Determination of Hexavalent Chromium in Refractories by Diphenylcarbazide Spectrophotometry

doi:10.19691/j.cnki.1004-4493.2021.03.006

China's Refractories ›› 2021, Vol. 30 ›› Issue (3): 28-32.DOI: 10.19691/j.cnki.1004-4493.2021.03.006

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Determination of Hexavalent Chromium in Refractories by Diphenylcarbazide Spectrophotometry

FU Yuanyuan¹^,^*(), HAN Junhua², CAO Haijie², LEI Xiaoyu², HAN Dan², XU Xiaoying²

1 CISDI Engineering Co., Ltd., Chongqing 400000, China
2 Sinosteel Luoyang Institute of Refractories Research Co., Ltd., Luoyang 471039, China

Online:2021-09-15 Published:2021-11-26
Contact: FU Yuanyuan
About author:Fu Yuanyuan was born in 1987 in Shaanxi Province, China. She majored in Chemistry and Bioinformatics and graduated from Sichuan University in 2015. She worked at the National Quality Supervision and Inspection Center for Refractories from 2015 to 2018, and is now working in CISDI Engineering Co., Ltd., engaging in refractory procurement.

Abstract

Abstract:

The high chrome refractories were crushed, ground into powder and sampled. A mixture solution of sodium carbonate and sodium hydroxide was used to extract the powder samples. The extracted solution from the samples was mixed and reacted with diphenylcarbazide to form colored substance. The hexavalent chromium content in the samples was determined by spectrophotometry. The effects of the extracting conditions, the color reagent reaction conditions, the sample mass, the working curve and the trivalent chromium coexistence on the results were studied. The experiments about determination, recovery and precision were carried out. The relative standard deviation was less than 5% and the recovery rate was 98%-104%.

Key words: refractories, hexavalent chromium, spectrophotometry

FU Yuanyuan, HAN Junhua, CAO Haijie, LEI Xiaoyu, HAN Dan, XU Xiaoying. Determination of Hexavalent Chromium in Refractories by Diphenylcarbazide Spectrophotometry[J]. China's Refractories, 2021, 30(3): 28-32.

Figures/Tables 9

References 14

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Method No.	Extracting steps	Cr⁶⁺content /(μg · g^-1)
1	150 mL mixed solution of 20 g/L NaOH and 30 g/L Na₂CO₃, boiling for 30 min	2.19
2	50 mL of water, 100 ℃, 30 min	1.26
3	50 mL of water, 80 ℃, 60 min	1.27
4	150 mL mixed solution of 20 g/L NaOH and 30 g/L Na₂CO₃, 90-95 ℃, 60 min	2.27
5	Room temperature, 60 min	0.65

Method No.	Extracting steps	Cr⁶⁺content /(μg · g^-1)
1	150 mL mixed solution of 20 g/L NaOH and 30 g/L Na₂CO₃, boiling for 30 min	2.19
2	50 mL of water, 100 ℃, 30 min	1.26
3	50 mL of water, 80 ℃, 60 min	1.27
4	150 mL mixed solution of 20 g/L NaOH and 30 g/L Na₂CO₃, 90-95 ℃, 60 min	2.27
5	Room temperature, 60 min	0.65

Mass of sample /g	Amount of extraction solution	Absorbance value	Cr⁶⁺content / (μg · g^-1)
1.004 7	1/4	0.536	341
2.000 0	1/8	0.525	336
3.006 4	1/20	0.327	348
4.007 0	1/20	0.437	349
5.006 0	1/20	0.537	343

Mass of sample /g	Amount of extraction solution	Absorbance value	Cr⁶⁺content / (μg · g^-1)
1.004 7	1/4	0.536	341
2.000 0	1/8	0.525	336
3.006 4	1/20	0.327	348
4.007 0	1/20	0.437	349
5.006 0	1/20	0.537	343

	Cr₂O₇^2-	CrO₄^2-	[Cr (H₂O₆)]³⁺ or Cr³⁺	[Cr (OH)]^-	[Cr (H₂O₆)]²⁺ or Cr²⁺
Valence states of chromium	+6	+6	+3	+3	+2
Color	Orange-red	Yellow	Purple	Bright green	Blue
pH	pH=2	pH=6	Acidic	Strong alkaline	Acidic

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Determination of Hexavalent Chromium in Refractories by Diphenylcarbazide Spectrophotometry

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Cr³⁺/μg	Cr⁶⁺/μg	Absorbance value	Recovered Cr⁶⁺/μg	Recovery rate /%
40	0	0.001	0.000 2	-
40	25	0.164	26	104
60	50	0.322	51	102
120	100	0.638	102	102
140	125	0.802	128	102

Equipment No.	Cr⁶⁺/μg	Absorbance value (x)	Working curve
Spectro- photometer 1^#	0	0.002	y = 0.160 0x+0.000 1 R²= 0.999 8
	10	0.063
	25	0.156
	50	0.307
	75	0.463
	100	0.623
	125	0.786
Spectro- photometer 2^#	0	0.003	y = 0.162 7x-0.000 1 R²= 0.999 7
	10	0.064
	25	0.156
	50	0.315
	75	0.466
	100	0.627
	125	0.764

Samples	Sample mass /g	Absorbance value	Cr⁶⁺ content /(μg · g^-1)	Mean Cr⁶⁺ content /(μg · g^-1) N=5
Industrial chromium oxide	5.003 2	0.515	329	328
Fused chromium oxide	5.007 8	0.434	280	276
Industrial chromium oxide	5.160 4	0.574	331	341
High chrome brick	4.983 9	0.173	113	115
High chrome brick	5.004 9	0.098	64	67
Magnesia chrome brick	5.000 8	0.116	74	72

Samples	Cr⁶⁺ content /(μg · g^-1) N=9	Standard deviation /(μg · g^-1)	Reletive standard deviation /%	Cr⁶⁺/μg	Recovered Cr⁶⁺/ μg	Recovery rate /%
Fused chromium oxide	340	4.84	1.4
High chrome brick	150	5.75	3.8
Pure chromium trioxide				5.00	4.94	98.8
Pure chromium trioxide				5.00	5.19	103.8

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