salt analysis

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10 Feb 2009 05:47:43 IST
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10 Feb 2009 05:47:43 IST
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salt analysis
Engineering Entrance , JEE Main , JEE Main & Advanced , Chemistry , Inorganic Chemistry , academic

SEMI – MICRO QUALITATIVE ANALYSIS OF SIMPLE INORGANIC SALT
_______________________________________________________________
CATIONS: Pb 2+ ,Hg 2+ ,Cu 2+ ,Cd 2+ , Ag + , Fe 2+ , Fe 3+ , Al 3+ , Zn 2+ , Mn 2+ , Co 2+ , Sr 2+ , Ba 2+ , Mg 2+ , NH4 +
ANIONS: CO3 2- , S 2- , SO3 2- , SO4 2- , NO2 - , NO3 - , Cl - , Br 2- , PO4 3- , CH3COO -
_______________________________________________________________
PRELIMINARY TESTS
1. Note the state (amorphous or crystalline) and colour of salt.
2. Test the solubility of the salt in the following solutions:
i. Water (cold and hot)
ii. Dilute HCl (cold and hot)
iii. Dilute HNO3 (cold and hot)
_______________________________________________________________
IDENTIFICATION OF ACID RADICALS (ANIONS)
This part is the classified into three groups:
FIRST GROUP OF ACID RADICALS
The acid radicals involved in this group are carbonate(CO3 2- ), Sulphide(S 2- ), Sulphite(SO3 2- ),
Thiosulphate(S2O3 2- ) and nitrate(NO2 - ). The group reagent is dilute hydrochloric acid.
EXPERIMENT OBSERVATION INFERENCE
Effervescence or evolution of gases 1 st group of acid radicals is present.
(a) Colourless, odourless gas turns lime water
milky The acid radical may be CO3 2- or HCO3 -(
b) Colourless with rotten eggs smell and turns
lead acetate paper black. Sulphide(S 2- ) is confirmed.
(c) Colourless gas with suffocating smell. Heat
and pass the gas through acidified K2Cr2O7
solution. The solution turns green
SO3 2- is confirmed.
(d) Colourless gas with suffocating smell with a
yellow ppt. of sulphur in the test tube. Heat and
pass the gas through acidified K2Cr2O7 solution.
The solution turns dark blackish green.
S2O3 2- is confirmed.
(e) Colourless gas followed by brown gas and it
turns starch iodide paper blue. NO2 - is confirmed.
Salt + dil. HCl
(f) Colourless gas with the smell of vinegar. The acid radical may be CH3COO --
1 -?Tests to distinguish between CO3 2- and HCO3 -
EXPERIMENT OBSERVATION INFERENCE
(a) Lime water does not turn milky. CO3 2- is confirmed. Salt + water, boil and pass the
gas through lime water (b) Lime water turns milky. HCO3 - is confirmed.
Confirmation test for Acetate
EXPERIMENT OBSERVATION INFERENCE
Salt solution + Neutral FeCl3 sol. Appearance of blood red colour. Acetate is confirmed
SECOND GROUP OF ACID RADICALS
The acid radicals involved in this group are Cl - , Br - and NO3 - . The group reagent is concentrated
sulphuric acid (H2SO4).
EXPERIMENT OBSERVATION INFERENCE
Effervescence with colourless or coloured gases 2 nd group Acid radical is
present
(a) Colourless gas with a pungent smell and gives dense
white fumes when a glass rod dipped in ammonium
hydroxide (NH4OH) is exposed.
The Acid radical may be Cl -(
b) Brown gas and the solution is not blue. The acid radical may be Br -
Salt +
Concentrated
H2SO4 and heat
if necessary.
(c) Light brown gas and brown gas with pieces of copper
turnings and the solution turns blue in the test tube. The Acid radical may be NO3 -Confirmation
test for Chloride
EXPERIMENT OBSERVATION INFERENCE
(a) Chromyl – Chloride test: Salt + few
K2Cr2O7 crystals + conc. H2SO4 and heat
Pass the vapours through the test tube
which contains NaOH solution.
To this yellow solution, add dilute
CH3COOH and lead acetate solution.
Red vapours are obtained.
The solution turns yellow.
Yellow ppt. is formed
Chloride is confirmed.
(b) Silver Nitrate test: Salt solution +
AgNO3 solution + dilute HNO3
White ppt. is formed
which is soluble in NH4OH. Chloride is confirmed.
- 2 -?Confirmation test for Bromide
EXPERIMENT OBSERVATION INFERENCE
(a) Globule Test: Aqueous solution of salt + two
drops of CCl4 + 1ml chlorine water and shake
well.
An orange-red globule is
obtained Bromide is confirmed.
(b)Silver Nitrate test: Salt solution + AgNO3
solution + dilute HNO3
A pale yellow ppt. slightly soluble
in NH4OH is obtained. Bromide is confirmed.
Confirmation test for Nitrate
EXPERIMENT OBSERVATION INFERENCE
Brown ring test: Strong solution of the substance + 2 or
3 drops of conc. H2SO4, and cool. Add freshly prepared
FeSO4 solution on the sides of the test tube.
A brown ring is formed
at the junction of two
liquids.
Nitrate is confirmed.
THIRD GROUP OF ACID RADICALS
The basic radicals involved in this group are SO4 2- and PO4 3- .
EXPERIMENT OBSERVATION INFERENCE
Test for Sulphate: Aqueous solution of salt + dilute
HCl + BaCl2 solution.
A white ppt. insoluble in dilute
HCl is obtained
Sulphate (SO4 2- ) is
confirmed.
Ammonium – Molybdate Test: 2ml of soda extract 1 +
dilute HNO3 + Ammonium Molybdate solution.
A canary yellow precipitate is
obtained.
Phosphate (PO4 3- ) is
confirmed.
1 Soda extract to be prepared if the given salt is partially soluble in water.
- 3 -?ANALYSIS OF BASIC RADICALS OR CATIONS
This is classified into 6 groups. They are mentioned as below:
GROUP RADICALS GROUP REAGENTS
I Pb 2+ ,Ag + Dilute Hydrochloric acid(HCl)
II Pb 2+ ,Hg 2+ ,Cu 2+ ,Cd 2+ Dilute HCl + H2S gas.
III Al 3+ ,Fe 2+ , Fe 3+ NH4Cl(s) + NH4OH
IV Zn 2+ ,Mn 2+ ,Co 2+ ,Ni 2+ NH4Cl(s) + NH4OH + H2S gas
V Ca 2+ ,Sr 2+ ,Ba 2+ NH4Cl(s) + NH4OH + (NH4) 2CO3
VI Mg 2+ , NH4 + -Nil-
Preparation of Original solution: A suitable solvent is found for the salt as given in the preliminary test. A
few drops are used as solution.
Test for NH4 + Radicals: This test is carried out before starting the analysis for the basic radicals.
EXPERIMENT OBSERVATION INFERENCE
(a) Salt + NaOH solution and heat it.
Expose a glass rod dipped in conc.
HCl to the gas and moist red litmus
paper.
Colourless gas with a pungent smell is
obtained.
Dense white fumes and moist red
litmus paper turns blue
NH4 + may be present in the
salt
(b) Original solution + Nesseler’s
reagent. Brown solution or ppt. is obtained NH4 + is confirmed.
FIRST GROUP OF BASIC RADICALS
The basic radicals of this group are Pb 2+ & Ag + .The group reagent is dilute HCl.
EXPERIMENT OBSERVATION INFERENCE
White ppt. is formed. May be Pb 2+ & Ag +
(a) ppt. dissolves in hot water. May be Pb 2+
(1) Original solution + Dilute HCl
Filter and add water to ppt.
and heat (b) ppt. is insoluble in water. May be Ag +
- 4 -?(a) A yellow ppt. is formed. Pb 2+ is confirmed. (2) Original solution + Potassium
Chromate solution. (b) A brick red ppt. is formed. Ag + is confirmed.
(3) Original solution + KCl sol.
ppt. obtained + water and
heat it.
A yellow ppt. soluble in hot
water, on cooling reappears as
golden yellow spangles. Pb 2+ is confirmed. The yellow ppt. is insoluble
in hot water.
SECOND GROUP OF BASIC RADICALS
The basic radicals of this group are Pb 2+ , Hg 2+ , Cu 2+ and Cd 2+ .The group reagent is Dilute HCl + H2S gas.
EXPERIMENT OBSERVATION INFERENCE
May be Pb 2+ Hg 2+ & Cu 2+ (a)A Black ppt. is observed. Original solution + Dilute HCl +
H2S gas. (b)A yellow ppt. is observed. May be Cd 2+
The identification of Pb 2+ , Hg 2+ , Cu 2+ and Cd 2+ are as follows:
EXPERIMENT OBSERVATION INFERENCE
(a) Original solution + Potassium
Chromate. A yellow ppt. is observed. Pb 2+ is confirmed.
(b)Original solution + NH4OH
A bluish white ppt. soluble in excess
of NH4OH is observed which gives
rise to a deep blue solution.
May be Cu 2+
(c) Original solution + dil. acetic
acid + potassium Ferro cyanide sol. A chocolate red ppt. is observed. Cu 2+ is confirmed.
(d) Dissolve the black ppt. in aqua
regia 2 + 1ml of distilled water,
heat & add 2 drops of SnCl2
A white ppt. is observed which turns
grey. Hg 2+ is confirmed.
(e) Original solution + dilute acetic
acid + H2S gas. A yellow ppt. is formed. Cd 2+ is confirmed.
2 Aqua regia is mixture of 3 drops of HCl + 1 drop of HNO3
- 5 -?THIRD GROUP OF BASIC RADICALS
The basic radicals of this group are Al 3+ , Fe 2+ and Fe 3+ .The group reagent is NH4Cl + NH4OH
EXPERIMENT OBSERVATION INFERENCE
May be Al 3+ (a) A white gelatinous ppt. is obtained.
(b) A dirty green ppt. is obtained May be Fe 2+
(1) Original solution +
NH4Cl(s) + NH4OH in
excess (c) A reddish brown ppt. is obtained May be Fe 3+
(a) White gelatinous ppt. soluble in excess of NaOH
is obtained which gives a colourless sol. The basic radical is Al 3+
(b) Dirty green ppt. insoluble in excess of NaOH The basic radical is Fe 2+ (2) Original solution +
NaOH solution
(c) Reddish brown ppt. insoluble in excess of NaOH The basic radical is Fe 3+
(3) Clear solution of
2(a) + solid NH4Cl and
heat
The white gelatinous ppt. reappears. Al 3+ is confirmed.
(4) Original solution +
acidified KMnO4 solution
which is added drop wise.
(a) The pink colour of KMnO4 is not discharged. Fe 3+ is confirmed.
FOURTH GROUP OF BASIC RADICALS
The basic radicals of this group are Zn 2+ , Mn 2+ , Co 2+ & Ni 2+ .The group reagent is NH4Cl + NH4OH
And H2S(g).
EXPERIMENT OBSERVATION INFERENCE
May be Zn 2+ , Mn 2+ or Co 2+ (a) a white ppt. is obtained
(1) Original solution + NH4Cl(s)
+ NH4OH in excess + H2S(g) (b) Buff or pale pink or flash coloured ppt.
soluble in dilute HCl is obtained. May be Mn 2+
(a) The white ppt. is soluble in excess of
NaOH giving a colourless solution. Zn 2+ is confirmed
(2) Original solution + NaOH
solution+. (b) The white ppt. insoluble in excess of
NaOH but turns brown. Mn 2+ is confirmed
- 6 -?A Blue colour in the alcohol
layer is obtained.
FIFTH GROUP OF BASIC RADICALS
The basic radicals of this group are Ca 2+ , Sr 2+ & Ba 2+ .The group reagent is NH4Cl(s) + NH4OH and
(NH4)2 CO3.
EXPERIMENT OBSERVATION INFERENCE
(1) Original solution + NH4Cl(s) + NH4OH in
excess + (NH4)2 CO3 solution. (a) A white ppt. is obtained. May be Ca 2+ , Sr 2+ or
Ba 2+
A yellow ppt. is obtained. May be Ba 2+ .
A thin white ppt. is obtained. May be Sr 2+ .
(2) Dissolve the white ppt. obtained in small
amounts of dilute acetic acid. Divide the
solution in three parts.
Part (1) + Potassium chromate solution.
Part (2) + Calcium Sulphate Sol. and heat.
Part (3) + Ammonium exalate solution. A white ppt. is obtained. May be Ca 2+ .
(a) Apple green coloured flame is
obtained. Ba 2+ is confirmed.
(b) Crimson red coloured flame is
obtained. Sr 2+ is confirmed.
(3)Flame tests: Make a paste of the given
salt with few drops of Conc. HCl in a watch
glass. Heat a Pt. wire in non luminous flame
till no colour is imparted to the flame. Dip
the Pt. wire in the paste and hold it in the
flame. (c) Brick red coloured flame is
obtained, Ca 2+ is confirmed.
SIXTH GROUP OF BASIC RADICALS
EXPERIMENT OBSERVATION INFERENCE
(1) Original solution + excess of NH4OH +
Ammonium Hydrogen Phosphate. A white ppt. is obtained. Mg 2+ is confirmed.
______________________________________________________________
*****THE END*****
Co 2+ is confirmed
(3) Dissolve the 1(a) in aqua regia, evaporate to
Dryness, add 1ml of distilled water and divide
the resultant product into two parts.
Part (1) + 1 ml of amyl alcohol + 100 mg of solid
NH4SCN and stir it.
Part (2) + 5 drops of dimethyl glyaxime reagent +
NH4OH. A pink ppt. is obtained. Ni 2+ is confirmed.
- 7 -


Comments (8)


New kid on the Block

Joined: 13 Mar 2009 15:31:09 IST
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10 Apr 2009 06:24:19 IST
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gud work

Blazing goIITian

Joined: 17 Mar 2008 20:56:33 IST
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10 Apr 2009 09:42:51 IST
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perfect article

New kid on the Block

Joined: 28 Jan 2012 11:44:39 IST
Posts: 1
28 Jan 2012 11:44:40 IST
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this should have been best presented in tabular format.this is however a good job

New kid on the Block

Joined: 23 Feb 2012 00:37:30 IST
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23 Feb 2012 00:37:30 IST
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I appreciate all your indulgence.Thank you for your patriotic service.

New kid on the Block

Joined: 14 Feb 2012 15:45:01 IST
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23 Feb 2012 08:08:38 IST
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Thats gr8thank u so much

New kid on the Block

Joined: 24 Aug 2012 19:50:54 IST
Posts: 1
24 Aug 2012 19:50:55 IST
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great discription. but it can be more better if u write it in a tabular form. more easy to learn it..... but still a gud work.... thnx

Hot goIITian

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26 Aug 2012 07:37:10 IST
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good work

New kid on the Block

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19 Sep 2012 19:15:43 IST
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Leran from Book " Bhoolana Bhool Jaaoge"????? ????? ???? ?? ????? ?????-1 1 ?? 10 ???? ??????? ???? ???? ????,??? ?????? ??? ???? ??????? ??? ?? ??? ??? ?? ??????????? ????? ????? ??????????? ????? ????? ????? ?1 -- ????????? -- H ? Hydrogen 2 -- ?????? -- He ? Helium 3 -- ?????? -- Li ? Lithium 4 -- ???????? -- Be ? Beryllium 5 -- ?????? -- B ? Boron 6 -- ?????? -- C ? Carbon 7 -- ????????? --N ? Nitrogen 8 -- ??????? --O ? Oxygen 9 -- ??????? -- F ? Fluorine 10 -- ????? -- Ne ? Neon 11 ?? 20 ???? ???? ?? ??? ?? ???? ????, ?????? ???? ??????? ?????? ? ??? ??? ????? ??? ????? ? ???? ?????? ????? ????? ????? ?????? ????? ????? ????? ?11 -- ?????? -- Na -- Sodium (????? ???? 'Natrium' ??) 12 -- ?????????? -- Mg ? Magnesium 13 -- ??????????? -- Al ? Aluminium 14 -- ??????? -- Si ? Silicon 15 -- ???????? -- P ? Phosphorus 16 -- ????? -- S ? Sulphur 17 -- ??????? -- Cl ? Chlorine 18 -- ????? -- Ar ? Argon 19 -- ???????? -- K --Potassium (????? ???? ?? ???? ?alium???) 20 -- ???????? -- Ca -- Calcium ???? ?? ????? ?????-221 ?? 30 ?????????? ??????? ??? ???????? ?? ??? ??????,????? ?????? ?????? ?? ???? ?????????? ???? ????? ??? ?? ??? ???? ?????? ????? ????? ??????????? ????? ????? ????? ?21 -- ?????????? -- Sc ? Scandium 22 -- ????????? -- Ti ? Titanium 23 -- ??????? -- V ? Vanadium 24 -- ???????? -- Cr ? Chromium 25 -- ??????? -- Mn ? Manganese 26 -- ???? --Fe -- Iron (????? ???? 'Ferrum' ??)27 --??????? -- Co ? Cobalt 28 -- ????? -- Ni ? Nickel 29 -- ????? --Cu -- Copper (????? ???? 'Cuprum' ??)30 --????? --Zn ? Zinc 31 ?? 40 ???? ??? ??? ????? ??????? ?????,?????? ????? ???? ?? ???? ????????? ?????? ??????? ??? ??? ????? ?????? ????? ????? ????? ?????? ????? ????? ????? ?31 -- ?????? -- Ga ? Gallium 32 -- ????????? -- Ge ? Germanium 33 -- ???????? -- As ? Arsenic 34 -- ???????? -- Se ? Selenium 35 -- ??????? -- Br ? Bromine 36 -- ???????? -- Kr ? Krypton 37 -- ???????? -- Rb ? Rubidium 38 -- ???????????? -- Sr ? Strontium 39 -- ??????? -- Y ? Yttrium 40 -- ????????? -- Zr -- Zirconium???? ?? ????? ?????-341 ?? 50 ????????? ???? ???? ??? ???,??? ?? ???? ??? ????? ???? ??? ??? ?????? ??? ?? ????? ???? ??? ?? ??? ?? ?????? ????? ????? ????? ?????? ????? ????? ????? ?41 -- ???????? -- Nb ? Niobium 42 -- ?????????? -- Mo ? Molybdenum 43 -- ?????????? -- Tc -- Technetium 44 -- ???????? -- Ru ? Ruthenium 45 -- ?????? -- Rh ? Rhodium 46 -- ??????? -- Pd ? Palladium 47 -- ????? -- Ag -- Silver (????? ???? 'Argentum' ??) 48 -- ??????? -- Cd ? Cadmium 49 -- ??????? -- In ? Indium 50 -- ????? -- Sn -- Tin (????? ???? 'Stannum' ??) 51 ?? 60 ????????? ???? ?????? ?? ??????? ???? ,???? ???? ?????? ???? ??????? ????? ???? ????? ?? ??? ?????? ????? ????? ????? ?????? ????? ????? ????? ?51 -- ????????? -- Sb -- Antimony (????? ???? ' Stibium' ??) 52 -- ???????? -- Te ? Tellurium 53 -- ?????? -- I ? Iodine 54 -- ?????? -- Xe ? Xenon 55 -- ??????? -- Cs ? Caesium 56 -- ?????? -- Ba ? Barium 57 -- ??????? -- La ? Lanthanum 58 -- ?????? -- Ce ? Cerium 59 -- ??????????????? -- Pr -- Praseodymium 60 -- ??????????? -- Nd ? Neodymium ???? ?? ????? ?????-461 ?? 70 ???????????? ?? ????? ??? ????? ???? ,???? ???????? ?? ?? ???? ??? ????? ?????? ??????? ?? ??? ????? ?????? ????? ????? ????? ?????? ????? ????? ????? ?61 -- ?????????? -- Pm -- Promethium 62 -- ??????? -- Sm -- Samarium 63 -- ???????? -- Eu -- Europium 64 -- ???????????? -- Gd -- Gadolinium 65 -- ??????? -- Tb -- Terbium 66 -- ???????????? -- Dy -- Dysprosium 67 -- ???????? -- Ho -- Holmium 68 -- ??????? -- Er -- Erbium 69 -- ?????? -- Tm -- Thulium 70 -- ?????????? -- Yb ? Ytterbium71 ?? 80 ???? ???? ???? ???? ???? ???? ?? ?????, ????? ??? ???? ???? ???? ??? ???? ? ????? ?? ?? ???? ???? ???? ???? ?? ??? ?????? ????? ????? ????? ?????? ????? ????? ????? ? 71 -- ???????? -- Lu ? Lutetium 72 -- ???????? -- Hf ? Hafnium 73 -- ??????? -- Ta ? Tantalum 74 -- ???????? -- W -- Tungsten (????? ???? ?? ????'Wolfram' ??)) 75 --?????? -- Re ? Rhenium 76 -- ??????? -- Os ? Osmium 77 -- ??????? -- Ir ? Iridium 78 -- ???????? -- Pt ? Platinum 79 -- ???? --Au -- Gold (????? ???? 'Aurum' ??)80 --???? --Hg -- Mercury (????? ???? 'Hydragyrum' ??)???? ?? ????? ?????-5 81 ?? 90 ???????? ???? ????? ???? ,???????? ?? ???? ???? ???????? ?????? ??????? ???? ?????? ????? ????? ??????????? ????? ????? ????? ?81 -- ?????? -- Tl ? Thallium 82 -- ???? --Pb -- Lead (????? ???? 'Plumbum' ??)83 --?????? -- Bi ? Bismuth 84 -- ???????? -- Po ? Polonium 85 -- ???????? -- At ? Astatine 86 -- ???? -- Rn ? Radon 87 -- ?????????? -- Fr ? Francium 88 -- ?????? -- Ra ? Radium 89 -- ????????? -- Ac ? Actinium 90 -- ?????? -- Th ? Thorium 91 ?? 100 ????????????? ?????? ??????? ??????,?????? ?????? ????? ???? ???????????? ??? ??????? ?????? ?????? ?????? ????? ????? ????? ?????? ????? ????? ????? ?91 -- ?????????????? -- Pa ? Protactinium 92 -- ???????? -- U ? Uranium 93 -- ???????????? -- Np ? Neptunium 94 -- ?????????? -- Pu ? Plutonium 95 -- ????????? -- Am ? Americium 96 -- ???????? -- Cm ? Curium 97 -- ????????? -- Bk ? Berkelium 98 -- ???????????? -- Cf ? Californium 99 -- ????????????? -- Es ? Einsteinium 100 -- ??????? -- Fm ? Fermium ???? ?? ????? ?????-6101 ?? 112 ???????? ???? ???? ?????? ???? ??? ,????? ???? ????? ???? ????? ???? ??????????? ???????? ??? ????????? ????????? ????? ????? ??????????? ????? ????? ??????101 -- ???????????? -- Md ? Mendelevium 102 -- ???????? -- No ? Nobelium 103 -- ????????? -- Lr ? Lawrencium 104 -- ???????????? -- Rf ? Rutherfordium 105 -- ??????? -- Db ? Dubnium 106 -- ?????????? -- Sg ? Seaborgium 107 -- ?????? -- Bh ? Bohrium 108 -- ????? -- Hs ? Hassium 109 -- ??????????? -- Mt ? Meitnerium 110 -- ??????????????? -- Ds ? Darmstadtium 111 -- ??????????? -- Rg ? Roentgenium 112 -- ???????? -- Uub ? Copernicium 113 ?? 118 ???? ?? ?? ???? ?????? ??????,?????? ?????? ??????????? ?? ????? ????? ??? ????????? ????? ????? ??????????? ????? ????? ??????113 -- ?????????? -- Uut ? Ununtrium 114 -- ???????????? -- Uuq ? Ununquadium 115 -- ???????????? -- Uup ? Ununpentium 116 -- ???????????? -- Uuh ? Ununhexium 117 -- ?????????????? -- Uus ? Ununseptium 118 -- ??????????? -- Uuo ? Ununoctium



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