st{lIndonesian National standard sNl a2-2803-2000

Granular NPK

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National Standardization Agencyffi

Colr tents

sNt 02-2803-2000

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Contents;Preface

12?

45o

78o

ScopeReferenceDe f in i t i on . . . . . . . .

Sampl ing methodTest nrethodTest ar3ceptance requirementMarking requirement .Packag ing . . . .

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Preface

The standard of Cornpact I \ rPK fert i l izer is revis ion of SNI OZ-2803-1gg2,formulated according to government programme for protect ing the consumers.

This standard has been discussed in the technical meet ing and pre-concensus in,-eurabaya on Cctober and discussed in the consensus meet ing on 26 March 1999 inJakarta which at tended by producer 's, research i ; rst i tutes and related departments.

Tl t is standard prepared by Surabaya Research lnst i tute, Ministry of Inclustry andTrade.

Granr / la r NPK

1 Scope

This s tandard cons is t , re ference, def in i t ion ,acceptance, requirement, packaging andfert i l izer.

sNl 02-2803-2000

spec i f ica t ion, sampl ing, tes t method, tes tmark ing requ i rement for granu lar NPK

Reference

The l r , ternat ional Fert i l izer Societv Publ icat ion.Off ic ia l Method and Analysis of The Associat ion of Off ic ia l Analyt ical Chemist,Twelf th ; \OAC Washington, 1975.Technical Requirements for Qual i ty Method and Fert i l izer Effect ively. Soi l andAgrocl imate Research lnst i tute, Agr icul ture Department.

3 Def in i t iongranular NPK fert i l izeris synthet ic fert i l izer in compact form, containing nutr ient component of ni t rogen,phosphate and ca l ium.

Specif icat io n

Tah, le Speci f icat ion of compact NPK

No. Test method

Nitrogen totalPzOsKzOAmount of N, P2O5 of ldWater content

Requirement

m in . 6m in . 6m in . 6

m i n . 3 0max.2

Note : Test i tem 1 to 3 base on dry weight

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5 Samp l ing me thod

sampl ing nre thod sha l l be car r ied out rn accord ing wi th SNI19-0428-1ggg, sarnpt ingmethod for solid tnaterial.

6 Test method

6.1 Tota l n i t rogen

6 .1 .1 P r inc ip leNitrogen in the sample is hydrolyzed by sul fur ic acid to form amnronium sulphatecompound. Nitrate and salvcylate acic j forrned ni t ro sal icylate, then i t is reducted withsod ium th io su lphate to form ammorr iunt . D is t i la te the ammonium compound in a lka l iand put the dist i l late in bar ic acid sol t , t ion. Ti t rate with sul fur ic acid unt i l green changein to p ink

6 . 1 . 2 R e a g e n ta) Sul fur ic acid-sal icylate solut ion 25 grarr sal icylate aci ,J dissolved with 1 l i t re water in

HzSOq.b) Sodium t io su lphate , Na2SrO. , SH2O.c) 1 granr bo; ic ac id d iso lves wi th aqt radest unt i l 100 ml .d) Bor ic ac id .so lu t ion, H2SOa, 0 ,05 N.e) Convray indicator0 0 ,15 gram brom creso l green an j 0 ,10 methy l red d isso lved unt i l 100 ml w i th

ethancl .g) Natr iurn hydroxide solut ion, Na OH 409b.h) Aquadest.

6.1 .3 Apparatusa) Analyt ical balance.b) Measuring f lask 100 ml, S00 ml, 1 l i t re.c) Pippete 25 ml.d) Kyeldahl f lask.e) Desti lation unit.

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f) Thermorneter 3000 C.g) Porcelain mortar for gr inding samole

6.1 .4 Procedurea) weight erccurately 0,5 gram sample, out into Kyedahl f lask.b) Add 25 rnl sul fur ic sal icylate acid, shake t i l l mixtured and let them for one night.c) The next day add 4 gram NazSzO:, 5H20 then heat in the low temperature, t i l l there

no bubble. Increase the temperature gradual ly t i l l 3000 C (for two hours) and let thencool .

d) D i l lu te wi th aquadest , move to meas ' r r ing f lask 5 ml , shake and add the aquadestunt i l l ine mark

e) P ippete 25 ml , p lace in the d is t i la t ion f lask , add wi th 150 ml aquadest and bo i l ingstone.

f) Dist i late af ter adding 10 ml NaOH 400,6 solut ion by col lect ing dist i l late in 20 ml bor icac id 1 % so lu t ion which added 3 drop o f Convyay ind icator .

g) Stop dist i l lat ion process i f d ist i late, reach '100 rnl .h) Ti t rate with HzSOa 0,05 N unt i l the t i t rat ion point is reached (green changed into

p ink) .i ) T i t ra te us ing the b lank sample

6 .1 .5 Ca lcu la t i on

( V l - V z ) x N x 1 4 , 0 0 8 x P x 1 0 0 1 0 0fotal Nitrogen , o/o = x----

100 - KAW

Explanat ion :Vr is HzSOq, use in sample t i t ra t ion, mlVz is volume of, ml HzSOa for blarrk t i t rat ion.N is normality of l- lzSOq14,008 is a tomic weight o f n i t roger rP is d i lu t ionW is sample weight , mgKA is Water content. %

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6,2 Phosphor in s i t r ic acid 2o/o as PzOs.

6.2.1 Pr inr; ip lePzOs content identity with colcrimetric Ottho-phospate dissolved is reacted withamrnonium rnol ibdovanadat perform t t re yel low of complex compound of mol ibdovanadatphosphoric acid. The colour intencity is nreasured at wave length 420 sct 440 mn.

6.2 .2 Reagenta) Citric acid solution, CoHeOz HzO 2o/o.b) Ammonium mol ibdat solut ion (80 g/ l ) = l \4 : B0 gr,

Ammoniunn tetra hydrate (NHo)u MOz, Ozr 4H2O be di luted unt i l 1 l i t re by aquadest.c) Ammonium metha vanadal (4 g/ l ) .= \ t = 4 gram ammonium metaa vanadat, NHcVOg

di luted with 500 ml HClOa, P.a anC di lute unt i l 1 l i t re by aquadest.d) Ammonirrm mcl l ibdovanadat mix 1 voiume of lVl and 1 volume V unt i l homogen. The

mixture i r ; done just before using.e) Standard so lu t ion o f PzOs.Weight accurate ly 0 ,9587 gram of potass ium d ihydrate

phosphate, KHzPOa (which dr ied for 2 hours ln the 1O5o C) and di lute unt i l 1 l i t re byaquadest .

f ) Aquadest

6 .2 .3 Apparatusa) Analyt ical balanceb) Electric dryerc) Mortar porcelain to gr ind the sampled) Screen mesh 80e ) Measur ing f l ask 100 m1 ,50 m l , 1 l i t r e ,0 F lask d iameter 7 cm.g) F i l te r paper Whatman 40.h) Er lenmeyer 500 ml .i ) Gooch p ipet te 5 ml , 50 ml .j ) Measur ing p ipet te 5 ml .k) Spectrophotometer

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6.2.4 Procedurea) Sample preparat ion

Weight accuracy 1 gram gr inding sample (passed mesh B0), put into porcelainmortar, add ci t r ic acid 2 % gradual ly also gr ind cont inual ly. Pour into measuring glass500 ml, c lean the mortar careful iy Di lute with c i t r ic acid 2 % unt i l the l ine mark,shake for 30 minutes. Fi l ter wi th paper Whatrnan 40, put in to the Er lenmeyer.

b) Pipette 5 rnl sample, put into measurir :g f lask 100 nr l .c) Di lute with 50 ml aquadest, add 5 rnl arr tmoniurn mol ibdovanadat then di lute with

aquadest unt i l l ine mark and shake.d) Prepare standard solut ion Pzos 0,5, '10 . 1 , S : 2,0 and 2,5 mg pzOs (pipette each

1 :2 : 3 : 4 and 5 ml by s tandard so lu t ion PzOs 0,5 mg/ml ) , put in to measur ing g lass100 ml then do as sample preparat ion.

e) Ti t rate the blank sample.0 Let the colour of development dur ing 10 minutes, read colour intensi ty with

spectrophotometer at the wave length 420 or 440 mm.g) Make standard curve.h) Calculate PzOs in the sample.

6.2.6 Calcu lat ionC x P

Phosporic dilute citr ic acid 2% as PzOs o/c - - 100 o/oW

Explanat ionC is P2Os content f rom standard curve, mgP is Di lut ion factorW is the weight o f sample , mgWa is Water content, %

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6.3 Potass ium as KzO

6.3.1 Grav imet r ic method

6 .3 .1 .1 P r inc ip lePotassiunt is precipi ta led as potassium cl"r lor ide and determined by gravimetr ic method.

6 .3 .1 .2 Reagen ta) Pec lor ide ac id HClOa, pab) Ethanol 96 %c) Bar ic ch lor ide so lu t ion, BaC12 10 %.d) Phenolphtalein indicatore) Calc ium ox ide, CaO, Pa0 Aquadest

6 .3 .1 .3 Apparatusa) Analyt ical balanceb) Breaker glass 400 mlc) Glass stirrerd) Gooche) Measuring f lask 500 mlf) Volumetr ic pipettegt Electric hs'aterh) Funneli ) Measur ing g lass 10 mlj ) Fi l ter paperk) Porcelain mortarl) Electric dryerm) Exicator

6.3. 1 .4 P ro ced u rea) Weight accurately 5 gram sample, di lute r ,v i th aquadest in the measuring f lask 500 rnl

and shake.b) Add aquadest unt i l l ine mark

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c) P ipet te 1O ml so lu t ion in to beaker g lass,400 nr l , add 15 ml BaClz 10%.d) Bo i led unt i l the sed iment is formed then coo l .e) Add phenolphta le in ind icator and CaO, p .a unt i l a lka ly react ion then heat them.f) Fi l ter and col lect the f i l t rate outprr t in the porcelain dish.g) Add B ml HClO.r P.a .heat thern ur r t i l d ry and whi te snroked appeared.h) Cooled add 5 ml HCIO q 1o/o in the a lcoho l 96%.i) St i r r and gr ind with st i r rer and f i l t rate with gooch which contains of 3 pieces of f i l ter

paper that measured i ts constant lve ight in the 12Oo C.j ) Dr ied the sed iment and gooch a t 120o C.k) Cooled and weight, repeat t i r is wcrk unt i l i ts weight is constant .

6 .3 .1 .5 Ca lcu la t i on

( W r - W r ) x P x 0 , 3 3 9 9 x 1 0 0 1 0 0Potassium as K,O oh = X

100 - KA\\/

Explanat icn :V/ is weight o f sample , gW2 is weight of empty gooch, gW1 is weight gooch + dry sed iment , gP is di lut ion factor0,3399 is chemical factor, KzOKA is water content. %

6.3.2 Spectrophotometr ic method

6.3 .2 .1 Pr inc ip leSoluble potassir rm determinat ion by spectroplrotometr ic method.

6 .3 .2 .2 Reagenta) Perchlorate acid, HClOa, p.ab) Nitrate acid HN03, p.ac) Potassiurn solut ion

Di lu te 25,34 CaClzwi th aquadest unt i l 1 l i t re .

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d) Potassium standard solut ion, rng/ lD i lu te KCI p .a . w i th aquadest as needed

e) Aqu adest

6 .3 .2 .3 Apparatusa) Analyt ical balanceb) Mortar porcelain to gr ind the samplec) Screen 80 meshd) Beake r g lass 100 m le) Measur ing f lask '100 ml , 500 ml , 1 l i t ref) Electr ic heaterg ) F u n n e l O 7 c mh) Paper f i l te r Whatman 40i) Volumetr ic pipette 2 ml, 5 ml, 10 rn,j ) Spectrophotometerk) Atomic absorbt ion spectrophotomcter, ) Lamp of potass ium khatode

6.3 .2 .4 P 'ocedurea) Weight more less 1 gram gr inded sanrp le (Pass o f B0 mesh) , put in to to the beaker

g lass 100 m lb) Add l0 ml HCIOq add 6 ml HNOr p .a . heat unt i l wh i te smoke appeared dur ing

5 minutes.c) Cooled, put in to measur ing f lask 500 nr l , d i lu te wi th aquadest , shake and f i l l un t i l l ine

markd) Fi l ter wi th paper f i l ter Whatman 40 into dry Er lenmevere) P ipet te sample so lu t ion as needed ano put in to measur ing f lask 100 mlf ) Add 5 nr l potass ium so lu t ion, d i lu te wi th aquadest unt i l the mark ar td shakeg) Do the same job for the sample b lankh) Measure the potassium concentrat ion hy atomic absorbt ion spectrophotometer at the

of length of wave 766,5 nm.

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6.3.2.5 Calculat ion

1 0 0C x P x 1 , 2 0 4 6

1 000Pottasium as K2O, o/o =

W

Explanat icn :C is potassium concentrate, mg/lP is d i lu t ion fac tor1 ,2046 is conversion factor KzO to KW is weight o f sample , mg

6.4 Water content

6.4.1 Dest i lat ion rnethod

6 .4 .1 .1 P r inc ip leWater ozeotropic separat ion with orgart ic solvent.

6 .4 .1 .2 Reagen ta) Xylolb) To luene

6 .4 .1 .3 Appara tusa) Analy t ica l ba lanceb) Bo i l ing f lask 500 mlc) Bo i l ing s tonecl) Electric ovene) Aufhauser apparatusf) l /easur ing; f lask, 5O ml

6 .4 .1 .4 P rocedurea) Weight accurately 5 gram sample, uut i r r to boi l ing f lask 500 ml and add 300 ml xylol

and bo i l ing s tone.

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b) Connect with aufhauser and heat at electr ic oven for t hour, star led from boi l ing,then turn of f the electr ic oven and let aufhauser cool .

c) Condensor rv i th xylol or to luene.d) Read the volume of water at aufhauzer apparatus.

6 .4 .1 .5 Calcu la t ion

WWate rcon ten t . oh= - x 10C

V

Explanation .V/ is weight o f sample , gV is volume of water. ml

6 .4 .2 Kar l F ischer method

6.4 .2 .1 Pr inc ip leTo disperse sample into methanol then t i t rate with Karl Fischer reagent which had waterequ iva lent .

6 .4 .2 .2 Reagenta) Kar l Fisher reagenb) Methanol wi th water content, maximun,0,1 o/oc) Aquadest

6 .4 .2 .3 Apparatusa) Analyt ical balanceb) Volumetr ic pipette, 50 mlc) Kar l Fischer t i t rate

6.4 .?- .4 Procedurea) Pipette 50 ml methanol.put into t i t rat ion r lask and t i t rate with Karl Fischer reagent

unt i l the; ye l low co lour changed to red ye l low.

b) Weight O, '1 gram aquadest , pur t i r , to t i t ra l icn f lask , cont inue the t i t ra t ion unt i l t l te endpoin t obta ined ( the co lour change f rcm ye l low to the red orange) .

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c) Calculate t l te water equivalent point f rom Karl Fischer reagent (F), mg water/ml.

Wa

V

Explanat ion :Wa is weight of water, mgV is volume of Kar l Fischer reageni which's needed to t i t rate aquadest, ml

d) Weight accurately 2 - 3 gram sample, put into t i t rat ion f lask and add 50 ml methanol,s t i r unt i l homogen

e) Ti t rate with Karl Fischer Solut ion unt i l end point obtained.

6.4.2.5 C;r lculat ion

V c x FWater content, % = x 1 0 0

W

Explanation :Vc is the volume of Karl Fischer reaction which need to t i trate the sample, mlF is the water equivalent, mg water/nri reactionW is vrelght of sample

7 Test acceptance requ!rcrnent

Produc t shou ld be accep ted when con fo rmed a l l o f qua l i t y spec i f i ca t ion o f g ranu la r NPKfert i l izer.

I Marking reeuirement

a) ProducVtrade nameb) N contentc) KzO contentd) PzOs content

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e) Ne t we igh tf ) Symbolg ) P roducer ' s nameh) The wr i t i ng DO NOT USE A HOOK

9 Packag ing

t The products shal l be packed in c lose packagirrg which doesn' t react wi th the contentand safe Cur ing t ranspor ta t ion and s tcrage.

C

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