Optimization of Preparation and Characterization of Copper Sulfate Pentahydrate Crystals

doi:10.19894/j.issn.1000-0518.240177

Chinese Journal of Applied Chemistry ›› 2025, Vol. 42 ›› Issue (3): 416-428.DOI: 10.19894/j.issn.1000-0518.240177

• Chemistry Teaching and Experiment Innovation • Previous Articles

Optimization of Preparation and Characterization of Copper Sulfate Pentahydrate Crystals

Yi-En DU¹(), Shao-Hua GUO²(), Ai-Hua ZHANG¹

^1.Department of Chemistry and Chemical Engineering，Jinzhong University，Jinzhong 030619，China
^2.School of Modern Engineering and Applied Science，Nanjing University，Nanjing 210093，China

Received:2024-06-05 Accepted:2024-12-23 Published:2025-03-01 Online:2025-04-11
Contact: Yi-En DU,Shao-Hua GUO
About author:shguo@nju.edu.cn
duyien124@163.com；
Supported by:
the Teaching Reform and Innovation Project of Higher Education Institutions in Shanxi Province(J20241335);the “Research Project on Higher Science Education” of the Professional Committee of Science Education, China Higher Education Society(21ZSKJYYB08)

Abstract

Abstract:

The preparation of copper sulfate pentahydrate （CuSO₄·5H₂O） crystals is an important comprehensive synthesis experiment in inorganic chemistry. In this paper， a set of experimental equipment for the preparation of copper sulfate pentahydrate by the reaction of copper powder with sulfuric acid （H₂SO₄） and nitric acid （HNO₃） was designed. The experimental conditions were discussed. The structure of recrystallization product and the content of crystal water were analyzed by X-ray powder diffractometer and synchronous thermal analyzer. The experimental results indicate that by improving the experimental apparatus and optimization of the experimental method， not only the purity and yield of the prepared product were significantly increased， but also toxic gases such as NO and NO₂ generated during the reaction process could be completely absorbed by the NaOH solution， thus achieving environmentally friendly green chemistry practices. This improvement and optimization not only increase the efficiency and safety of the experiment， but also promote the cultivation of students' experimental skills and scientific literacy.

Key words: Copper sulfate pentahydrate, Preparation, Experimental method optimization, Crystal, Compositional analysis

CLC Number:

O614.8

Yi-En DU, Shao-Hua GUO, Ai-Hua ZHANG. Optimization of Preparation and Characterization of Copper Sulfate Pentahydrate Crystals[J]. Chinese Journal of Applied Chemistry, 2025, 42(3): 416-428.

Figures/Tables 19

Fig.1 Ball-and-stick model of copper sulfate pentahydrate crystal

Fig.2 Experimental apparatus for the preparation of copper sulfate pentahydrate

Fig.3 The CuSO4·5H2O-C crystals were prepared （A） by heating a solution with an alcohol lamp until a crystalline film formed， and by heating solutions to 20 mL with （B） an alcohol lamp and （C） a water bath； CuSO4·5H2O-R crystals were recrystallized by reducing the volume of the respective crude crystal solutions to 10 mL：（D） water bath heating of solution （A），（E） alcohol lamp heating of solution （B）， and （F） water bath heating of solution （C）

Table 1 Effect of heating mode on product

编号	1	2	3
CuSO₄溶液的加热方式	酒精灯加热至出现晶膜	酒精灯加热至溶液为20 mL	水浴加热至溶液为20 mL
CuSO₄·5H₂O-C颜色	浅蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-C）/g	8.59	11.20	11.56
y（CuSO₄·5H₂O-R）/%	72.88	95.02	98.07
m（CuSO₄·5H₂O-C）/g	6.00	6.00	6.00
CuSO₄·5H₂O-R颜色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-R）/g	4.85	5.19	5.26
y（CuSO₄·5H₂O-R）/%	58.91	82.19	85.97

Fig.4 XRD patterns of CuSO4·5H2O-C crystals prepared by （a） heating with an alcohol lamp until a crystalline film appears on the surface and by heating the solution to 20 mL using （b） an alcohol lamp and （c） a water bath heating method； XRD patterns of CuSO4·5H2O-R crystals prepared by reducing the volume of the respective crude crystal solutions to 10 mL：（d） water bath heating of solution （a），（e） alcohol lamp heating of solution （b）， and （f） water bath heating of solution （c）

Fig.5 The CuSO4·5H2O-R crystals were prepared at water bath temperatures of （A） 30，（B） 50，（C） 70 and （D） 90 ℃， respectively

Table 2 Effect of water bath temperature on products

编号	4	5	6	7
T（H₂O）/℃	30	50	70	90
CuSO₄·5H₂O-C颜色	蓝色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-C）/g	11.37	11.46	11.43	11.39
y（CuSO₄·5H₂O-C）/%	96.46	97.23	96.97	96.63
m（重结晶用CuSO₄·5H₂O-C）/g	6.00	6.00	6.00	6.00
CuSO₄·5H₂O-R颜色	蓝色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-R）/g	5.25	5.32	5.31	5.25
y（CuSO₄·5H₂O-R）/%	84.40	86.21	85.82	84.55

Fig.6 The XRD patterns of CuSO4·5H2O-R crystals prepared at water bath temperatures of （a） 30，（b） 50，（c） 70 and （d） 90 ℃， respectively

Fig.7 The CuSO4·5H2O-R crystals prepared under conditions of H2SO4 solution concentrations of （A） 3，（B） 6 and （C） 9 mol/L， respectively

Table 3 Effect of sulfuric acid solution concentration on products

编号	5	8	9
c（H₂SO₄）/（mol·L^-1）	3	6	9
CuSO₄·5H₂O-C颜色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-C）/g	11.46	11.36	11.39
y（CuSO₄·5H₂O-C）/%	97.23	96.38	96.63
m（重结晶所用CuSO₄·5H₂O-C）/g	6.00	6.00	6.00
CuSO₄·5H₂O-R颜色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-R）/g	5.32	5.34	5.30
y（CuSO₄·5H₂O-R）/%	86.21	85.78	85.36

Fig.8 XRD patterns of CuSO4·5H2O-R crystals prepared at H2SO4 solution concentrations of （a） 3，（b） 6 and （c） 9 mol/L， respectively

Fig.9 The CuSO4·5H2O-R crystals prepared at concentrated HNO3 solution volumes of （A） 3，（B） 6，（C） 9 and （D） 12 mL， respectively

Table 4 Effect of concentrated HNO3 volume on the products

编号	5	10	11	12
V（浓HNO₃）/mL	6	3	9	12
CuSO₄·5H₂O-C颜色	蓝色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-C）/g	11.46	11.43	11.41	11.37
y（CuSO₄·5H₂O-C）/%	97.23	96.97	96.80	96.46
m（重结晶用CuSO₄·5H₂O-C）/g	6.00	6.00	6.00	6.00
CuSO₄·5H₂O-R颜色	蓝色	蓝色	蓝色	蓝色
m（CuSO₄·5H₂O-R）/g	5.32	5.20	5.27	5.15
y（CuSO₄·5H₂O-R）/%	86.21	84.04	85.02	82.79

Fig.10 XRD patterns of CuSO4·5H2O-R crystals prepared at concentrated HNO3 solution volumes of （a） 3，（b） 6，（c） 9 and （d） 12 mL， respectively

Fig.11 The CuSO4·5H2O-R crystals prepared in the presence of （A） 3 and （B） 6 mol/L HNO3 solutions， respectively

Table 5 Effect of HNO3 concentration on products

编号	13	14
c（HNO₃）/（mol·L^-1）	3	6
V（HNO₃）/mL	15	15
CuSO₄·5H₂O-C颜色	蓝色	蓝色
m（CuSO₄·5H₂O-C）/g	11.60	11.54
y（CuSO₄·5H₂O-C）/%	98.41	97.90
m（重结晶用CuSO₄·5H₂O-C）/g	6.00	6.00
CuSO₄·5H₂O-R颜色	蓝色	蓝色
m（CuSO₄·5H₂O-R）/g	5.23	5.20
y（CuSO₄·5H₂O-R）/%	85.78	84.85

Fig.12 XRD patterns of CuSO4·5H2O-R crystals prepared in the presence of （a） 3 and （b） 6 mol/L HNO3 solutions， respectively

Fig.13 Thermogravimetric analysis diagram of some prepared CuSO4·xH2O crystals

Table 6 The mass of the three selected CuSO4·xH2O crystal samples and the number of water molecules lost

编号	5		13		14
编号	m（CuSO₄·xH₂O）/mg	失去H₂O/个	m（CuSO₄·xH₂O）/mg	失去H₂O/个	m（CuSO₄·xH₂O）/mg	失去H₂O/个
升温前	13.33366	0	12.56798	0	13.06236	0
94 ℃	11.36896	1.531	10.80421	1.446	11.37396	1.315
104 ℃	11.33269	1.594	10.73752	1.510	11.33377	1.351
128 ℃	9.51743	3.552	9.06845	3.419	9.54741	3.261
208 ℃	9.43013	3.667	9.00937	3.499	9.48985	3.335
256 ℃	8.54975	4.957	8.16050	4.784	8.58863	4.615
618 ℃	8.53085	4.988	8.04777	4.979	8.46873	4.806

References 11

1	吴萍，陈维，唐亚文. 五水硫酸铜晶体制备实验优化条件的探究［J］. 江苏教育学院学报（自然科学）， 2013， 29（5）： 51-52， 75.
	WU P， CHEN W， TANG Y W. Study on optimum conditions of preparation experiment of copper sulfate pentahydrate crystal［J］. J Jiangsu Educ Univ （Nat Sci）， 2013， 29（5）： 51-52， 75.
2	宋鑫明，刘丹霞，郑彩娟，等. 水合硫酸铜制备实验的改进［J］. 化学教学， 2015， 6： 68-69.
	SONG X M， LIU D X， ZHENG C J， et al. Improvement of preparation experiment of hydrated copper sulfate［J］. Educ Chem， 2015， 6： 68-69.
3	李泽全，余丹梅. 大学化学实验［M］. 北京：科学出版社， 2017： 8.
	LI Z Q， YU D M. University chemistry experiment［M］. Beijing： Science Press， 2017： 8.
4	宋心琦. 普通高中课程标准试验教科书·实验化学［M］. 北京：人民教育出版社， 2007： 29.
	SONG X Q. High school curriculum standard experimental textbook experimental chemistry［M］. Beijing： People's Education Press， 2007： 29.
5	谢光明，龙小玲，沈飞，等. 用辉铜矿制取硫酸铜的试验研究［J］. 湿法冶金， 2012， 31（4）： 227-229.
	XIE G M， LONG X L， SHEN F， et al. Experimental research on preparation of copper sulfate using chalcocite［J］. Hydrometall China， 2012， 31（4）： 227-229.
6	满瑞林，甘源，余嘉耕，等. 五水硫酸铜的催化氧化制备［J］. 湖南化工， 1998， 28（3）： 31-32.
	MAN R L， GAN Y， YU J G， et al. Preparation of copper sulfate pentahydrate by catalytic oxidation［J］. Hunan Chem Ind， 1998， 28（3）： 31-32.
7	张仕秀. 硫酸铜制备实验的改进［J］. 文山师范高等专科学校学报， 2005， 18（2）： 176-178.
	ZHANG S X. Improvement of experiment on the preparation of bluestone［J］. J Wenshan Teach Coll， 2005， 18（12）： 176-178.
8	袁余洲，包明龙，张宏志. 制备五水硫酸铜的实验探讨［J］. 玉林师范高等专科学校学报， 2000， 21（3）： 58-59.
	YUAN Y Z， BAO M L， ZHANG H Z. Experimental study on preparation of copper sulfate pentahydrate［J］. J Yulin Norm Coll， 2000， 21（3）： 58-59.
9	黄理耀. 五水硫酸铜制备实验的改进［J］. 实验室研究与探索， 2004， 23（11）： 53.
	HUANG L Y. Improvement of preparation experiment of copper sulfate pentahydrate［J］. Res Explor Lab， 2004， 23（11）： 53.
10	张洪香，王洪玲，李晓亚. 实验室硫酸铜制备的绿色化改进［J］. 沧州师范学院学报， 2018， 34（1）： 124-128.
	ZHANG H X， WANG H L， LI X Y. Exploration of green preparation of copper sulfate in laboratory［J］. J Cangzhou Norm Univ， 2018， 34（1）： 124-128.
11	汪竹青，孙佳音，吴根华. 五水硫酸铜晶体的制备实验分析及优化［J］. 合肥师范学院学报， 2019， 37（3）： 50-51.
	WANG Z Q， SUN J Y， WU G H. Experimental analysis and optimization of preparation of copper sulfate pentahydrate crystals［J］. J Hefei Norm Univ， 2019， 37（3）： 50-51.

[1]	Yun-Yang LI, Rui-Zhe ZHENG, Yan ZHOU, Tu-Xun HAIREGU, Biao DONG. Research on the Regulation of Upconversion Fluorescence Spectral Properties on Single Particles [J]. Chinese Journal of Applied Chemistry, 2025, 42(3): 365-374.
[2]	Da-Wei TONG, Ming KONG, Yu-Bin XIANG. Synthesis， Photophysical Properties， Theoretical Calculation and Cell Imaging of a Tetraphenylethene Imidazole Compound with Methoxy Group [J]. Chinese Journal of Applied Chemistry, 2023, 40(9): 1322-1329.
[3]	Cong-Hui MIAO, Dilinuer AILI, Zheng-Kun LIAO, Jing-Shan LU, Qing-Hua LIU, Jiang-Yuan LI, Nulahong AISHA. Preparation of Fly Ash-based ZSM-5 Zeolite Molecular Sieve and Hydrogen Storage Properties [J]. Chinese Journal of Applied Chemistry, 2023, 40(7): 995-1003.
[4]	Yu-Chen TAO, Xiao-Hui HOU, Deng-Ke YIN, Ye YANG. Effect of Electric Field-Regulating Cholesterol-based Liquid Crystal Films on the Growth and Differentiation of Fibroblasts [J]. Chinese Journal of Applied Chemistry, 2023, 40(4): 546-553.
[5]	Zhi-Peng DU, Yang ZHOU, San-Gen ZHAO. Synthesis， Crystal Structure and Birefringence Properties of Silver Cluster Compound Ag₃B₆O₁₀I [J]. Chinese Journal of Applied Chemistry, 2023, 40(2): 229-235.
[6]	Jin-Jian LIU, Na LIU, Feng-Yi YANG. Synthesis and Photochromic Properties of Two Isostructural Viologen Coordination Polymers [J]. Chinese Journal of Applied Chemistry, 2023, 40(2): 245-251.
[7]	Zheng-Ce AN, Li-Ping WANG, Bo ZHOU. White-Light Upconversion and Application of Er³⁺/Tm³⁺ Co-Doped Ytterbium-Based Nanoparticles [J]. Chinese Journal of Applied Chemistry, 2023, 40(12): 1623-1629.
[8]	Shi-Wei LI, Xu HU, Chen-Xiao LUO, Zhi-He LIU, Zhi-Yong ZHANG, Xiang-Ru WANG. Synthesis and Microwave Properties of Fluorinated Triphenylacetylene Isothiocyano Liquid Crystals [J]. Chinese Journal of Applied Chemistry, 2023, 40(12): 1682-1692.
[9]	Fan LIU, Shao-Yong HUANG, Quan CHEN. Static Crystallization and Shear Induced Crystallization of the Poly（L-lactic acid） Telechelic Ionomer [J]. Chinese Journal of Applied Chemistry, 2023, 40(10): 1412-1419.
[10]	Jin LIN, Fang-Zhu WANG, Ling-Ling LYU. Preparation of Pseudo-boehamite from Industrial Materials and Its Application in Selective Hydrogenation of Isophorone [J]. Chinese Journal of Applied Chemistry, 2023, 40(1): 79-90.
[11]	Gao-Yong ZI, Bang-Fu HUANG, Meng DAI, Zheng-Yu YANG, Zhen-Jing WEN, Wan-Jun LI, Liu-Bin LUO. Effect of Chlorine Removal on Crystallization in the Mother Liquor of Ammonium Sulfate [J]. Chinese Journal of Applied Chemistry, 2022, 39(9): 1437-1446.
[12]	Xian WANG, Xiao-Long YANG, Rong-Peng MA, Chang-Peng LIU, Jun-Jie GE, Wei XING. Atomic Dispersion Ir‑N‑C Catalysts for Anode Anti‑poisoning Electrolysis in Fuel Cell [J]. Chinese Journal of Applied Chemistry, 2022, 39(8): 1202-1208.
[13]	Mei-Lun ZHANG, Hong-Ran LING, Zai-Chun SUN, Bing-Chu MEI, Wei-Wei LI. Research Progress on the Preparation Methods of BaMgF₄ Powders [J]. Chinese Journal of Applied Chemistry, 2022, 39(6): 900-911.
[14]	Li-Jun WU, Shou-Jie GUO, Chao ZHANG, Zhi-Sheng LI, Wei-Cong LI, Chang-Chun YANG. In⁃situ Electrochemical Preparation of Li⁃Na Alloy and the Co⁃storage of Li⁺ and Na⁺ Ions [J]. Chinese Journal of Applied Chemistry, 2022, 39(11): 1757-1765.
[15]	Hui LI, Zhen-Hua ZHU, Chen ZHAO, Jin-Kui TANG. Air‑stable High Performance Macrocyclic Dysprosium（Ⅲ） Single‑Ion Magnet [J]. Chinese Journal of Applied Chemistry, 2022, 39(10): 1586-1592.

Optimization of Preparation and Characterization of Copper Sulfate Pentahydrate Crystals

RichHTML

PDF

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 19

References 11

Related Articles 15

Recommended Articles

Metrics

Comments