con- ‘tinue heating for 39 min. Disconnect the trap. Devalog the colour according te the 2nd to 10th lines of 7.3.3.1, using close-fitting ground-glass stopper as needed. Dilute to about CopmrigMt by the Intentional Organization Por Standardization Sal dou D4 126-28 200 20 mibby adding & ml of water and mix. Allow ta stand for 15 min, Carry our the spectroplictometic measurement with a call of 1 cm optical path length at s wavelength of about 685 nm, after adjusting the spectrometer (6.2) to zero against water. ‘The purification ts completed when the obtained absorbance is below 9,086 icomesponding to 1 ng of Si. 11. Test report The test report shall include the following information: @) all information necessary for the identification of ‘the sample, the laboratory and the date of analy: sis; b) the method used by reference to this Internstionel Standard; c} the results, and the form in which they aro ox. pressed; d} ary unusual features noted during the deteimi- ration: ¢} ary cparaticn nat specified in this intornational Stancard, ex any optional operation which may have influenced the rasults.aie SO WOT TS94E) Annex A informative} Additional information on the interna’ nal cooperative tests. Table3 was cerived from the resuns of international «NOTE 4 _These ‘bur samples were omitiad trom tke re analytical Vials carrisd out in 1969 ard 1881 on 12 steesion eakuletion for the fellowing reasons, steel semples and four iron samples in nine countriae Sample 1) fpue ion) sult eontot less thon to [pure fron) sulfur content is less than invoNving 11 oF 3 laboratories Samole 1 (pure iron) sul “he results of the trials were reported in document sumple 7 teen tent ISOjTC 17)SC 1 N 839, March 1990 and document BTS ah (Stainless Staab: titanium ent ISO/TC 17/SC 1 N 916, February 1992, Tho graphical ‘nl Yepresentation of the precision data is given in Sample 19) ¢highsiicen swelt;siison content annex B. 27 & bin The test samples used are listed in table A.1 Samate 12) nodular ironk: sticon content 23.% (min) Table At Sulfur content, % inn} Precision ‘Sample Cortiied Found Repeatability | Reproduelbliy oa Re r zg By 1) JSS 002-2 inure iron) 00308 | ooosce | ooosae | 9,008 | 0.00010 | 0.00000 2) JSS 098-2 fpure irord aoc04 | 00042 | 000042 | 0,00010 | 000016 | 0,c0016 3) ECAM 0964 (unalioyedatesd | 9.9008 | oo0ee« | occas | s,00017 | 000032 | oc0029 4) JSS 2444 tunelleyed steel eo015 | 90064 | 900188 | 0.00028 | o,00077 | 0,co0.40 9) JSS 240-8 junaloyed steel) eco | 000575 | oo0ses | 00082 | oonrsz | ocov78 )_EGAM 483-1 (cast iran) acce6 | coos 17 | onvere | ooore7 | amos | o,coves 7) NBS 3483 istainloss steed 0.9007 | 0000s: | 00052 | 00011 | 000080 | c.con09 8) JSS 654-10 {stainless steel 00007 | 00064 | 000062 | 0.00018 | 0.00029 | o,cov10 9} 18S 611-8 thah-spesd steed 00013 | 090: 35 | 000134 | 0.00016 | aoosa | c.conz3 10) CCAM 191-1 thiah-sicon steed | 0.0017 | oao:s2 | ano1as | 9.00021 | aon 44 | 0,c0072 41) BCRM 285-1 thigh-lioy steal) | 9.9024 | oao2 1 | agosi1 | o00021 | 0.00076 | o.coaze 42) ECRM 481-1 nodular “ont c.coa | 900924 | anos 20 | 000043 | omy | c.coo4t 13) JSS 8509 tstailess sree 0053 | 0052 | 000840 | o,000¢2 | oooag7 | c.con29 44) ECRM 235-1 thighalloy stooll | 00072 | oaosat | ancean | nneor6 | 0.0063 | c.co03s 15} USS 654? {staitlass stool 0,908.3 | 000912 | ovesos | o,00042 | 900158 | 0,000 57 16)_N3S.299 ‘Se-steinless steal} voray | corzs | cora | oo125 | 0.00318 | 0.00108 Yigy) general mean within @ dey Fz _general mean between days 1) Tost portion = 0:25 g 9 Copmright bythe International Urganization Por Standardizstion Sal dou D4 126-28 200ISO 10701:1994(E} — Annex B (informative) Graphical representation of pre 0.905 Rejected see ncte 4) on02 2904 Precision oa0as oo00z F ogoor L- (a ea000s F- 00000 80007 GOR 6005 ons O07 8008 007-002 Sulfur content sored} la r= 0,622 4 Ig is, ~ 1,895 5 Igk= 075 8 g He, - 1.4005 Ig Ry = 0,548 7 Ig 52 — 2,036 8 where ey _ is the everage sulfur content, exoressed as a percentage by mass, obtained within a day; Wea_ is the average sulfur content, exoressed as a percentage by mass, obtained between days, Figure — Logarithmle relationship between sulfur content fi.) and repestability (7) or reproducibility tk and 10 CopmrigMt bythe Intcnational Urganization Por Standardization Sal dou 04 1b26-29 2002 ISO ICS 77,080.00 Descriptors: scl, iron, cherical nahsia, detenrinsicn of content, sulphur, secirometic methed rica besedion 10 pages Copright bythe International Urganization Por Standardizstion an 04 1:25:29 2008