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Author: Subject: KBr.CuBr2 double salt aka KCuBr3
Fery
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[*] posted on 7-2-2020 at 08:09
KBr.CuBr2 double salt aka KCuBr3


I found this info about 1 year ago:
http://copper.atomistry.com/cupric_bromide.html
Quote:
double salts are exemplified by the black 2LiBr,CuBr2,6H2O; KBr,CuBr2, lustrous, dark-coloured prisms; and the green 2NH4Br,CuBr2,2H2O

From the 3 possibilities I chose the KBr variant because it is anhydrous (stability) and surprisingly in 1:1 ratio - others are 2:1 and also Cu2+ is known to form [CuBr4]2-

Reagents:
48% HBr, CuO (prepared by myself from CuSO4 + 2 KOH -> Cu(OH)2 and then Cu(OH)2 -> CuO + H2O), KBr, conc. H2SO4 (as desiccant).

Glass:
2 beakers (25 ml), 700 ml glass jar (from pickles, honey etc) suitable for containing both beakers inside.

Procedure:
Put 5,01 g 48% HBr into 25 ml beaker and add 1,30 g CuO in small portions (in excess as I prepared it by myself so it was far from 100% purity), slightly warm, and at the end short mild boil to expel traces of Br2 (HBr used was just right from the bottle, not freshly distilled). Filter out small unreacted excess of CuO and wash the filter with H2O.
Add 3,68 g KBr into the beaker and dissolve it.
Let it to evaporate at room temperature for 1 week.
Put the beaker into a jar. Put 10 ml of conc. H2SO4 into another 25 ml beaker and insert the beaker into the jar and close the jar lid tightly.
After 10 days no visibility of crystals but the volume of Cu solution with slightly smaller volume. Remove the formerly 10 ml H2SO4 (now diluted and with little expanded volume) and replace with 15 ml of fresh conc. H2SO4.
After 1 week not yet signs of crystallization, volume of thick Cu solution in beaker about 5 ml, but after 2 weeks the salt climbing up the beaker walls finally, after 3 weeks completely dry crystals without any H2O.
I chose jar and 2 beakers method instead of desiccator to prevent rapid drying. The slower the process the bigger crystals (the surface of H2SO4 in 25 ml beaker is much smaller than in desiccator).

photos will follow soon...

all materials concerning the product in the attachment

Attachment: CorrigeChimieEquilibre-6.pdf (821kB)
This file has been downloaded 357 times

Attachment: holmes1975.pdf (387kB)
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Attachment: inoue1967.pdf (363kB)
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Attachment: stepakova2007.pdf (330kB)
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1026.png - 248kB 1027.png - 262kB




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Fery
International Hazard
*****




Posts: 1015
Registered: 27-8-2019
Location: Czechoslovakia
Member Is Offline


[*] posted on 7-2-2020 at 08:25
photos


48% HBr + 0,10 g CuO

IMG_20200105_190908_0_sm.jpg - 13kB IMG_20200105_191214_7_sm.jpg - 27kB



after adding 1,00 g CuO totally

IMG_20200105_191834_2_sm.jpg - 26kB IMG_20200105_191904_5_sm.jpg - 28kB



after adding 1,30 g CuO totally (excess)


IMG_20200105_193114_4_sm.jpg - 28kB



after filtering and carefully slowly washing the filter with H2O, photographing sky, sun, trees through the beaker

IMG_20200112_122404_5_sm.jpg - 17kB IMG_20200112_135541_2_sm.jpg - 18kB IMG_20200112_135548_9_sm.jpg - 17kB IMG_20200112_140616_4_sm.jpg - 25kB IMG_20200112_140758_0_sm.jpg - 87kB



the product

IMG_20200207_152902_3_sm.jpg - 31kB



the detail of crystals (higher resolution photos)

IMG_20200207_153305_9_sm.jpg - 3.8MB IMG_20200207_153323_5_sm.jpg - 4MB




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