UDC 669’3 : 620’199 : 546’491*175-381 ( First Reprint FEBRUARY 01991) IS : 2801-1933
( Reaffirmed 2015 )
Indian Standard
METHOD FOR
MERCUROUS NITRATE TEST FOR COPPER i
AND COPPER ALLOYS
( First Revision )
1. soope- This standard pruscribesthe methodrfor conducting mercurou8 nitrato te8t for wrought
copper and copper base alloy products. lt is an accdsrated test for the purpose8 of detecting
the presence of residual ( internal ) stress that might bring about failure of the material in service
or storage through stress corrosion cracking.
1.1 While this method has also been used for testing assemblies and partial auemblioa, it is not
‘intended for that purpose end 8ome modification may b8 required for such use.
2 TerminaloSlY - For the purpo8e,of this standavtj, tb fctflowing definitions shrll ripply.
2.1 stress Corrosion Crackif@ - Spontaneous failure ‘ib “,metals by cracking under combined
sction of corrosion and stress, residual or applied. 7I
2.2 Residurl Stiess,- StresrrIhat remains within a. boc&& 4.ieruit of plartic deform8tion.
kfd Applied Stress - Stress that is set up 8nd exists in 8 body during application of 8n external
.
3. M8rourour Nit& SWuti&- 0~9 psrcent.
3 1 Concenfretion - The test rokrtlog shalt be -an sq mWWrou8 nitrat solution containing
10 g of mercurous nitrate end lb ml of concl)ntmtd d ( ap gr l-42 ) per lltre of solution.
3.2 Prsprrstion - The solution 8h&i tie pr8p8red by the following proocrdures.
3.21 Pmmdure A - ( HgN08.2H80 ) or 10’7 Q
of meuxttou, titrate mo ml of dlstiiied water acidi-
#ed w&h 10 ml of c er the cryrrtals are completely
dl88olved, dilute the solution with
Nok - The morcuroul nitmte crWtat$ ara the monohydrrtr and dihydratr form end
dould be hendled with oeution boo&r#a ti their When wrlghlne crymto, the weight, of
thr wetor of crystrlliutlon 8huuld b@t8ka intO mercurous nitrate crystals lre photoeon&
tive and whin they have turned yallOw 110 diffic
3.2.2 Procedure B 1 Dissolve 76 g of mercury in 11 ml of dilute nitric acid ( 1 : 1 ). Care-
fully dilute with distilled water to 1 000 ml. This tprovides a concentration of 100 g of nitric
acid after a slight loss due to heating. Add the water in small portions while stirring to prevent
local overdilution. This gradual dilution, together with; the excess acid, will prevent precipitation
of basic salts of mercury. Dilute 100 ml of this solution ( 10 percent ) with 7 ml of concentrated
nitric acid ( sp gr 1.42 ) and 893 ml of water.
Noto - If heating i8 usedin either of the ebovr pfooedureo,the container should b6 covered with we&h
9leu to prevent 108sof nitric acid and water to the atmosphere.
4. Tort Piece
4.1 The length of the test piece shall be at least 150 mm for products of diameter less than- .ar
equal to 76 mm. For products of diameter greater than 75 mm, the length shall be subjaot te
agreement between the purchaser and the supplisr.
4.2 Care should be taken to avoid grinding stressesduring cutting of the test piece. Burrs, if any,
should be removed by filling.
4.3 Test pieces for the mercurous nitrate test shall not be marked for identification by stamping.
Adopted 25 June 1988 @ March 1989, BIS Gr 2
%-. 1 I
BUREAU 0.F INDIRN STA’ND-AR,DS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
IS : 2206 6 1888
6. Procedure
6.1 First degrease the test piece. Then totally immerse it in an aqueous solution of sulphuric
acid ( 16 percent by volume ) or in a mixture containing 60 parts by volume of distilled water and
40 parts by volume of concentrated nitric acid for a period not exceeding 30 seconds, to remove
all traces of carbonaceous matter and oxide films. Remove the test piece from the pickling
solution and wash it immediately in running water. Then drain the test piece free of excess water
and totally immerse it in the mercurous nitrate solution. Use at least 1.6 ml of test solution per
square centimetre of exposed surface of the test piece.
5.2 After 30 minutes, remove the test piece from the mercurous nitrate solution and wash it in
running water. Wipe off any excess mercury from the surface of the test piece. Examine the
test piece at once, unless otherwise specified in the material specification. The material speci-
fication may permit a lapse of time before examination, which may vary with the alloy being
tested. In case of doubt regarding the presence of cracks, volatilize ( with caution ) the mercury
on the surface of the test piece by the application of heat on a hot-plate or in an oven. Then
examine the specimen for cracks under suitable magnifying equipment at a magnification of 10 to
18 X.
Caution - Mercury is a definite health hazard and, therefore, equipment for the detection
and removal of mercury vapour produced in volatilization is recommended. The use of
rubber gloves is advisable.
6.3 A solution, the concentration of which is not in accordance with that specified in 3, shall not
be used. Howover, the spent solution can be used after proper replenishment procedure given
in Appendix A.
Caution - Mercury is a definite heahh hazard in use and disposal. The’method of mercurous
nitrate solution disposal is given in Appendix B.
6. Test Requirements
6.1 Theinterpretation of the visual appearance of the test Pie&3 after testing is to be specified
in the relevant material specification.
APPEN’DIX A
( c/8US@ 5.3 )
REPLENISHMENT PROCEDURE OF SPENT MERCUROUS NITRATE SOLUTION
A-l. The spent solution may be reclaimed by replenishing the mercurous nitrate solution to a’
1 percent concentration as follows.
A-T.1 Measure, as accurately as possible in a small graduated, cylinder, 60 ml of the spent
mercurous nitrate solution.
A01.2 l’ransfer the solution to a Erle’nmeyer flaska’nd add 10 ml of nitric acid ( 1 : 1 ).
A-1.3 Add slowly potassium permanganate solution ( 1 percent ) from a burette with a constant
shaking until there .is, an excess as indicated by the pink colour, which persists for several minutes,
A-l.4 Add.ferrous sulphate cystals until the solution, when shaken, becomes clear. Then titrate
the solution with O-1 N potassium cyanide solution ( KCN ) to the appearance of a reddish brown
colour. Repeat the procedure with 50 ml of a standard mercurous nitrate solution ( 1 percent ).
A-1.5 The ratio, R, of the number of ml of potassium cyanide solution required to titrate the
spend solution, to the number of ml required to titrate the standard solution, determine the
number of ml, X of 10 percent mercurous nitrate in 3 percent nitric acid required to replenish
1 litre of spent solution. Values of R and X for a litre volume are given in Table 1.
IS : 2206 l 1999
TABLE 1 REPLENIBHMENT OF BPENT MERCUROUS NITRATE SOLUTION TO 1 PERCENT
CONCENTRATION
( Clause A-l.5 )
x.. 111.1 (1 --R)
where
R = fraction of mercury remaining in rolution ( determined by titration ), and
X = number of ml of mercurouB nitrate solution ( 10 percent ) to be added to 1 litre of spent mercurous
nitrate solution to raise the concentration of mercurous nitrate to 1 percent.
R X R X
O-10 100~0 0.56 48-S
0.12 97.6 0.56 46’7
o-14 96.6 0.60 44.4
O-16 93.3 0.62 42-2
0.16 91.1 O-64 40’0
O-20 66.9 0’66 37.8
0.22 66.7 0.68 as.6
0.24 a44 070 33.3
0.26 822 0.72 31.1
0.28 80.0 0.74 28.9
030 77-a 076 26’7
0.32 755 0.78 244
0.34 73.3 0.80 22.2
036 71’1 0.82 20’0
0.36 68.9 0.84 178
o-40 66.7 086 16*6
0’42 64.4 088 13.3
0’44 62’2 0’90 11’1
0.46 60.0 O-82 8-9
O-48 57.8 0.04 6’7
0.50 55’6 O-96 4.4
0.52 593 O-98 2.2
0’54 51.1
APPENDIX B
( Clause 5.3 )
METHOD FOR DISPOSAL OF SPENT MERCUROUS NITRATE SOLUTION
B-1, To mercurous nitrate solution, add sodium hydroxide to PH 1 O-1 1.
B-2. Filter precipitated mercury and other heavy metals.
B-3. Though the filtrate is low in free merCUrOUS or mercuric ions, it must be further treated
before disposal.
B-4,. To each litre of filtrate, add two drops ( O-1 cm3 ) of 24 percent ammonium sulphide.
B-5. After the second filtering, the filtrate may be discarded.
B-6. The precipitate should be collected and stored with the mercury contaminated test samples
and sold to a metal reclaimer.
3
IS:2306 -1888
EXPLANATORY NOTE
This standard was first published in 1962. In this revision, the following modifications have
been made:
a) The procedure have been updated and brought in line with IS0 and ASTM standards.
b) Appendices A and B giving the replenishment procedure of spent mercurousnitrate
solution and method of its disposal have been added.
In the preparation of this standard, assistancehas been derived from the following standards:
a) IS0 196-l 978 Wrought copper and copper alloys - Detection of residual stress -
Mercury (I) nitrate test, issued by the International Organization for Standardization
( IS0 ).
b) ASTM B 164-82 Method for mercurous nitrate test for copper and copper alloys, issued
by the American Society for Testing and Materials, USA.
Printed at Central Electric Press, Delhi-28 4
