Determination of Lithium, Iron and Phosphorus in Carbon Composite Lithium Iron Phosphate by Perchloric Acid Digestion-Inductively Coupled Plasma Optical Emission Spectrometry

Bin-bin ZHANG; Jing-bin LI; Shi-ning WANG; Peng-fei HE; Xiao-qin ZHA

doi:10.3964/j.issn.1000-0593(2021)09-2703-07

Spectroscopy and Spectral Analysis, Volume. 41, Issue 9, 2703(2021)

Determination of Lithium, Iron and Phosphorus in Carbon Composite Lithium Iron Phosphate by Perchloric Acid Digestion-Inductively Coupled Plasma Optical Emission Spectrometry

Bin-bin ZHANG^*, Jing-bin LI^{1; 2;}, Shi-ning WANG^{1; 2;}, Peng-fei HE^{1; 2;}, and Xiao-qin ZHA^{1; 2; 3;}

Author Affiliations

1. Luoyang Ship Material Research Institute, Luoyang 471023, China

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Figures & Tables(15)

Fig. 1. 30×picture of digestion solution after twice

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Fig. 1. 30×picture of digestion solution clarify visual

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Fig. 1. 20×picture of class two water

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Fig. 1. 20×picture of blank glass slide

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Fig. 2. Solvent blank intensity peak of Fe259.940 nm

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Fig. 2. Solvent blank intensity peak of Li610.365 nm

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Fig. 2. Solvent blank intensity peak of P178.222 nm

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Fig. 2. Solvent blank intensity peak of P213.618 nm

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Table 1. Chemical compound and analysis method of lithium iron phosphate

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Table 1. Chemical compound and analysis method of lithium iron phosphate

标准号	元素	化学成分/%	分析方法
	Li(除碳含量)	4.4±1.0	ICP-OES
GB/T 30835^[2]	Fe(除碳含量)	35.0±2.0	重铬酸钾滴定法
	P(除碳含量)	20.0±1.0	磷钼酸铵容量法
	Li	4.3±0.3	ICP-OES
GB/T 33822^[3]	Fe	34.0±2.0	电位滴定法
	P	19.5±1.5	喹钼柠酮重量法
	Li	3.9~5.0	火焰光度法
YS/T 1027^[4,5,6]	Fe	33~36	重铬酸钾滴定法
	P	18~20	磷钼酸喹啉称量法

Table 2. Digestion conditions of sample
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Table 2. Digestion conditions of sample
消解试剂消解情况
12 mL王水黑色不溶物
9 mL HCl+1 mL H₂SO₄ 少量黑色不溶物
12 mL王水+1 mL H₂SO₄ 少量黑色不溶物
5 mL HClO₄ 消解完全
5 mL H₂SO₄ 消解完全

Table 3. Parameters of ICP-OES
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Table 3. Parameters of ICP-OES
编号高频功率
/kW 雾化器流量
/(L·min^-1) 观测方向观测高度
/mm
1 1.2 0.7 轴向 /
2 8
3 径向 12
4 15
5 1.3 0.6 轴向 /
6 8
7 径向 12
8 15
9 1.1 0.8 轴向 /
10 8
11 径向 12
12 15

Table 4. Test results of sample under the different parameters

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Table 4. Test results of sample under the different parameters

条件序号	元素	线性系数	检测结果/%	平均值 /%		RSD/% n=7
1	Fe259.940	0.997 1	34.312; 34.757; 34.752; 34.675; 34.837; 34.855; 34.597	34.68		0.538
	Li610.365	0.999 3	4.524; 4.605; 4.623; 4.628; 4.602; 4.569; 4.600	4.593		0.782
	P178.222	0.998 0	19.247; 19.360; 19.663; 19.489; 19.583; 19.581; 19.524	19.49		0.737
	P213.618	0.998 0	19.125; 19.471; 19.629; 19.517; 19.482; 19.420; 19.437	19.44		0.797
2	Fe259.940	0.998 9	34.172; 34.409; 34.438; 34.685; 34.884; 34.926; 35.036	34.65		0.922
	Li610.365	0.998 8	5.119; 5.116; 5.099; 5.122; 5.137 5.181; 5.151	5.132		0.528
	P178.222		线性系数r<0.995 0
	P213.618	0.998 5	19.073; 19.107; 19.061; 19.078; 19.238; 19.078; 19.248	19.12		0.424
3	Fe259.940	0.998 6	35.219; 35.272; 35.388; 35.304; 35.080; 35.513; 35.753	35.36		0.619
	Li610.365	0.998 1	5.279; 5.290; 5.345; 5.315; 5.272; 5.380; 5.363	5.321		0.804
	P178.222		线性系数r<0.995 0
	P213.618	0.998 6	19.714; 19.698; 19.775; 19.739; 19.633; 19.945; 19.831	19.76		0.514
4	Fe259.940	0.999 4	35.321; 35.193; 34.731; 34.734; 34.670; 34.453; 34.362	34.78		1.02
	Li610.365	0.999 0	5.433; 5.416; 5.381; 5.369; 5.390; 5.300; 5.254	5.362		1.20
	P178.222		线性系数r<0.995 0
	P213.618	0.999 8	19.735; 19.583; 19.204; 19.355; 19.193; 19.198; 19.107	19.34		1.21
5	Fe259.940	0.998 0	34.759; 34.853; 34.794; 34.693; 34.676; 34.272; 34.678		34.68		0.547
	Li610.365	0.999 1	4.840; 4.843; 4.786; 4.795; 4.758; 4.717; 4.759		4.785		0.954
	P178.222	0.998 2	19.102; 19.209; 19.144; 19.150; 19.013; 18.080 4; 19.951		19.20		1.87
	P213.618	0.998 3	19.125; 19.471; 19.629; 19.517; 19.482; 19.420; 19.437		19.44		0.797
6	Fe259.940	0.998 1	34.193; 34.299; 34.315; 34.349; 34.225; 34.158; 34.124		34.24		0.249
	Li610.365		线性系数r<0.995 0
	P178.222		线性系数r<0.995 0
	P213.618	0.998 4	18.562; 18.591; 18.515; 18.325; 18.313; 18.101; 18.244		18.38		0.993
7	Fe259.940	0.998 8	34.121; 34.561; 34.401; 34.432; 34.167; 34.054; 33.287		34.22		0.743
	Li610.365		线性系数r<0.995 0
	P178.222		线性系数r<0.995 0
	P213.618	0.998 5	18.889; 19.066; 19.825; 18.933; 18.782; 18.626; 18.457		18.80		1.08
8	Fe259.940	0.999 3	34.370; 34.391; 34.579; 34.341; 34.359; 34.403; 34.262		34.39		0.281
	Li610.365		线性系数r<0.995 0
	P178.222		线性系数r<0.995 0
	P213.618	0.999 5	19.042; 19.031; 19.168; 18.935; 19.004; 18.948; 19.028		19.02		0.403
9	Fe259.940	0.998 4	35.940; 35.969; 36.111; 36.254; 36.327; 36.226; 36.179		36.14		0.402
	Li610.365	0.999 8	4.573; 4.600; 4.617; 4.610; 4.624; 4.631; 4.632		4.612		0.451
	P178.222	0.999 3	20.502; 20.409; 20.880; 20.970; 20.675; 20.761; 20.888		20.73		1.01
	P213.618	0.999 1	20.185; 20.336; 20.393; 20.403; 20.464; 20.450; 20.417		20.38		0.465
9	Fe259.940	0.999 6	35.621; 35.876; 35.935; 36.340; 36.500; 36.592; 36.829		36.24		1.21
	Li610.365	0.999 3	4.910; 4.969; 5.003; 5.054; 5.076; 5.083; 5.146		5.034		1.57
	P178.222		线性系数r<0.995 0
	P213.618	0.999 6	19.829; 19.922; 20.043; 20.294; 20.150; 20.261; 20.444		20.14		1.08
11	Fe259.940	0.999 4	35.154; 35.295; 35.304; 35.346; 35.616; 35.473; 35.793		35.43		0.616
	Li610.365	0.999 5	4.889; 4.840; 4.855; 4.861; 4.896; 4.856; 4.922		4.874		0.594
	P178.222		线性系数r<0.995 0
	P213.618	0.999 4	19.600; 19.575; 19.725; 19.653; 19.951; 19.782; 19.859		19.74		0.701
12	Fe259.940	0.999 0	34.898; 34.874; 35.134; 35.263; 35.362; 35.532; 35.770		35.26		0.926
	Li610.365	0.999 2	4.838; 4.792; 4.813; 4.848; 4.852; 4.873; 4.882		4.843		0.656
	P178.222		线性系数r<0.995 0
	P213.618	0.999 3	19.568; 19.522; 19.558; 19.495; 19.776; 19.859; 19.998		19.68		0.992

Table 5. Calibration curve & RSD of method

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Table 5. Calibration curve & RSD of method

元素	分析谱线 /nm	线性范围 /(μg·mL^-1)	检出限 /(μg·mL^-1)	线性回归方程	相关系数	RSD/% (n=7)
Li	610.365	1.00~9.00	0.030	y=70 044.439 814 63x+76.311 870 12	0.999 9	0.353
Fe	259.940	20.0~40.0	0.020	y=1 688.372 295 67x+531.221 606 48	0.999 4	0.616
P	178.222	10.0~30.0	0.022	y=130.354 403 64x+6.919 913 16	0.999 3	1.01
P	213.618	10.0~30.0	0.038	y=219.349 601 58x+19.366 530 67	0.999 4	0.701

Table 6. Test result of standard recovery rate

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Table 6. Test result of standard recovery rate

元素	分析谱线/nm	本底值/%	加标量/μg(Wt%)	测定值/%	回收率/%
Li	610.365	4.612	100(1.00%)	5.684	107
			300(3.00%)	7.815	107
			500(5.00%)	9.953	107
Fe	259.940	35.43	100(1.00%)	36.36	93.6
			300(3.00%)	38.16	91.2
			500(5.00%)	40.62	104
P	178.222	19.49	100(1.00%)	20.61	112
			300(3.00%)	22.58	103
			500(5.00%)	24.96	109
	213.618	19.74	100(1.00%)	20.74	101
			300(3.00%)	23.04	110
			500(5.00%)	24.70	99.3

Table 7. Test result of IRR

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Table 7. Test result of IRR

分析谱线/nm	测定值/%	平均值/%	F统计量	双尾截尾概率P值
Li 610.365	A: 4.56; 4.62; 4.55; 4.58	A: 4.58	0.197	0.442
Li 610.365	B: 4.55; 4.71; 4.58; 4.60	B: 4.61	0.197	0.442
Fe 259.940	A: 34.72; 34.78; 34.46; 34.88	A: 34.71	0.307	0.067
Fe 259.940	B: 34.87; 35.61; 35.03; 35.05	B: 35.14	0.307	0.067
P 178.222	A: 19.65; 19.90; 19.59; 19.75	A: 19.72	0.310	0.636
P 178.222	B: 19.51; 20.05; 19.68; 19.93	B: 19.79	0.310	0.636
P 213.618	A: 19.43; 19.41; 19.17; 19.34	A: 19.34	0.763	0.188
P 213.618	B: 19.40; 19.39; 19.49; 19.48	B: 19.44	0.763	0.188

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Bin-bin ZHANG, Jing-bin LI, Shi-ning WANG, Peng-fei HE, Xiao-qin ZHA. Determination of Lithium, Iron and Phosphorus in Carbon Composite Lithium Iron Phosphate by Perchloric Acid Digestion-Inductively Coupled Plasma Optical Emission Spectrometry[J]. Spectroscopy and Spectral Analysis, 2021, 41(9): 2703

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