Table Of Contentइंटरनेट मानक
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IS 15837 (2009): Anhydrous Diboron Trioxide [CHD 30:
Nuclear Materials]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee””
“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
IS 15837 : 2009
'J-TTW"lJ 1fT;:rC/J
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-
Indian Standard
ANHYDROUS DIBORON TRIOXIDE - SPECIFICATION
ICS 27.120.1O;71.060J)I
© SIS 2009
B UREA U OF I NDIAN STANDARDS
MANAK BHAVAN,9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
Price Group 3
lilly 2009
Nuclear Matcriuls Sectional Commiuce. CliO 30
\ ..- :
r:~:
f'(lREWORIJ
Thi-,Indian Standard was adopted by the Bureau of Indian Standards.after the draft finalized by the Nuclear
Matcrinls Sectional Cornmiucc had been approved by the Chemical Division Council.
Boron compounds arc used for controlling the rate of nuclear reactions in the nuclear reactors and thus play
a \~r")' crucial role in reactor control. The material must therefore meet criteria like isotopic composition,
impuriry content.
There i~ no ISO Standardon the subject.This standard is formulated based on the indigenous manufacturers'
data/practice-, prevalent in the field in India.
The compoxition of the Committee responsible for formulation of this standard is given in Annex G.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final
value obxcrvcd or calculated, expressing the result of a test or analysis, shall be rounded off in accordance
with IS 2 : Jl)()() 'Rules for rounding off numerical values (reviseds>. The number of significant places
retained in the rounded off value should be the same as that of the specified value in this standard.
IS 15837 : 2009
Indian Standard
ANHYDROUS DIBORON TRIOXIDE - SPECIFICATION
1 SCOPE 3 TERMINOLOGY
This standard prescribes the requirements and the
For the purpose of this standard. the following
methods oftests for Diboron Trioxide (13:0,) used in
definitions shall apply.
nuclear reactors,
3.1 Nuclear Reactor - A device in which a self
2 REFERENCES
sustaining nuclear fixsion chain reaction can he
The standards listed below contain provisions which maintained and controlled (fi~sion reactor).
through reference in this text.constitute provisionsof
this standard. At the time of publication. the editions 3.2 Reactor Contrnl - The intentional variations
indicated were valid. All standards are subject to of the reaction rate in a nuclear reactor obtained by
revisions and parties to agreements based on this adjustment 01 reactivity to achieve or maintain a
standard arc encouraged to investigate the possibility desired state of operation.
ofapplying the most recent editions of the standards
indicated below.
~ REQUIREMENTS
ISNo. Tille
4.1 Description
8883 Methods ofsampling chemical and
The material shallhe in the form offine free flowing
chemical products:
dry white powder, free from odour. dirt, foreign
(Pan I) : ::!005 General requirements and
matter and visible impurities.
precautions (first revision)
(Pan 2/Sec I): Sampling equipment. Section I For ~.2 Chemical Requirements
!97X solids
10614 : 1983 Method for atomic absorption ~.2.1 The material shall conform to the isotopic
spectrophotometric determination content of natural boron that is lOB shall be
of sodium and potassium 19.9±0.3 atom percent and IIB shall be 80.I ±0.3
12046 : 1987 Method for determination of atom percent when tested inaccordance with method
manganese by atomic absorption given in Annex A.
spectrophotometry
12491 1988 Method of determination of 4.2.2 The material shall also conform to the
magnesium by atomic absorption requirements prescribed in Table I when tested in
spectrophotometry accordance with methods referred in col 5 of
13320 : 1992 Determination of iron by atomic Table I.
absorption spectrophotometry -
Test method
Table 1 Requirements for Dlboron Trioxide
51 No. Characteristic Requirement Method or Test. Rer to
IS No. Annex
(I) (3) (4) (5)
i) Diboron Trioxide (as B,O,) percent by mass. Min 99 B
ii) Chloride (as CI) percent by mass. Mux 0.002 C
iii) Sodium (as No) percent by mass. Max 0.003 IS 10614
iv) Iron (as Fe) percent by mass. Max 0,005 IS 13320
v) Calcium (as Cal percent by mass, Max 0.002 D
vi) Magnesium (as Mg) percent by mass. Max 0.005 IS 12491
vii) Heavy metals (as Pb) percent by mass. Max 0.002 E
viii) Cobalt (as CO) percent by mass. Max 0.0005 F
ix) Manganese (as Mn) percent by mass. Max 0.0006 IS 12046
IS 15837 : 2009
5 PACKING AND MARKIN(; granted to manufacturers or producers Illay be
obtained from the Bureau of Indian Standards.
5.1 PackinK
6 SAMPLING AND CRITERIA FOR
Unless otherwise agreed to between ihe purchaser
CONFORl\llTY
and the supplier. the powder shall be packed in
suitable containers such as HOPE bottles and sealed 6.1 The sumples shall be collected according 10 the
under moisture proof conditions. method prescribed in IS XXX3 (Part I) and with the
help ofthe equipment prescribed in IS XXX3 (Part 21
5.2 MarkinK
Sec I).
5.2.1 The containers shall be securely closed and
6.2 Criteria for Conformity
bear legibly and indelibly the following particulars:
6.2.1 Sampling plans to meet acceptance criteria
a) Name ofthe material.
and inspection and measurement procedures that
b) Minimum assay and maximum impurity
describe the method of compliance with this
concentration.
standard shall be established by the seller and
c) Gross and net mass. submitted to the buyer for approval.
d) Date of manufacture and batch number. and
6.2.2 Each sample taken shall be sufficient to
c) Naiucofthe manufacturerand his recognised perform the following in the event they are necessary
trade-mark. ifany. or desired by the buyer:
5.2.2 IUS Cerrificution Marking
a) Quality verification tests by the seller.
The product may also be marked with the Standard b) Acceptance tests by the buyer,
Mark. c) Referee tests in the event these become
necessary. and
5.2.2.1 The usc of the Standard Mark is governed
by the provisions ofBureau ofIndian StandardsAct. d) Retention of archive samples by the seller.
19Xo and the Rules and Regulations made 6.3 Archive samples shall be retained by the seller
thereunder. The details of conditions under which for a period of time specified by the buyer and
the licence for the use ofthe Standard Mark may be delivered to the buyer upon request.
ANNEX A
(Clause 4.2.1)
THERMAL IONIZATION MASS SPECTROMETRICMETHOD FORTilE
DETERMINATIONOFTHE ISOTOPICCONTENTOFnORON
A-I APPARATUS is evaporated under infra-red lamp to get sodium
tetraborate. The residue is redissolved in
A-1.1 Thermal Ionization Mas.s. Spectrometer
demineralized water and concentrated into a tiny
drop. Using a capillary this drop is carefully loaded
:\-2 REAGENTS on adegassed rhenium/tantalum filament. Passabout
O.IlA current through the filament to dry the sample
A-2.1 Demlncralized Water
on the filament. Then momentarily increase the
filament current to about 1.6A to dull red heat. The
A-2.2 Sodium Carbonate
loaded filament is taken into the ion source of the
thermal ionization mass spectrometer.
A-3 PROCEDURE
:\-3.2 After the pressure in the mass spectrometer
A-3.1 Dissolve 3.23 rug of B~O; in boron-free becomes less than 10'"rnb,the filament iselectrically
demineralized water.Warm if necessary. Dilute toget heated slowly to about 0.8 to 1.2A (700'C- 900'C).
it concentration of I ppm of boron. Two ml of this Thermal ionization of the sample results in the
solution (containing about 2 Ilg ofB) is treated with formation of Na.,BO,· ions and after optimising the
a known amount of sodium carbonate to maintain focusing and otheranalysis parameters, the Na,BO,
atom ratio of B: Na equal to I:I.The treated sample molecular ions at m/z 88 and 89 corresponding t"o
2
IS 15837 : 2009
lOB" and B" are mass unalysed by the magnetic'
!I
analyserofthe mass spectrometer,The ion intensities
R ::: measured atom ratio of J!lB/IIB
are measured by a suitabledetector(FaraduyCupor
electron mulriplier or Daly scintillutiou detector). at percent of IIIB::: ---B.- x llJ()
The ratio of the ion intensities give-,the atom ratio I+R
of '''B/I'B. From this isotopic composition can be at percent of "13::: _1_ x (00
calculated. I+R
:\'OTE - \\\'11 Irall1l'l! pcrsouncl all' Il'LlUIIl..'J It\( 111.1"
A·4 CALCULATION
'Pl"\,:llllJllL'lri..: an.IIY~I'. ~'a" JI...cruninauon duriu!! 1111:
IlIB 1,'.uurvc ..If an;l!y"l.\. if ;111) should 1,1." ;1~"'l'(I:Jillt"d :tIIJ
R= appropflJh." ,:,urrCI,:ltoli I";h..:h)r... dl.".h','rmllh.'J h~ '1II.1I~"I"
liB •.\oloph.: rerercncc m;l1l'riab..
ANNEX B
lTable I, Sl No. (i)I
TEST FORPURITY OF 8 0
: .\
B-1 REAGENTS 8-2 PROCEDURE
B-1.1 Mannitol orSorbitol - Neutral.The reagent Weigh accurately about 2 g ofthe dried materialand
shall satisfy the test given in B-1.1.1. dissolve itinabout 120 ml ofwater by slight heating
if required. Add about 15 g of mannitol or sorbitol
B-I.1.1 Five g of mannitol/sorbitol dissolved in
and 0.4 1111 ofphenolphthalein.Titrate with standard
50 ml of carbondioxide free water shall require for
sodium hydroxide solution to a distinct pink colour.
neutralization not more than 0.3 ml of 0.02 N
sodium hydroxide solution using phenolphthalein 8-3 CALCULATION
as indicator. 3AIlI x V
8;01'percent by mass ::: M
8-1.2 StandardSodiumHydroxideSolution- I N.
where
8-1.3 Phenolphthalein IndicatorSolution \' ::: volume in ml of standard sodium
hydroxide solution used in the titration,
Dissolve 0.1 g of the phenolphthalein in 60 ml of in ml, and
rectified spirit and dilute with water to 100 ml. =
M mass of the dried material taken for the
test, in g.
ANNEX C
[Table 1,SI No. (ii)]
SPECTROPHOTOMETRICDETERMINATIONOFCHLORIDEIN DIBORONTRIOXIDE
C-I PRINCIPLE Add with stirring 500 ml of hot nitric acid. Gently
heat the solution until complete dissolution. Make
A known weight of the sample is heated to I 100"C
the solution to I000 ml.
in a current to steam.The hydrogen chloride formed
is collected in the condensate, and the chloride is C-2.3 Mercuric Thiocyanate Solution, .. percent
determined by spectrophotometry after the addition - Dissolve4gofrecrystallized mercuric thiocyanate
of mercuric thiocyanate and ferric alum. in 100 ml ofethyl alcohol.
C-2 REAGENTS C-3 PROCEDURE
C-2.I Double Distilled Water - Freshly distilled Aknownweightofthe sampleinpowderform istaken
water is used through out the experiment. in a silica reaction tube and is heated to I lOOT . A
constant current of steam is passed over the sample
C-2.2 FerricAlumSolution, 12 percent- Dissolve
for an hour at I 10<J'C. On pyrohydrolysis. hydrogen
120 g offerric alum sail in 430 ml ofboiling water.
3
IS ISlD7 : 2009
chloride is Iormed which is then collected along with Construct a calibration plot between the known
the condensed steam in a collection tube. About S() amount of chloride and the absorbance by taking a
l)() IIII of the condensate is collected. This i, then series of standard samples containing known
concentrated to about20 1111.About 21111eachofferric concentration of chloride in the range I to
alum and mercuricthiocyanate arc added and the total 100 ppmw. The concentration of chloride can then
volume is made uptu 25 nil. The solution is allowed be read from the calibration plot.
to stand for 20 min and then absorbance is measured
at -txo nm against a reagent blank,
ANNEX D
ITahle I. Sl No. (v)J
TESTFOR CALCIUM
1>-1 API'ARATl}S dish.Add 5drops ofhydrochloric acid and evaporate
to dryness.To the residue add 25 rnl ofmethanol and
I>-LI Platinum Dish
5 drops of hydrochloric acid and again evaporate to
dryness. Moist the residue with sulphuric acid and
1>-2 REACENTS
ignite. Dissolve the residue in 50 ml of water. add
1)-2.1 Methanol 10 ml of anunonia-uuuuoniuru chloride buffer
solution. 25 ml uf strong ammonia solution and
D-2.2 Hydruchloric Add 5drops of sodium sulphide solution. Titrate with
EDTA solution lbing methyl thymol blue as
D-2..1SulphuricAdd
indicator uruiI the blue solution become colourless
1)-2.~ Ammonia Solution orgrey.
The amount of calcium present is calculated by the
1>-2.5 Ammonia-Ammonium Chloride Hufrer
formula as given below:
Solution
=-A x-B
1>-2.6 Sodium SulphideSolution Ca. percent by mass x 0.1
1'-1
1>-2.7 F.DTA(lUll 1\1) where
A volume of EDTA required for titration. in
D-2.8 Meth)"1Thymol Blue IndicatorSolution
011;
D-.' I)ROCEDURE /J mass of Ca equivalent 10 I ml of EDTA
solution, in mg: and
Weigh accurately about 5 g of the powdered sample .\I = mass of sample taken for the test. in g.
and dissolve it in 25 1111 of methanol in a platinum
ANNEX E
lTable I, 51No.(viil]
TEST FOR HEAVYMETALS
E-I AI'PARATl'S E-2.3Standard Lead Solution
E-l.l Nessler Cylinders- 50 1111 capacity and Dissolve 0.1831 g of lead acetate [Pb(C~HP~)2"3HPl
:\es~krilcr. in 100 ml of water and clear any cloudiness that
might appear with a few drops of acetic acid. Dilute
E-1 REAGENTS
the solution to I 000 ml. Take 100 ml of this
solution and make it upto I 000 rnl. One m1 of this
E-2.1 Dilute Hydrochloric Acid - Approximately
solution contains 0.01 mg oflead (as Pb).
IN,
E-2.2 Hydrogen Sulphide Solution - Saturated
and freshly prepared.
IS ISHJ7 : 21111'1
E-3 PJ{OCEDU{E cllnll,,1I,'sl IIsing 2 1111Ill'sl:m,brd k:lol ~,"ulilln ;,"d
the ,a111" <j1l;lIlllly "I' rt'a~t:III.' III lhe '/lIn,' Illliil
Dissnlw I.()O() g of B:O, in 25 ml "I Ihll
\olun«, "flh,' re:I<.:linll mixture. ("lIllp:lre Ih,' ,'"Inlll
deminerulizcd water, aJd n.S 1111 of dihlled
III the s,\IUli'1I1~ :illl'l lu min. Inll'n~lly III the (Ilh'ur
hydrochloric acid, heat to liO'C, transkr 10 a !':t'ssla
pr\l,lu(l'd In Ihc' tt'sl solution shall he cuhcr l''1u:d \II
cylinder and add III 1111 of hydrogen sulphide
k" :" ,'dlllp;I,nJ1(\ Ikll in the couuol I"sl <oluuon.
<oluuon. Make up the xolution tu 5011I1.Carryout :1
:\~:\EX F
17;")lt' I. SI.\'o. (\ili)1
()ETI':J{'11;\:\T10~ OFCOBALT I!': I>lBOI{()~ TRIOXIDE
BY ATO:\lIC.\BSOJ{PTlO~ SPECTI{():\lETRY
F-I PRINCIPLE o.S 10 I em di.unetcr and condition \\nh dilutc 11<'1.
Trauxtcr Ihe di'Sllhed mel: Oil 10 the cuhunn ;lIld
-\ known amount of B.O I.' dl,,,)1\,'d III \\;I,h the t'I\IUlIlIl with dixtillcd water. Horou dUles
deruiucrulizcd water, Th« ,:all(\nl,' impuriuc :lnc! dm\n. W:I,h the column with miniuunn IWo bed
boron arc xcpnrutcd l'mplo)ing a strong ;lcid cali"n volumes. Reject the w;lshings. Wash llle COIUIIlII
exchange resin. Cohall hl'lJ up 1111 Ih\' column is with about I() ml of 3 M lIel and collect the
eluted ill dilute HCl. c'onl'\'lllr;Il,'d and introduced washinp ill a fresh vial. It should he mentioned that
into acetylene-air /I;III1C' and the intvuvity of line al the volumes of eluant» given above is oulv
2-W.711111(tllTesponding t" c'ohail is measured. indicative and il may he necessary to oprimisc the
elution Sll'pS during the ion exchange separation
1"-2 :\1'1':\RYITS
procedure. Evaporate the washings collected and
dissolve in distilled water,
F-2.1 .-\tomk Ahxurptiun Spectrometer
Setup the atomic absorprion spectrometer system.
F-J I{EA(;r~NTS Introduce the solution into the air-acetylene flame
and measure the intensity of absorption signal at
F-3.1 AStrongCation Exchange Rcsin (1-1-Form) 240.711111.
Prepare a series of solutions containing known
1"-3.2 Double Distilled Watcr no
amountsofcobalt in I to I I-tg/ml range. Cunstruci
F-4 PROCEDURE a calibration plot by analysing all the standard
solutions. Plot the intensity again!>t the amount of
W~igh out a known amount of 8,0, (100 mg) and cobalt present in the standard solution. The amount
dissolve in demineralized water. Warm ifnecessary. of cobalt in sample solution can he read from the
Set up a strong acid cation exchange resin calibration plot. This can then he converted into
(Ambertitc IR-l~() or cquivulent) 8-10('01 long and concentration,
5
