电感耦合等离子发射光谱法测定氧化铁颜料中微量镉

doi:10.3969/j.issn.1001-1803.2020.03.013

Abstract

Abstract:

Cd214.439, Cd226.502 and Cd228.802, commonly used in determination of cadmium in ferric oxide pigments by ICP-OES, are interfered by the iron spectrum. By using rhodium as the internal standard, the interference at these three spectral lines in the mass concentration range of 0-20.0 g/L of iron was studied. The results showed that, iron interfered most at Cd226.502, next at Cd214.439, and least at Cd228.802. The interference values ranged from 0.130-1.430 mg/L, 0.031-0.329 mg/L, and 0.005-0.025 mg/L, respectively. At Cd226.502 and Cd214.439, the interference intensity grew with the increase of iron mass concentration, but not so much at Cd228.802. Finally, Cd228.802 was selected for screening analysis. The sample was weighed as 0.500 g, which could be judged as qualified when the test result was less than or equal to 5.0 mg/kg, and unqualified when the test result was more than 6.2 mg/kg. Only when the test result was somewhere in between, other methods would be used for analysis and confirmation. Therefore, the selection of Cd228.802 for analysis could greatly improve the screening efficiency.

Key words: ICP-OES, ferric oxide pigment, cosmetic, cadmium

CLC Number:

TQ658

Hao-jie HUANG,Fei-fei XU. Determination of cadmium in ferric oxide pigments by ICP-OES[J].China Surfactant Detergent & Cosmetics, 2020, 50(3): 208-212.

Figures/Tables 11

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References 9

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温度/℃	升温时间/min	保持时间/min
120	5	3
160	5	3
180	5	20

ρ（铁）/（g·L^-1）	6次检测干扰值/（mg·L^-1）						干扰平均值/ （mg·L^-1）	0.500 g样品干扰值/ （mg·kg^-1）
0	-0.000 3,	-0.000 9,	-0.000 7,	-0.000 1,	-0.000 8,	-0.000 6	-0.000 6	-0.03
2.0	0.029,	0.031,	0.031,	0.031,	0.032,	0.031	0.031	1.5
4.0	0.061,	0.059,	0.055,	0.062,	0.062,	0.060	0.060	3.0
8.0	0.120,	0.129,	0.128,	0.127,	0.123,	0.128	0.126	6.3
12.0	0.179,	0.187,	0.184,	0.176,	0.180,	0.187	0.182	9.1
16.0	0.249,	0.251,	0.224,	0.232,	0.244,	0.250	0.242	12.1
20.0	0.336,	0.310,	0.323,	0.343,	0.339,	0.320	0.329	16.4

ρ（铁）/（g·L^-1）	6次检测干扰值/（mg·L^-1）						干扰平均值/ （mg·L^-1）	0.500 g样品干扰值/（mg·kg^-1）
0	-0.000 4,	-0.000 1,	-0.000 1,	0.000 2,	-0.000 4,	-0.000 2	-0.000 2	-0.01
2.0	0.128,	0.127,	0.132,	0.127,	0.135,	0.132	0.130	6.5
4.0	0.235,	0.252,	0.229,	0.250,	0.236,	0.246	0.241	12.1
8.0	0.507,	0.523,	0.525,	0.530,	0.493,	0.522	0.517	25.8
12.0	0.831,	0.813,	0.772,	0.752,	0.762,	0.772	0.784	39.2
16.0	1.02,	1.01,	0.939,	0.981,	1.02,	1.05	1.00	50.2
20.0	1.47,	1.36,	1.40,	1.39,	1.50,	1.46	1.43	71.5

ρ（铁）/（g·L^-1）	6次检测干扰值/（mg·L^-1）						干扰平均值/ （mg·L^-1）	0.500 g样品干扰值/（mg·kg^-1）
0	-0.003 1,	-0.001 3,	-0.001 6,	-0.001 8,	-0.003 1,	-0.002 7	-0.002 3	-0.11
2.0	0.006,	0.003,	0.005,	0.005,	0.004,	0.006	0.005	0.2
4.0	0.021,	0.027,	0.032,	0.026,	0.023,	0.019	0.025	1.2
8.0	0.017,	0.023,	0.017,	0.022,	0.025,	0.019	0.021	1.0
12.0	0.017,	0.020,	0.019,	0.018,	0.019,	0.016	0.018	0.9
16.0	0.031,	0.023,	0.017,	0.024,	0.024,	0.030	0.025	1.2
20.0	0.022,	0.025,	0.018,	0.025,	0.025,	0.022	0.023	1.1

基体	内标比率/%	ρ（未校正）/ （mg·L^-1）	ρ（校正）/ （mg·L^-1）
镉标准溶液	105	0.103	0.098
氧化铁（无填料）	92	0.093	0.101
云母氧化铁	87	0.088	0.101
珠光氧化铁	80	0.084	0.104

Determination of cadmium in ferric oxide pigments by ICP-OES

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样品编号	Cd228.802	Cd214.439	Cd226.502	判定
1	0.8	4.1	17.9	合格
2	0.9	4.7	21.4	合格
3	1.1	5.9	23.6	合格
4	0.7	4.9	19.2	合格
6	0.2	3.3	14.9	合格

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ρ（铁）/（g·L^-1）	加标量/（mg·L^-1）	平均回收量/（mg·L^-1）	回收率/%	RSD/%
0	0.10	0.098	98	0.8
8.0	0.10	0.121	121	2.8
20.0	0.10	0.125	125	2.3