13
Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. इंटरनेट मानक !ान $ एक न’ भारत का +नम-णSatyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” प0रा1 को छोड न’ 5 तरफJawaharlal Nehru “Step Out From the Old to the New” जान1 का अ+धकार, जी1 का अ+धकारMazdoor Kisan Shakti Sangathan “The Right to Information, The Right to Live” !ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह Bharthari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 3025-60 (2008): Methods of sampling and test (physical and chemical) for water and wastewater, Part 60: Fluoride [CHD 32: Environmental Protection and Waste Management]

IS 3025-60 (2008): Methods of sampling and test (physical and … · 2018-11-14 · IS 3025 (Part 60) : 2001' v 5,6.1 Al('t/lOdIVitholll Distillation 5.6.1.1 The sample shall not

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Page 1: IS 3025-60 (2008): Methods of sampling and test (physical and … · 2018-11-14 · IS 3025 (Part 60) : 2001' v 5,6.1 Al('t/lOdIVitholll Distillation 5.6.1.1 The sample shall not

Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 3025-60 (2008): Methods of sampling and test (physicaland chemical) for water and wastewater, Part 60: Fluoride[CHD 32: Environmental Protection and Waste Management]

Page 2: IS 3025-60 (2008): Methods of sampling and test (physical and … · 2018-11-14 · IS 3025 (Part 60) : 2001' v 5,6.1 Al('t/lOdIVitholll Distillation 5.6.1.1 The sample shall not
Page 3: IS 3025-60 (2008): Methods of sampling and test (physical and … · 2018-11-14 · IS 3025 (Part 60) : 2001' v 5,6.1 Al('t/lOdIVitholll Distillation 5.6.1.1 The sample shall not
Page 4: IS 3025-60 (2008): Methods of sampling and test (physical and … · 2018-11-14 · IS 3025 (Part 60) : 2001' v 5,6.1 Al('t/lOdIVitholll Distillation 5.6.1.1 The sample shall not

IS 3025 (Part 60) : 2008

~ ~~~ cfi~ -R-;rr 3lTx ~afUT

(lfTm ~~) c#r~

( q$ MI :r=rfte-rur )

Indian Standard

METHODS OF SAMPLING AND TEST (PHYSICAL ANDCHEMICAL) FOR WATER AND WASTEWATER

PART 60 FLUORIDE

( First Revision )

ICS 13.060.50

© BIS 2008

BUREAU OF INDIAN STANDARDS~tANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

April 2008 Price Group 4

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H)REWORD

This Indian Stunda rd I Pan (,0) ( Fi rs' 1<.:\ ,swn l \\ as ad opted hy the Bu reau o f Indian St.mdards, utte r the draf tfinal ized by the hl\'ironnh:nl Protection and Waste \l anagt:lIlent Se cu un a! Committee had been approved hy theChcmicul Div ision Council.

As per IS 1050(J : It)\) I 'Drink ing \\ atc r - - Spcciricar ion (ji!"St revision )' , the dexirubl c Ii III it and pen n i-v ihie Iim il

(in the absence ofultcrnate sour,'t'l for fluoride in the drinking water is I ,Omg/1. ,\lll .\ and 1,5 IIIg/1. JI11,\ rt: sp"l'lI\t'I~ .

Beyond this level it causes flu orosis ,

The Committee rcvpon siblc for the to rmulation of IS 3025 : 1')64 'Method s o f sampling and te st (phys ical and

chemical) for water used in ind ustry ' had decided to revi se the standard and pub lish it as se pa rate pa rts. This

standard is on,' of the different parts under the IS J0 25 series of standards and supersede 23 o f [S 3025 ,

Electrochemical probe method given in th is standard is prepared based o n the method spec ifi ed in ISO! 0359-1' Wate r qualit y _. Determination o f t'luorulc - - Part I : Ekcl rocht:m ical pr obe method for potable and lightly

pollute water ' , It is rcchnic ull y cqu ivulcnt except that measurement is made without filtrat ion of the solut ionthrough membrane fi lrcr,

The composition of the Commitrcc rcsponstblc for the formulation of this standard is given at Annex A,

In report ing the results of a I,' st or analysis made in accordance with thi s standard , if the final va lue , observed orcalculated, is 10 be rounded o il, it sha ll he done in acco rdance with IS 2 : 1960 ' Rules for rounding off numerical

values (Tn'i ,H'd)' ,

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IS .\025 (I'a rt Mil : 2001'

I'I{/i{['l ~'f{[ll(/{llll

METHODS OF SAMPLING AND TEST (PHYSICAL ANDCHEMICAL) FOR WATER AND WASTEWATER

PART 60 FLUORIDE

( n-« Revision )I SCOPE

1.1 This standard (Pa rt (0 ) pres cr ibe» thre e meth odso f te,t for dct eruunat ion o f flu o ride co utc nt in \1 .ncr

and wastew ater.

Where the sample is highly col oured or turb id or hasinterfering subs tanc es in excess o f the limit s gi venabove, the method with Ji stillat iun (descr ibe dunder 5.6.2 ) sha ll he used o r the sa m ple shall beappropriately diluted before this test. With samples ofunknown composition or where greater accuracy isneeded, the method with distillation shall be employed.

a ) Zircon ium ulizarin mcthod II ithout distillation.

b) Zirconium alizarin method w ith dixtillution .and

c) Elec troche m ica l probe method .

1.2 The method without d istill ation t dc scr ibcdunder 5.6.1 ) and electroch emic al pr obe meth od isrel iable for sa mples of pot able and Iightly pollutedwater in wh ich the interfering substances arc not inexcess of the limits given below:

nu,(il \", ary of term s r~latill ~ 10 water,,~wa ~ ~ and industr ia l effl uent s.Part IGl ossary of term s relating to water., e w ag e and industrial e tflucnt «.Part 2

IS v".7022 t Part II :

I (J7 ,~

7022 (Part 2 ) :1<)7<)

5.3 Interference

The colour (red to yel low with increasing concentrationof fluoride) obtained with zircon ium al izarin reagentis matched against that produced with a series ofsta ndard fluoride solutions .

5.1 Principle

5 ZmC()~Il!1\I ALIZAIUN METHODS

5.2 Range and Applicability

Thi s method is suita b le for estimation of flu orideco nte nt up to 1.0 mg/I of flu or ide as F. The minimumdetection limit of thi s method is 0.05 mg/I flu oride as F

For the purpose o f this standard. defin itions given inIS 70 22 (Pall 1) and IS 7022 (Part 21 ,hall appl y.

3 TERl\lIJ"OLOGY

Sampling and sample preservat ion shall be done a,prescribed in IS ~025 (Part I) .

4 SAMPLING AND PRESERVATION

2 000 mg /I

.100 Illg/l

400 mgll

2 Ill g/I

0 .5 rng/l

5 mg/l

Chlorides (as CI)

Sulphates (as SO~)

Alkalinity (as CaCO ,)

Iron (as Fe)

Aluminium (as AI)

Phosphates (as PO,)

2 REFERENCES

The standards listed below contain provisions whichthrough reference in thi s text con stitute provis ion s ofthi s standard. At the time of publication. the ed ition sindicated were val id. All standards are subject torevi sion and parties to agreement s based on thisstandard are encouraged to investigate the po ssibilityof appl ying the mo st recent ed itions o f the standards:

IS No.265 : 1993266 : 19933025 (Part I) :

1986

TitleHydrochloric ac id tfourtli revision )Sulphuric ac id (Thi rd revision)Method s of sampling and test(physical and chemical) for waterand wa stewater: Part I Sampling(fi rst rel'i Jiofl)

Iron . alkalin ity. phosphates interfere. if present abovethe values given in 1.2 . Interference of free residualchlorine can he removed by adding sodium arsen ite .Alum inium gives neg ative error because o f formationof AI-F complex wh ich withdraws fluor ide from thereaction of zirconium.

5.4 Apparatus

5.4.1 Nessler TIthes, 100 rn! cap acity.

5.4.2 Distiltation Apparatus - The di st illat ionapparatus sha ll co ns ist o f a Claisen flask of 100 mlcapacity. a large fla sk for generating steam and anefficient condenser. The main neck of the Cl aisen fla sksha ll be filled with a two-holed rubber stopper throughwh ich shall pass a thermometer and a glass tube (for

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IS 3025 (Part 60) : 2001'

v

5,6.1 Al('t/lOdIVitholll Distillation

5.6.1.1 The samp le shall not contain free chl orine ; ifnecessary, it shall be dechlorinated with a slight excess

of sodium thiosulphate solution before usc .

5.6.1.2 Take 100 1111 of the dear sample and a series of

dilutions of standard sodium fluoride solution in 100 mlof distilled water in Nessler tubes and add 5 .0 1111 ofthe zirconium alizarin reagent 10each . The sample and

standards shall be at the same temperature to with inl oe 10 2°e. Mix and compare the colours after stand ing

for Ih exactly , Note the volume of standa rd so di um

fluoride solution contained in the tube with which amatch with the sample under test is obtained.

5.6.2 Method with Distillation

5.5.8 Ccmceutratcd Sulphuric Acid - See IS 266.

5.6 Procedure

5.6.2.1 Introduce into the Claisen flask a number offragments of Pyrex glass or glass beads, 0 .2 g of silve r

sulphutc.? 01101' distilled water and IS ml of perchloricacid . Heat the flask until the temperature reaches 120°C

to 125 °C, connect to the steam supply and regulate the

gas and steam so that the distillation proceeds at atemperature of I3re to 1·1O°e. Distil 150 ml in 25 to

35 min and steam out the condenser towards the end

of the distillation . Discard the first distillate. Di stil a

further) SO 1111 and determine the fluorides in it by themethod given in 5.6.1.2. The figure for this blank sha ll

not exceed a.oo I 5 mg and shall be approximatelyconstant for any further 150-ml fraction.

5.6.2.2 Make I SO 1111 of the sample alkaline to

phenolphthalein indicator with sodium hydroxide

solution. add a few drop in excess and concentrate to

20 ml. When cool. transfer quantitatively to the

distillation flask and carefully add 15 ml of

concentrated sulphuric acid. If the amount of chloridein the aliquot exceeds 5 mg. add about 5 mg of silversulphate for each milligram of chlorine. Connect upthe apparatus and distil 150 ml as in 5.6.2.1. Determine

the fluoride content of the total 150 mIDI' distillate asin 5.6.1.2 .

JOOOWFluoride (as F). mg/I = ---

5.7 Calculation

5.7.1 Method without Distillation

,I) Dissolve 0 .3 g of zirconium oxychloride(ZrOCI :.XII :OJ, or 0 .25 g or zirconium

oxynitrute IZrO (NO,) :.21LOj in SO III I ordistilled water. Dis,olvl' D.0 7 g of alizarin

so d iu m monusulphonatc (u li zar in S ) in

another SO ml quantity o f d istillt:d water andadd the latter solution slowly to the zirconiumsolut ion with continuous stirring . The:resulting solution clears on standing for a few

minutes.

h) Oi lute I 12 ml of concentrated hydrochloricacid (.H't' IS 2(5) to 500 ml w ith di stilled

water. Also add 37 011 of concentratedsulphuric acid ( .It'(' IS 266) 10 .lOU III I of

distilled water and then dilute 10500 1111. Mixthe two diluted acids when cool.

c) Dilute the clear zirconium solution prepared

in (u) to I 000 ml with the mixed acid solutionprepared in ( b ), The reagent is at first red. but

w ithin an hour it changes to orange-yellow

and is red for usc. The solution shall be storedin the dark if kept in a refrigerator it is stable

for 2 to 3 months . Whcn 5 011 of this reagentare added to 100 ml of distilled water

containing no fluorides , it soon turns pink.

Fluorides discharge the pink colour of the lakeso that thc so lu tion acquires a more yellow

tint .

co nncct ing wit h t hc sl': ,1111 vu p p ly ). borh the

thermometer and Ihl' rube ex tending almovt 10 thebottom of the flask . The Side neck of the flask shall becluvcd with a rubber stopper and the side ann connectedwith the condenser. Steam shall he gl'llI:rall:d fromW'II.:r made alkaline with sodium hydroxide. Localoverheating of the C'Iaivcu flavk shall he avoided byusc of an ash':slos hoard with a hold which shall fitclosely to th.: lower surface of thv flu-k .

5.5 ,1 Sodium Thiosulpluuc Solllli"l1 --- apprux iuiarc ly0 .1 N.

5.5 Reagents

5.5.2 Standard Sodium Fluoride Solution - Diwolvc

0 .221 g of dry sodium fluoride in distilled water andmake up to I 000 111 1. Dilute I 000 ml of the solution1O I 000 1111. One millilirrc of this diluted solutioncontains 0 .0 I mg of fluoride (as F) . The solut ion sh all

he kepI in polyethylene or wax -lined gla" buttlcv.

5.5 .•\ Zirconium ..\Ii~(/ rill Rrugcnt

5.5'" Silver Sulphate

5.5.5 Perchloric Acid - 60 percent.

5.5.6 Phenolphthulcin Indicator

5.5.7 Sodium Hydroxide Solution - 10 percent wA.

where

\V = weight of fluorides (as F) in the standardsolution matched by the sample. in rng; and

V = volume of the sample taken for the test

in 5.6.1.2; in 011.

2

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IS 3025 (Part 601: 2008

5.7.2 Met/wei with Distillation 6... Apparatus

6 ELECTROCHEMICAL PROBE METHOD

6.1 Range and Applicability

W = weight of fluorides (as F) in the standardso lu t io n marched hy 150 ml o f thedistillate. in mg: and

V volume of the sample taken for the test in5.6.1.2 . in ml.

The electrochemical technique method is directlysuitable for measuring fluoride concentration s from0.2 mg/l to 2.0 gIl. After the addition of a knownamount of fluoride. concentrations as low as 0 .02 mglI can be detected (see 7.3 ). The method is not suitablefor waste waters and industrial effluents.

6A.4 Measuring Cells - capacity 100 ml, made ofpolypropylene and lilted with a thermostated jacket.

6.4.5 ~Vcl1a Bath - capab le of supplying water to thejacket of the measuring cell (set' 6.4.4) at a temperatureof 25 °C :t O.2°C.

6A.3 Reference Electrode

Either a calomel electrode . filled with saturatedpot assium chloride (Ke l) solution. or a silver/silverchloride electrode shall be used .

6 .... 1 Milli vol: Mcu:« - A 1111111\lIlt meter with animpedance of not les s than Io' ~n . ca pable of resolvingpotential d ifferences of 0 .1 m V or better.

6.... 2 Fluoride lon- selcctiv« Electrode -- The e.m.t.response, lIsing standard solutions. shall not be lessthan 55 m V per decude change in fluor i deconcentration at ~5 cC.

!'OTl : -- Sin g le jun cti o n. xlceve -rype e lec trode s " hic h reducethe liquid -liqu id ju nc tion potent ial are preferable .

I 000 It'

IIFluor ide (as F). mg/l =

where

6.2 Interferences

The electrode will respond directly to hydrox ide ions.The formation of HF under acid ic conditions will re­duce the measured fluoride concentration. Therefore,buffer all test aliquots to a pH between 5 and 7 toprevent such interference. Cations such as calcium.magnesium, iron and aluminium form complexes withfluoride or precipitates to which the electrode does notrespond. Therefore the buffer solution also containstrans-I,2-diaminocydohexane-N,N.N' ,N ' -tetraaceticacid (CDTA) as a decomplexing agent to free boundfluoride . The boron tetrafluoride anion, is notdecomplexed by the addition of buffer.

6,3 Principle

When a fluoride ion-selective electrode comes intocontact with an aqueous solution containing fluorideions, a potential difference develops between themeasuring electrode and the reference electrode. Thevalue of this potential difference is proportional to thelogarithm of the value of the fluoride ion activity inaccordance with the Nemst equation.

NOTES

1 Temperature and ion ic strength may influence the potentialdifference . Accord ingly. the se parameters shall be the sameduring calibrat ion and measurement and shall be kept constantthroughout the procedure.

2 The activity of the fluoride ions is also pH-<lependant. Valuesof pH between 5 and 7 have proved favourable for measurement.Special buffer solutions are used to fix the pH and the activitycoefficient. On these assumptions. this method will no longerrefer to activities. but to fluor ide ion concentra tions. Fluorideion-selective electrodes operate bet .... een 0.2 mg/I and 2000mgll. and show a linear relationship between the potent ial andthe logarithm of the numerical value of the fluoride activity.

6.4.6 Magnetic Stirrer, with a polytetrafluoroethylene(P'TFlij-coated s tirring har.

6.4.7 Polyethylene Beaker, of capacity 100 ml.

6.5 Reagents

6.5.0 Purity of the Reagents - Unless specifi edotherwise. only purc chemicals and fluoride freedistilled water shall be used in tests.

NOTE - 'Pure chemicals sh3J1 mean chemicals Ihal do nOIcontain impurities .... hich affect the resu lt of analysiv,

6.5,1 Sodium Hydroxide 5 (M) - Di ssolve cautiously100 ± 0 .5 g of sodium hydroxide in water, cool anddilute to 500 ml.

6.5 .2 Total Ionic Strength Adjustment Buffer(T1SAB) - Add 58 g of sodium chloride (NaCl) and57 ml of glacial acetic acid [p(CH3COOH) = 1.05 g/rnl]to 500 ml of water in a 1 litre beaker. Stir untildissolved . Add ISO ml of the sodi um hydrox idesolution (6.5.1) and 4 g of CDTA (trans-I.2­diaminocyclohexane-N,N,N' .N 'tetraacetic acid ).Continue stirring until all the solids have dissolved andadjust the solution to pH 5.2 with sod ium hydroxidesolution using a pH meter. Transfer to a I 000 ml one­mark volumetric flask. make up to the mark with waterand mix .

NOTES

1 The solution is stable for about 6 month s. but do not U'C it. I f

a precipitate forms .

2 Th is solution is commerciall y available .

6.5.3 Fluoride, Stock Solution, I 000 mgll

Dry a portion of sodium fluoride (NaFJ at 150 GC for

3

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IS 3025 (Part 60) : 200M

4 h and coo l in a desiccator. Dissolve 2.2 10 :t 0.00 I gof the dried material in water contai ned in a I 000 mlone-mark volumetric flask, Make up to the mark withwater and mix. Store the so lution in a screw-cappedpolyethylene container.

6 .5.3.1 Fluoride, working standard solution I, 10mgll

Pipette 10 ml of the fluoride stoc k solution (see 6.5.3)into a I 000 mione-mark volumetric tlask . Make upto the mark with water and mix . All standard solutionsshould be stored in plastic bottles and arc usable forone month.

6.5.3.2 Fluoride, working standard solution II, 5 mgll

Pipette 5 ml of the fluoride stoc k solution (s t' t' 6.5.3)into a I 000 mione-mark vo lumetric flask and makeup to the mark with water.

6.5.3.3 Fluoride. working standard solution III. I mg/1

Pipette 100 ml of the working standard solution I(see 6.5.3.1 ) into a I 000 mione-mark volumetric flaskand make up to the mark with water,

6.5.3.4 Fluoride, working standard solution IV, 0.5 mgll

Pipette 100 ml of the working standard solution "(see 6.5.3.2) into a I 000 mi one-mark volumetric flaskand make up to the mark with water.

6.5.3.5 Fluoride. working standard solution V, 0.2 mgt I

Pipette 20 rnl of the working standa rd solution I(see 6.5.3.1) into a I {)()() ml one-rnark volumetric flaskand make up to the mark with water.

7 PROCEDURE

7.1 Preparation for Measurement

Since the electrode characteristics of a fluor ide ionse lec tive electrode generally vary with time, checkthe calibration curve on the day of use . To acceleratethe establishment of the equilibrium potential,condition the electrode pr ior to mea surement in thefollowing way . Prior to measurement. immerse theelectrode for I h in the cell (see 6.4.4) which containsthe reference solution 5 (see Table I). After rinsingwith the first solution to be measured, the electrodeis ready for use.

7.2 Measurement

Pipette 25 ml of the buffer solution (see 6.5.2). followedby 25 ml of the water sample. into a measuring cell(see 6.4.4). Ensure that the pH is 5.2 ± 0.2; if necessary,adjust the pH w ith hydrochloric acid or sod iumhydrox ide solution. using as little as possible.

NOT E - If a prec ip itate is fo rme d . perform the analvsis witha d iluted sample . An y d ilut ion of the sample should 'be takeninro account J ur ing the ca lc ula tio n or the result s.

4

For a series of determinations. start the measurementwith the lowest concentration and finis h with thehighest following the anticipated concentration of thesamples. After measuring the high concentrations,recondition the electrode before measuring the lowconcentrations (see 7.1). Measure all the solutionsaccording to the following procedure. Wait untilconstant temperature (for example 25 ± 0.5°C) isreached and carry out all the measurements at thistemperature. Put a stirring bar into the mea sur ing cell(see 6.4.4) and place it on the magnetic s tirrer« see 6.4.6) . Insert the electrodes (see 6.4.2) into thesolution and fix them in place. Adjust the stirring rateto about 180 mini I to 200 min/I. When the potentialdoes not change by more than 0.5 m V in 5 min , switchoff the stirrer. After at least 15 s, record the valueobtained. Rinse the stirr ing bar and the electrodes withthe next solution to be mea sured. before starting thenext measurement.

7.3 Measurement After ConcentrationEnhancement

If a water sample contains less than 0.2 mgll F, proceedas follows:

Add 500 ml of the fluoride standard solution I(see 6.5.3.1) to 25 ml of the sample using a pistonpipette, and 25 ml of the buffer solution (see 5.4 .2)with a volumetric pipette; continue as described in 7.2.When calculating the result, subtract the amount offluoride ions added from the total result.

7.4 Calibration

Establish a calibration function using the five refer­ence solutions in the corresponding concentrationrange. For the range 0 .2 mgll to 10 rng/l, proceed asfollow s:

a) Pipette 25.0 ml of the buffer solution(see 5.4.2) into each of five measuring cells(see 6.4.4), and

b) Pipette the respective volumes of the workingstandard fluoride solutions specified in TableI into the measuring flasks.

For the establishment of the calibration function pro ­ceed step by step from the most dilute solution to themost concentrated solution, rinsing after eachmea surement with the solution of the next highestconcentration. After the above measurements have beencompleted. recondition the electrode for 5 min to 10min, using the reference solution 5 (see Table 1) inorder to eliminate memory effects.

8 CALCULATION AND EXPRESSION OFRESULTS

Plot the calibration values on semi-logarithmic paper.

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IS 3025 (Part 60) : 200S

Table 1 Preparation of Reference Solutions

(Clauses 7.1 and 7.4)

SI No. Reference Solution Buffer Solution Working Standnd SolutionNo. r

A

"'ml No. ml(I) (2) (3) (4) (5)

i) I 25 I 25ii) 2 25 II 25iii) 3 25 III 25iv) 4 25 IV 25v) 5 25 V 25

FluorideConcentntion

rng/l(6)

1051

0502

Use the following order of measurement (the numbers refer to the reference soluuons m thIS Table):

5 - rinse - 4 - rinse - 3 - rinse - 2 - rinse - I - rinse with 5 - recondition - repeat measurmg run.

If the individual values of the parallel series vary from the first series by more than I :l: 0.5 mV, repeat the measuring run Regularchecking of the calibration graph is essential. Ensure that the slope IS not less than 55 mV, otherwise check the equipment and establisha new calibration graph.

NOTES

1 The term 'Concentration' refers to the concentration of the working standard solutions and the sample solution but not to theconcentration of the measuring solutions after addition of the buffer.

2 See 6.5.3.1 to 6.5.3.5.

with the fluoride concentrations, in milligrams per li­tre, on the abscissa and the cell potential, in millivolts,on the ordinate and establish the regression line. Readthe value for the samples by using the regression lineand express the mass concentration of fluoride inmilligrams per litre.

NOTE - The evaluation may also be calculated using theNernst equation.

9 PRECISION

An inter-laboratory trial, carried out in Germany in1982, gave the results shown in Table 2.

Table 2 Precision Data

SI p x WFR a. Ve,

No. Sample a. vc,I n

rng/l rng/l % mz/l % mg/1 %

(I) (2) (3) (4) (5) (6) (7) (8) (9) (10) (II)

1 Drinking water 12 48 0.275 0.283 - 0.021 7.4 0,0068 2.42 Drinking water + F" 13 52 2.4 + 0.275 2.596 - 0.103 4.0 0.0395 1.53 Drinking water + F"

+ 15mgAI13 52

5.0 + 0.275 4.340 - 0.110 2.5 0.0559 1.3100 mg Mg500 rng Ca

4 Distilled water + F'+ 100 mg Fe15mgAI II 43 0.6 0.531 88.5 0.024 4.5 0.011 6 2.2

100ml!.Ml!.500 mz Ca

5 Distilled water + F+ 100 rna Fe15ml!.AI 12 48 8.6 6,864 79.8 0.195 2.8 0.0701 1.0

100ml!.Ml!.500 ma Ca

6 Same as 5 + F 12 48 60.6 46.351 76.5 1.560 3.4 0.6433 1.4

nprWFR

number of laboratoriesnumber of valuesmass concentrationmean valuerecovery rate

0,

vc,0.VCR

5

repeatability standard deviationrepeatability variation coefficientreproducibility standard deviationreproducibility variation coefficient

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IS 3025 (Parl60) : 2008

ANNEX A

(Foreword)

COl\lMlrrEE COMPOSITION

Environment Protection and Waste Management Sectional Committee, CHD 32

( Jr~{"" :'l/tum

In personal .:apaCIl) (-lOIN . C. R. l'ark , Nr ... Drlhl / /()U/Y )

Bhabha Atomic Res c arch C e nIre , Murnbai

Hharat Heavy Electrrcalv Limited , lIardwar

CeIllcnt Manufacturcr-; ' As"",iali un, New Delh i

Central Fuel Research Institute . Dhanbad

Centra l Lcath er Research lnvriture, Chennai

Central Pollur ion Coruro! 1311ard . New Delhi

Crop Ca re Fedc rat ion o f Ind ia , New Delhi

Indian lnvtitutc of Technology. Department 01 C tvil Engrncenng.

Ncw Delhi

Deihl College III' En~ine,·r ing. Delh i

Directorate General , Faelory Advice Service and I.a bour Institute,

Murnhar

Directorate General o f Health Services. New Delhi

Engineers India Limited. New Delhi

Envirotech Instruments Private Limited . New Delhi

Feder..tion of Indian Chambers of Commerce & Industry (FlCCn,

New Delhi

(Iujar ..t Pollution Control Board, Ahmedabad

Hindu-tan Lever Limned. Mumbai

Indian Chemical Manufacturers " A ssociation. Mumbai

Indian Council of Agricultural Rcse.. rc h, New Delhi

Indian Counc il of Medical Research, New Delhi

Indian Oil Corporation Limited. Faridahad

II'C1.. Vadodara

Industrial Toxicology Research Centre . Lucknow

M iniSIrY of Defencce (R & D\, DRDO, New Delh i

~lini slry of Environment and Forests , New Delhi

Min istry of Non -conventional En ergy Sources, Sew' Delhi

Municipal Corporation of Greater :-.Iumb .. i, Mumbai

6

PRlI> Dn.u- Brsw...s (Chairman )

DR (Sllk'MMIl G. G. P....~,lITDR I. V. S .o\RAlJlli (Alternate)

DR N. C; SIlRI\'ASTA'...

DR L C. R...M

DR S. R....J...M ...N.

DR S. D. M ...~IlUANI

DR C. S . SIlARM ... (Alternate /)DR S. K. TYAG' (Alternate II)

SIlRI A . K . (;IlOSE

SHRI R . P. SHARMA (Alternate )

SIIR' P . N. PARS'ESHAW...RAN

DR M VKESIl KHARE

DR ATlJl MITIAl (Alternate I)

DR ARVINIl NEMA (Altemate II)

DR RAKESII MEIiRafRA

SHRI V. K. MINOCHA (Alternate I)

DR ( S IIRIM...rt) A . MANOAl (Alternate II)

SIfRI S . S . GA" T"'M

SHR' BR U M OHAN (Alte rnate)

DR ( S IIRIMATI) MAllft UR' SIlARM ...

SHRI B. B. LA!.

SIlRI SUSHEEL SAOH (Alternate s

SHRI RAKESH A G.... RW...1.

DR R....JENORA PRAsA n (Alternate )

Ms ANT .... RA Roy

SIlR' D . C. DAVE

SHRI B. B . DA'E

SHRI Arnrv... JHAVAR (Allernate)

SHRI V. N. DA S

SHRI A. A. PANJWANI (Altemate)

DR R. C. MAHESHWARI

DR H. N. SAIYAD

DR M . P. S'NGH

SHRI ASIT...M DESAI

SIlRI MnuR BANERJI (Alternate)

DR S. K. BH'RG"'VA

SIIRI 1. C. KAPOOR

REPRE SENTATIVE

SIIRI \'INOO K UM.'R JAIN

DEPl:TY Crrv ENGINEER Crvu, (ENVT)

DEPFIT EXECUTIVE EN GINEER (Alternate)

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IS J015 (Part 60) : lOO!!

()rgulli:.arioll

:-;,,"on ..1 Insu iut e u f Occ upat ion al Health I IC~I K I , Ahme da bad

Nau o nu] Thermal Power Corpora lion Limite d , ~" w Delhi

~CC Il~t New De lh i

Rel iance lndusrric-, Limned. Mumbai

S hr iram Inst itu te of Industrial Re search . New Del l"

SUS Indi a Lim ite d . Chennai

S tee l Authori ty o f Ind ia Limited , Ne w Del h i

The Energy and Resources Institute . J",' w Del hi

Thapar Cent re for Indust riul Research and Deve lo pment. Patiala

T he Fe rti liz e r A vsoc iat ion o f Ind ia . New Delh i

Tow n & Country Plan nin g O rgan izar ion . M iu istry of Ur ba n

Development . New Dclh i

illS Di rectora te General

D K \ ' KK" " " ~L K I '"

() j.l A . t\ !\Il Jrr,.tlf k Jl I iA ltrr na tr)

D. v I. 1'" ,."() k T"p " :'J"' I)' tA ltr rnutrv

S lU oI l K ( j l ll 'AI

S IIK I M. S, Il, " " " ,,,D. S, :\ 1" 1' ,A llemulel

Dw: E. S t "I)! k"''''''DH l ' K . S ".U" II ' (.-\Ir.' '-' /II1,' 1

S " K' v (i , K , :-.; " K

Dw: J....C I II ...U Kt ' lA W: (A /tr llla /")

SilK' V, ~I , 5"" ,KI

S" KI 1' , U I." IAlra ll u l ,')

COl. R, K, J OII K' (Rtt n)

[). SI','" I'A~ ')l y (Altr rnatrv

DK MAll leSII"AK Roy

[)K S, K , CI1 AKKAIIOKlY (..1/1""" 11'"

Ih . ( S ll k l " .' -JI } B. S \\ ,\\lI ~ ·'IH ,"

I) . 5, 1' ",,) (A lte rna te';

5 11. , K, K, J OAIl " !.K

OK SAs:rO\lt VJI>II YA DIIA. \"oI (A I /ema Il')

O K t. . C. S .J<'ASHH . Scienns ' I" and IkaJ (C UD ,

[Representi ng Directo r Ge ne ral (/;'" 011,, ioll

Member Sec reta rySHR I N , K , pA J

Sc ie ntis t ' E ' (C UD ). BIS

7

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