Standard for Edible Salt (Ordinary, Washed and Iodized)

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U S~tllHC'lillffiHLUfiltutrua @0!S ant tuan.t,Un f181~91Dn fag~m ifiiDoon s~ms~blh;1~~tU18~tAt'drnitlJ~tlJlm ci , 0 ~ 0 • tITTgt1H9Jt1mrut9filit1jUu~~LflH98 t I 9Jltlltt:lmmsfotitBi f1t1H~tfinJtma !SID HSt,n.tm ~g1~90~ faaMm w1Doo0 ~ti~tiLflr 1 arujlUln'!ffitAm ci nrum1~3fmfitt]t1tt:lmmm~lllfint1t]tithnsg fit'dntlH~f!)tBig~mrfilllfiu1n 1 1 I HUrufithtlruntlrumsntitht,ffr~rutt:lrummuUITT~'1Jt:ljH!jJtt,fis ,, '1 fll]fU1StlrutnuC]tl9n ~irtft,9 mmue]tit'itt,mH~ yme]ti9n»uruGythfi ci tJnnruth~mi}lmBint1mrujutlt]{jLflnsg ~rnrmsm.n~tmrnHwnnnrt]{jth1mrntumfii 1 b51~1~6~$ : SLS 79: 1987-Specification for edible common salt (Ordinary, Washed and Iodized) SLS 80: 1970-Seylon Standards specification for free-flowing table salt CODEX STAN 150-1985, Rev. 1-1997, Amend. 1-1999, Amend. 2-2001-Codex standards for food grade salt. ~s~~tfi~~~ CS 0055:2007 gJn~ ~5ruts~G~~c~5rui3~Gn ~5ruMs ~s~5ru~~~) Edible Salt (ordinary, washed and iodized) ~~rJuts&firuiiinnmai11 tlilHil~n~fi »ITTYm mn1r.;~uat1m1tg '1Jlfi 1~ tmt'hlts mnnn~Jtlmntlmst11~Wll'hltgm'hl at1murui:1s~mrunumti»~rnntr1snumts11m nummit1 St1Hum~CTjr:J '1 ( (~~\ b. lie.ss!.!~ess (t>J..wv-l~ ctc&\- b vv..l"'°" , ~ HUmfithtlmntlmtnsnt1thtrfr~1ruttlmtnStlilitil~";}r:JJtitiJtt~S '1 flt!jfWStlmnm'] ~~ ~&~ n9nru~t9 mnmt]nfittmtr'S ymQJri'9nnumrs11m~ 1 -:::::: Vti.A.::> ~ f\\\.~-\ W\\AQ l\Mr ~Ot0&tD) m. 0 numu'!;!ITTSt1nummit1 t!j1tnthtmtlt~~mfoot191~thnnu91 num~CTjr:J t!j1hi 1 munutfi~mt1 0 t19r~thtmtl9ythtHJi 1 1 m. ID tlmntlmts&t!jfhimsmillru YtUuniittJtUlmtilliiru '1 uum1ist!j1tnsmti1is~g tr:Jmmm1Tmtlli'] ~uth ~n~ firnurnth~ firnu~yajltl ruummjru st1 ium~ttlJt19tr:Jmtg9JnumHs~gt£firu 1 m. m tlmntlmtS&t!j1tntrummrntrmn~J1tr:Jmmsfot1ut1mnt1 0 tsimmtr:lmmmgm~ 1 truurnH1GN1L'hltr:lmms~tilliimqt1~rnm~t1ttmm1srnnt1 0 1 mnt10: mnhfrJnthluruu1tmn " 1~N1l~ <::# mnmnrui: 0 (OA.'M~ 0 »Um c. uum 0 c. oo »Um °' mmru d n .. ti'i:Teil mlt1 »mr:J I V oOJ a o. • ': '"• v rutruigm;mm f'.inthmmmrnmru 6.0 6.0 5.0 aurugs a ncP 0 <::# 0 1.0 0.5 0.5 v mmntrs1mirunt19n»tmrn1 v ~ ~nth aurugs tu ... 1 ncP \V..~~ '> m~uru rnmrurunv 1 l>- 96 0 96 5 97.0 eiJt3Jt!lj! ,, (NaCl) HUJUHn finthffifiH.UtS · · ~uC.J..... 2.0 fil11m~1ruimu~9mun~eiJt3JHtJl ttfiu- - 1 v nn finthmmm1stiiru~n woW _s&\ ~ 30-50 ~trJt3 (I) ~nth mg/kg tBHUru~n - ... \~ 7.5- 8.5 auruiJs rn M"' nnnncJmru: Uj1Citmrunrnitrurugmmriim~~tlJt3 tsitJ%jH9J~tmu~n~fis~~nti'US 1 1 1 " ~SS~ tLUgtumu1tmfi I u1mnn~trJt3tsigtlmrutlrunHBU,j1~uthtl 50 mg/kg I I 1 ,' 1iuru1'.isrn1msfil11m~n~fiutlu1milllstlJ1tl91~1uurunti!m1t3rumuuwtLm~~fit3ru 1 1 ~ammurutinttfitmrut~m mforuru1'.Jsror~mstruruu1mruifiruifithHfimm~1 fillltnnt3umtltrrm:r: I tl lJ fi- mmrusu (As) HSUj1tLUSthtl O.rit!LfilfiLn U'1Jlftth As. 2- 9~lt3tl (Cu) HSUj1tLGSthtl ~t!Lfilt:iLn uqpfith Cu. TI- fililll (Pb) HSUjftt,tisthtl ~trt,filt:il,fi uqpfith Pb. m- rn~Hcj}tr (Cd) HSUj1tt,usthtl o.ritrt,nifitn U'1Jlftth cd. ,, ., fl. ~SS~t?es.5 Hmilm'tstlmn11yiiuruu1tmi:;rnrH~truimmmtr~~thrnifth~fomrumrnli~tm 1 ttlHJmmmrn1H~f~~~t3'u~fitmrurnrnli~tmtsttmt'.Jm~umun1rnrmstt~f~thtl v 1UJnt3rutlmntlrums~fitmt3rutt3tfmd'funru itifilll~tlmn rnnfu~tl m1'1?fl~n stl m1~nti'USHurufilntlu1tmfi1]f1nmsuwi1~ttljtu~n~unsfim'tsrnmt;Jilfill1m~ ,, 2 a. • A m~s ~~ ~ tS~ em~6 ~ ~~fi~nn "I> ,., 0 ~ ~ rn~tg ~fi"15c:Q1tHUntirumr»~HITT~Hil'i:l~~th~ CS 001 :2000 uruntirutlruhnun~ '1 ..... HUrutiYm .... urum~rurng mrtntfti~tl~msrutlrnjtBi!Jiltrlft1Jit]~rul]m9jS '1 tBitruMUn I tfu~tls~m9 mrtnmsmnsil~n"1lc:Q1tiJ1Mrn1Wttlrummnsms~uITTtlttrntr : n- t~gtlruntlru ... " Hlirut:rnrn" ... ~ tJ 0 .> a- rnyigstlmrum~s mtlutn stl1y ~nmnmm fi- mruit3mtr u mnttlrumsmumm (Jo> ""' 1 c.r..1 tu- g-gs~~ ~ntlllfil'i:l y figJtiilY ,, il- trua9J~ ,, y truauti u- 1umrut~Ytstiruntlru ci e>. l!J Jiururni~ e>. l!J. 0 tlmntlrurngrnrmmrn~tlntltl~~mt»9foJs ci tBitmMumrn~tl8Yi!m9 rnrtn I msiinstl~nruc;wuJ1Mrn1Wttlrumnmsms~nmtlttrntr : n- rnyigtiruntlru" Hlimrnltl" c t.J c cl a- rnyigstlmrum~s mtlutn s~vy ~nmnmm ei- mruit3mtr u u mnttlmmsugumm ~ 1 c.>'U ill- g-gs~~ ~ntlll,iil'i:J y it9jl,ii1Y ,, il- tffi89jfi ,, y tffiBljtl u- UJmrut~tJtstimm~m ci @.ID. l!J tl~Snrt)tlttirumst111mn~~tltl!!n9t]stl!!nmfimrtnmmrn~tltBiOtltnru '1 tBi 1 trutnrustzm91]ftnmsiinstlqrinruc;wnJ1Mrn1Mttlrumnmsms~uITTtlttrntr : n- t~gtlmntlru ... " Hururuitl" ei- tru39Jii y truafjtl '1 ,, 3 @.cn @.m.0 tlmritlrutsgrnfirimmru~utilitlMmHJtsi!Jtltltl~rutH9t9JBtMmuit3rumsrmru I Yst~tlthtl nrlfIUJi'tlu1 ytru~tltmtmuumru~tlMHrHJrun~ru '1 tsitrun~u yfiluntru~us~ruSJ rnririmsmn'Bil'lJlnMtJ;J1uJ1rumi~tt3rumumsms~r rtfitnB~ualilttfilH: n- tmngtlmritlru" »uru»rut3" ~ u 1 a- tbl.[lgstlmMru~s tntmtn Billy lifitufimru ei- mllii~mH W' umntt3mm£mgumm 1 tJo1.I '1 ill- 9lJ~mrn ~rithLfilH y ri9JLll1H v tl- tffiB9j~ y U1H3fjt:l v u- mnJth" ~mmnt~tl~riUithfistlry~mrn~tmm9riJ" '1 .> 0 0 0 ' ts- ttl-rn v tlru~rntltlnnrum 1 ~- tut9Mt~a1sumntlm -i tsitmuitlmnumrnrmmtfitmrutmruut~Htuinn~u.Umi!ruYttGs stlrnrms rufiwnutlum1~tlmmtl~amrituimrn11: tbl.[lgtlmritlmUJrfomstumrurmil uJlrumirutsitru'JJln 89ltnrnn" nurut!jruH - nuruijajti" .. »urumiruth~tt:Jrt I .. nurums1mijs" <Jru '1 mHrnrMHrHJ '1 @. m. l£l tl~SnL]tlttlrumswnmmtlil!Jn9QJBilUnmA U)ftnmmfu~tltsi!]~tnfil '1 tm 1 trumru'B~m9 U]ftnmsmn'2il'JJlnfil'.Y1uJ1rumiru it:Jrumumsms~r~rims ~ualilttfilH : n- tmngtlmntlru" num»ruti ~ u .. 1 ~- tmB9J~ ytruBfjtl -i v mtt}fiQ!JttlirutJJl~~mm~m '1 ~ 1 1tiMl~1sm~mn~Jtlmtitlmfilntlt~rnmL]lfitifmH~tmiHmHmr~Jf1s~~mnsg mrmsfmniitsirJtlSUM*~ n '1 1 4 AN N d. §~~1t~GijG~~ tmnt~1H'.ltmnsrm1nmijttiJ~tirn& tsimrut~mttrnt'i1]1ttlittnriit~trhitu~mrun ttlru'lPmfmntlmN-n s~ttf1tuirutfitrtn9nuny9nttlrumsrnrr~~ ~u9nun 1 rnn~tm~w1himatt~r~mtrrtfru1l~ttlrumsfo~q~auruw§ a tlru m 1 d. c;.10 u 0 " • 0 OJ 0 9Jnmgtu91]1rnturnrumuim1~truitrt9'lmHmrnirts~ij~nag ., turustuuisumt] 'i " m~rnntBjltr x + l .ls ttlrutnBt'iilllfrlt~ruttUttnrumgtlrum~1mmmilllrunUltr - U OJ • OCI 0 0 o; t9imruttlrutnat~mrumtrtlilllu v n n.m.m ~uth~ti:1Bfillliithfitru~mfi~s l n 1 fSI _ Mean ( X) = Sum of the obser\.·ed values Number ofvalues - Standard deviation (s) = The positive square root of the quotient obtained by dividing the sum of squares of the deviations of the test results from their arithmetic mean, by one less than the number of test results. 5 ~ f'i. 0 9Je'i: .. • o&) 0 0 0 0 0. """ 0 ~ • • nrumrun3rumst,utn9S~9Ul~u~ S~'1Jn!J~WH1i!t1Hstlrunng y rnmr~n~~1i!ru 1 mrmii~nthth9J~1i!lil ,, '1 • .~ • 6 f'i.~ gm rnmnnm.utlruettlru ,, fi.l!J.0 ~Jrlmntirur\9J~B1i!li19 ,, UJftnmmgm~t~Hju'1]1firimblH~trnlm9i's~rnr~Jf1s 11. l!J. l!J tl~smrutm]rl9JftB1i!m ,,

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0 "": .o mf rn rnnfmmstrnrmru mi 'U ':t} 'I U. N 11. m. l!J ~Jrlmnrlrug~mmrui IB~otrnH mrfomsi:lmuc:nfimrus~m9ti:lrummt~ruuru I 0 o,) ' °'~ 0 Ort. °' 0 ~uuuryu n. l!J.IB ti:hmtt,ut,mruaumruirnmrmnliJrlrunrlruruHrnJ tUllilfiJ rlmnrlruti:Jrug~rumsrng rnrfo'12nJHTltrurnrTIJfti:lrumsfa~t1~tluryu l!J. 0 8~ 1 IB.IB '1 t,ufilmumrumiirngmsnbUtltt,tfa rlmm~rurimbUu rnrfomstt,~rumn mc:nfimrus~m9ti:lrummwrumn~ug~tluryun. l!J. IB ttlimmrms'1'SnJ'1timrni I 0 '°"? 01 ·""" • c) mHmrnittsrnimnnnrumi tuimrumr:tfuautsnmurlrunrlrusHm9u3rums 0) 0 0 'U O'N ~ 11 U. U. ':J tt,UruurutErn l]ftnms'1'9nJ'flGmt9imHrnr~Jfti:lrumsfa~rJ~Tiru;m , !B. 0 9~ !B. l!J '1 6 • Ol Mtllilt:r I n. m. ~ rullilrutsiiJtimr;timtr3mmmt~ruuru~r;nutlru;m , n. m. m 1]1tfimsmiru~m~tthij msth9r~iiJtimr;timmiru~m~t~ruit; tUiruiiJtimr;timti3mmsg~mtSg 1]1tr; mm~rn~rnimtrmH~J1tttitl 9tr3mmsfounumnu0 , 1 • • • d mmruurnnrum Determination of moisture a.0 emu a. 0.0 ftsr1rnr;iiJtimr;timmfi~§!J1H9tutmm 1£l~ounmmquqrirutJn t~HJ~tJ1rut9i thttrji 1 mJltl~mmnumsug~r;rrisaJmmtJJ~m , 1 a. 0.1£l yuiiJtimr;timtutmm 0otmtr tllfi~mtmuur3uti3mmsyusurugrithtfs <r3u , " tlllilg mmrm stlmsmiitlgmiru) 1 u 1 rut:rmsinU9rutrmmfilmUlrrm .... v ~~0-0~0 et 'tJ 1 111 " 1 " HilJltru nurru:mmtiiu~r;tl~r; ~ niiu 1 t~~~gtmhfi tmnu;PUfftJUrutlliiH 1 , Jt;ytln I t~filHSITT~fil~n ucugf1tr34 2uyur3ttim9rnj~1QJ iUJm;Jrurnri~ru~ " , rnumryumu~nmnthtl9~1istmru~ o.000unt:r 1 a.~ mnnuun rutlliit:r <rnmrufir;thmru) = ml - m 2 x 1oo ml fit - iiru~umuruii1timr;timtr3mmsrunruntlt~mru t1 1J TifithUmt:r 0 C""I " • ..., 0 c 0 tnrutjUttmrurn~Jtimntim ~nthtmt:r 1 mruju'1~3tlruntlruir.3rumaMl!n .. Preparation of the dried sample Spread about 200g of the sample obtained as in 8-1-1 on a Petri dish and dry by the method given in 8-1-2. The dried material shall be referred to as the dried sample and shall be used in the tests where so indicated. 7 m1nnniirtn1trmitlrutiarnnmnl19n

1 I Determination of insoluble matter in water D.1 Procedure D.1.1 Weigh, to the nearest O.Olg, approximately 20g of the dried sample (see Appendix C), dissolve it in 200 ml of water and heat to boiling. Cool and filter the solution through a weighed glass crucible. Wash the residue with water until the washings does not give any opalescence when tested with silver nitrate solution. Collect the filtrate and washings in a one-liter graduated flask and dilute to the mark. Reserve the solution so obtained for subsequent tests. D .1 .2 Dry the crucible along with the residue at l 05 °C to 110 °C and weigh. Repeat drying and weighing procedures until the difference between two successive weightings does not exceed 0.001 g. D.2 Calculation m Insoluble matter in water, per cent by mass = - 1 x 100 where, m1 = mass, in g, of the residue; and m2 = mass, in g, of the dried sample taken for the test. Note: The residue will include free-flowing agents if added. m1nnniiriJtlJYtr! " Determination of sodium chloride E.1 Determination of anions and cations to calculate sodium chloride Determine the anions and cations given in first column of Table 3, by the methods prescribed in second column of the table. Table 3: Anions and cations Anion or cation Method of test Carbonate, as C0 3 Appendix F Calcium, as Ca Appendix G Magnesium, as Mg Appendix G Sulfate, as S04 Appendix H Total chloride, as Cl Appendix J Potassiwn, as K Appendix K 8 E.2 Calculation of residual chloride Express the carbonate as calcium carbonate or as sodium carbonate in absence of calcium and magnesium. If there is excess of calcium over the calcium carbonate, combine all the calcium with the sulfate and express the result as percentage of calcium sulfate. If there is excess of sulfate over what is required for calcium, combine the excess with magnesium and express the result as percentage of magnesium sulfate. If there is excess of calcium over the calcium sulfate, express it as percentage of calcium chloride and deduct the chloride corresponding to it · from the total chloride. Calculate the balance of magnesium as magnesium chloride and deduct the chloride corresponding to it from the chloride content. Also, deduct from the chloride content and amount of chloride corresponding to potassium content and express it as percentage of potassium chloride. The remaining chloride content is referred to as residual chloride. E.3 Calculation of sodium chloride Sodium chloride, as NaCl, per cent by mass = Residual chloride, as Cl x 1.648 mniMnmmunn .. Determination of carbonate F.1 Reagents F. l. l Hydrochloric acid, standard volumetric solution, c (HCl) = 0.1 mol/l F .1.2 Methyl orange indicator solution Dissolve 0.1 g of methyl orange in I 00 ml of water. F.2 Procedure Pipette out 100 ml of the solution reserved in D-1-1 and titrate against standard hydrochloric acid (F-1-1) using methyl orange (F-1 -2) as indicator. F.3 Calculation 3V Carbonate, as C03, percent by mass = - m where, V = volume, in ml, of standard hydrochloric acid used in the titration, and m = mass, in g, of the dried sample taken for the test in D-1-1. 9 e . t t A It mrrrnnnmmMJY .. a~ tntr]MJY Determination of calcium and magnesium G.1 Reagents G.1.1 Standard calcium solution Weigh, 1.000 g of calcium carbonate dried at 120 °C and dissolve it in the minimum quantity of dilute hydrochloric acid. Dilute the solution to one liter in a graduated flask. One milliliter of this solution is equivalent to 0.4008 mg of calcium. G.1.2 Ammonium chloride- ammonium hydroxide buffer solution Dissolve 67.5 g of ammonium chloride in a mixture of 570 ml ammonium hydroxide (rel. den = 0.90) and 250 ml of water. Also dissolve separately a mixture of 0.931 g of disodium ethylene diamine tetra acetate dehydrate and 0.616 g of magnesium sulfate (MgS04 , 7H2 0) in about 50 ml of water. Mix the two solutions and dilute to one liter. Note: Five milliliters of buffer solution added to 50 ml of distilled water shall not consume more than a drop of EDT A solution to change to distinct blue with e1iochrome black T indicator. G.1.3 Eriochrome black T indicator solution Dissolve 0.1 g of the dye in 20 ml of rectified spirit. This solution shall be prepared fresh every week. G.1.4 Standard EDTA solution Dissolve 3.72 g of sodium ethylene diamine tetra acetate dehydrate in water and dilute in a graduated flask to one liter. The solution shall be standardized frequently against standard calcium solution following the procedure given in G-2. G.1.5 Dilute solution hydroxide, approximately 10 per cent (mN) solution. G.1 .6 Murexide indicator solution Grind 0.2 g of murexide with 10 g of sodium chloride until the mixture is homogeneous. Thus 0.2 g of the mixture is suitable for 100 ml of the sample solution. G. l.7 Calcein indicator Grind thoroughly 0.1 g of calcein and 0.06 g of thymolphthalein with 10 g of potassium chloride. G.2 Procedure G.2.1 Standardization of EDTA solution 10 G.2.1.1 Transfer 25 ml of standard calcium solution (G-1-1) into a conical flask, add 25 ml of water, 10 ml of ammonium chloride-ammonium hydroxide buffer solution (G-1-2), 5 drops of eriochrome black T indicator solution (G-1-3) and titrate against the standard EDTA solution (G-1-4) to a pure blue end point. G.2.1.2 Titrate 25 ml of the buffer solution (G-1-2) with EDTA solution (G-1-4) using eriochrome black T indicator (G-1-3). Subtract the buffer correction for 10 ml (usually it will be 0.1 ml) from the reading obtained in (G-2-1-1) and note the final titre value. Calculation the calcium equivalent to 1 ml of EDT A solution (saym1). G.2.2 Determination of calcium and magnesium G.2.2.1 Transfer 100 ml of the solution reserved in D-1 -1 into a 250 ml conical flask, add 10 ml ammonium chlo1ide-ammonium hydroxide buffer solution (G- 1-2), and 5 drops of eriochrome black T indicator solution (G-1-3). Titrate against standard EDTA solution (G-1-4) till red wine colour of the solution changes to pure blue end point. Note the volume of the EDTA solution used in the titration. G.2.2.2 Transfer 100 ml of the solution reserved in D-1-1 into 250 ml conical flask, add 5 ml of sodium hydroxide solution (Gl-5) and stir well. add 0.2 g of murexide indicator (G-1-6) or 100 mg of calcein indicator (G-1-7) (see Note) and titrate against standard EDTA solution (G-1-4) till red wine colour of the solution changes to pure blue end point with murexide or green to purple with calcein indicator. Note the volume of the EDTA solution used in the titration. Note the volume of the EDTA solution used in the titration. Note: Patton and reeder's indicator may also be used in place of murexide indicator or mixed calcein indicator. G.3 Calculation . m 1 xV2 Calcium, as Ca, per cent by mass = 2 . m(V. 1 1 - V) Magnesrnm as Mg, per cent by mass = 0.6080 2 m2 where, m 1 = mass, in mg, of calcium equivalent to ml of EDTA solution (as determined in (G-2-1 ); V 1 = volume, in ml, of standard EDTA solution used in G-2-2-1; V2 = volume, in ml, of standard EDTA solution used in G-2-2-2 ; m1 = mass, in g, of the dried sample taken for the test in D-1-1. 11 " §iS~~~ e m:nruu1filruunet I ., Determination of sulfate H. I Reagents H .1.1 Standard barium chloride, 0.025 mol/l solution. Dissolve 6.108 g of barium chloride dehydrate in water and make up to one liter. H.1.2 Dilute hydrochloric acid, approximately 1 mol/l solution. H. 1.3 Ammonium chloride-ammonium hydroxide buffer solution, same as in G-1 -2. H. 1.4) Eriochrome black T indicator solution, same as in G-1-3 . H.1 .5 Standard EDTA solution. Weigh 3.72 g of disodium ethylene diamine tetra acetate dehydrate in water and dilute in a graduated flask to one liter. The solution shall be standardized for frequently against standard barium chloride solution (H-1-1) and follow the procedure given in (G2-2). One milliliter of the standard EDTA solution is equivalent to 0.001 374 g of barium or 0.000 96 g of sulfate. H.2 Procedure H.2.1 Pipette out 20 ml of standard barium chloride solution (H-1-1) into a conical flask, add 2 drops of hydrochloric acid (H-1-2) and 10 ml of ammonium chloride-ammonium hydroxide buffer solution (H-1-3). Dilute with water to about 50 ml, add five drops of eriochrome black T indicator solution (H-1 -4) and titrate against standard EDT A solution (H- 1-5) to pure blue end point. Note the volume of the EDTA solution used in the titration. H.2.2 Pipette out 100 ml of the solution reserved in D-1 -1 and add two drops of hydrochloric acid (Hl-2) and heat to gentle boiling. To the hot solution, add with a pipette 20 ml of standard barium chloride solution (H-1-1). Boil gently for about 5 minutes and then cool to room temperature. The solution will be neutral or slightly acidic when tested with a litmus paper. Add 10 ml of ammonium chloride - ammonium hydroxide buffer solution (H-1-3) and five drops of eriochrome black T indicator solution (H-1-4). Titrate against standard EDTA solution to pure blue end point. Note the volume of the EDT A solution used in the titration. H.3 Calculation Sul fate, as S0 4 , per cent by m ass = 0.96 Vi + V2 + V3 m where, V1 = volume, in ml, of standard EDTA solution used in H-2-1; V2 = volume, in ml, of standard EDTA solution used in G-2-2-1 (total Ca and Mg); V3 =volume, in ml, of standard EDTA solution used in H-2-2; and m = mass, in g, of the dried sample taken for the test in D-1-1. 12 m11iruinn1Mm .... I Determination of total chloride J .1 R eagents J.1.1 Potassium chromate indicator, 5 per cent (m/v) solution. J.1.2 Silver nitrate, standard volumetric solution c(AgN03) = 0.1 mol/l. J.2 Procedure J.2.1 Transfer 10 ml of the solution reserved in D-1-1 into a conical flask and add 1 ml of potassium chromate indicator solution (J-1 - 1). Titrate against standard silver nitrate solution (J-1 -2) until the reddish brown tinge persists after brisk shaking. Carry out a blank determination. J.3 Calculation Total chloride, as Cl, per cent by mass = 354.6 V x c m where, V = volume, in ml, of standard silver nitrate solution used in the titration, corrected to blank; c = concentration, in mol/l, of standard silver nitrate solution used; and m = mass, in g, of the dried sample taken for the test in D-1-1. m1nruintjmMMJY .. Determination of potassium K.1 Apparatus K.1.1 Simple flame photometer, equipped with potassium filter corresponding to wave length of 767 run. K.1.2 Ordinary laboratory apparatus K.2 Reagents K.2.1 Standard potassium solution Weigh 1.0 g of potassium chloride, dissolve in distilled water and dilute to one milliliter with distilled water in a measuring flask. This solution contains 0.1 g of potassium chloride per I 00 ml. K.2.2 Standard dilute potassium solutions Dilute 10 ml, 20 ml, 40 ml, 60 ml, and 80 ml of standard potassium solution (K.2-1) to 100 ml with distilled water in different measuring flasks. Each flask now contains 0.01 g, 0.02 g, 0.04 g, 0.06 g, and 0.08 g of potassium chloride per 100 ml. l3 K.2.3 Sample Solution Dissolve approximately 10 g of the dried sample (see Appendix C) in minimum quantity of distilled water and dilute to 100 ml in a measuring flask with distilled water. K.3 Procedure Adjust the galvanometer to read zero by distilled water and 100 by standard potassium (K-2-1). Spray various diluted solutions (K-2-2) and obtain the corresponding galvanometer reading. Plot the concentrations against galvanometer reading. Draw a smooth curve over the points which give a calibration curve in the range of 0.01 g of potassium chloride per 100 ml to 0.1 g of potassium chloride per 100 ml. After washing with distilled water, spray the sample solution (K-2-3) and obtain the galvanometer reading. From the graph, read out the corresponding concentration of potassium chloride in the solution. K.4 Calculation mi Potassium, as K, per cent by mass = 52.4 - m2 Where, m 1 = mass, in g, of potassium chloride in the sample solution; and m2 = mass, in g, of the dried sample taken for the test. c) ~t5~t5 ~ t5 ~ " "" mnmnmMittn~it3rurnnmn~9n ttnintiJt3JY!il 1 • Calculation of matter soluble in water other than sodium chloride Matter soluble in water, other than sodium chloride, per cent by mass = 100 - (m1+ m1) where, m 1 = matter insoluble in water, calculation as in D-2; and m 2 = sodium chloride content; calculated as in E-3. mtn'11lniimt3 I W Determination of Iodine M.1 Reagents and materi als M.1.1 Methyl orange indicator solution Dissolve 0.01 g of methyl orange in water and dilute to 100 ml. M.1.2 Phosphoric acid, analytical reagent grade, approximately 85 per cent (m/V) solution. M.1.3 Bromine water, saturated aqueous solution Determine the approximate concentration (milligram of bromine per milliliter) by adding from a burette a measured volume to a flask containing 5 ml of 10 per cent (mN) solution of potassium iodide and 5 ml of dilute sulfuric acid and titrating the liberated iodine with 0. 1 mol/l solution of sodium thiosu lfate. One milliliter of 0.2 mol/l solution of sodium thiosulfate is equivalent to 8 mg of bromine or 12.7 mg of iodine. M.1.4 Salicylic acid M.1.5 Potassium iodide M.1.6 Sodium thiosulfate, standard volumetric solution, c(Na2S203) = 0.005 mol/l. Prepare 0.1 mol/l solution by dissolving 25 g of analytical reagent grade sodium thiosulfate in 1OOO ml water. Dilute 50 ml of this solution to l OOO ml. NOTE: Sodium thiosulfate solution should be standardized. M.1.7 Starch solution, freshly prepared 1 percent (mN) solution. M.1.8 Sodium chloride analytical reagent. M.1.9 Potassium iodate. M. l . l 0 Sulfuric acid, approximately 1 mol/l. M.2 Quantitative tests for iodate and iodine M.2.1 Procedure M.2.2 Transfer about 2 g of salt to a test tube and dissolve in 10 ml distilled water. M.2.3 Add about 1 ml of 10 percent Kl solution and 2 ml of 1 M sulphuric acid and few ml of starch solution. M.2.4 If iodate is present the solution will turn blue due to the liberation of iodine. M.2.5 Estimate the amount of iodate as given in procedure M-3. M .2.6 If there is no blue colour, there is no iodate in the salt. The salt may have iodide or may not be iodized. M.2.7 To check for the presence of iodide. M.2.8 Transfer about 2 g of salt to a test tube and dissolve in 10 ml distilled water M.2.9 Add about 1 ml of 10 percent KI0 3 solution, 2 ml sulphuric acid and few mJ of starch solution. M.2.10 If iodide is present, the solution turns blue due to the liberation of iodine. M .2.11 Estimate the amount of iodide as given in Procedure M-4. M.2.12 If there is no blue colour, there is no iodide in the salt. The salt may have iodate or may not be iodized. M.2.13 If there is no blue colour by both tests, then the salt does not have iodide or iodate. 1'0TE : These qualitative tests must be carried before an opinion is expressed. M.3 Procedure (If iodine is added as IODATE) M.3.1 Weigh 10 g of salt accurately and dissolve in 100 ml of distilled water in a 250 ml conical flask which can be stoppered. M.3.2 Add 2 ml of 1 mol/l sulfuric acid to solution. Add 5 ml l 0% (mN) potassium iodide and stopper immediately. Shake it well and keep in dark for 5 minutes. M.3.3 Titrate this solution with a standard sodium thiosulfate solution 0.005 mol/l, to a light straw colour and add 2 ml of 1 per cent starch solution and continue titration to colourless end point. M.3 .4 Carry-out a black test using 10 g of analytical grade solution chloride. 15 M.4 Procedure ( If iodine is added as IODIDE) M.4.1 Weigh 10 g of salt accurately and dissolve in 100 ml of distilJed water into a 250 ml conical flask, which can be stoppered. Neutralize to methyl orange indicator (M-1-1) with phosphoric acid (M-1-2) and add 1 ml in excess. M.4.2 Add excess bromine water (M-1 -3) to give approximately 20 mg to 25 mg bromine and boil the solution gently until colourless and then for 5 minutes more. Add a few crystals of salicylic acid (M-1-40 and cool the solution to room temperature. Add 1 ml of phosphoric acid (M-1-2) and approximately 0.5 g of potassium iodide (M-1-3) and titrate the liberated (M-1-7) near the end of titration. Carry out a black detennination on reagent and make one or more. Control determinations, using l 00 ml of sodium chloride solution (M-1-8). M.5 Calculation . I nfl,. 21150(v; -V2 )xC Iodme as , m 8 .<g = m where, V 1 = volume in ml of standard sodium thiosulfate solution for the sample. V2 = volume in ml of standard sodium thiosulfate solution required for blank detenn.ination. C = concentration in mol/l of the sodium thiosulfate solution. m = mass in g of the sample taken (dry basis) . nufmnnpH Determination of pH N.1 Procedure Weigh, to the nearest 0.1 g,20 g of the dried sample (see Appendix C) and dissolve in 100 ml of distilled water. Measure the pH of the solution at 27 ± 2 °C using a standard pH meter.