X射线荧光光谱法测定加氢精制催化剂中的镍、钼、钨和磷

doi:10.11962/1006-4990.2019-0650

Abstract

Abstract:

A series of standard samples with different component contents were prepared by simulating the composition of hydro-fining catalyst,and the matrix effect was corrected by empirical coefficient method.Then a method for the content determina-tion of nickel,molybdenum,tungsten and phosphorus in hydrofining catalysts was established by X-ray fluorescence spectro-metry.The determination range（mass fraction） is as follow：w（NiO）=1.92%~7.1%,w（MoO₃）=8.80%~13.69%,w（WO₃）=8.81%~14.50% and w（P₂O₅）=2.04%~6.96%.This method has high accuracy and precision that the correlation coefficients of the four quantitative calibration curves established by this method were all higher than 0.999 and the relative standard deviation of the determination result was less than 1%,which met the needs of scientific research and industrial production.

Key words: X-ray fluorescence spectrometry, hydrofining catalyst, nickel, molybdenum, tungsten

CLC Number:

TQ136.12

Wei Yuewen,Zhang Dandan,Qi Bangfeng. Determination of Ni, Mo, W and P in hydrofining catalysts by X-ray fluorescence spectrometry[J]. Inorganic Chemicals Industry, 2020, 52(11): 91-94.

Figures/Tables 13

References 11

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分析元素	分析线	2θ/ （°）	分析晶体	探测器	衰减器	计数时间/s	PHA
Ni	Kα	48.65	LiF（200）	S.C	1/1	20	50~550
Mo	Kα	20.32	LiF（200）	S.C	1/10	20	110~450
W	Lα	43.00	LiF（200）	S.C	1/1	20	60~535
P	Kα	141.21	GeH	P.C	1/1	20	105~280

标样编号	w（NiO）	w（MoO₃）	w（WO₃）	w（P₂O₅）	w（载体）
1	1.92	13.69	8.81	6.96	68.62
2	3.07	12.71	10.36	6.00	67.86
3	4.03	11.74	11.40	5.04	67.79
4	4.99	10.76	12.43	3.96	67.86
5	6.14	9.78	13.50	3.00	67.58
6	7.10	8.80	14.50	2.04	67.56
7	1.92	11.74	11.40	5.04	69.90
8	7.10	11.74	11.40	5.04	64.72
9	4.03	13.69	11.40	5.04	65.84
10	4.03	8.80	11.40	5.04	70.73
11	4.03	11.74	8.81	5.04	70.38
12	4.03	11.74	14.50	5.04	64.69
13	4.03	11.74	11.40	6.96	65.87
14	4.03	11.74	11.40	2.04	70.79

编号	w（NiO）/ %	MoO₃		WO₃		P₂O₅
编号	w（NiO）/ %	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps
1	1.92	11.74	401.27	11.40	570.57	5.04	88.28
2	4.03	11.74	385.26	11.40	504.39	5.04	90.51
3	7.10	11.74	356.90	11.40	441.57	5.04	84.96

编号	w（MO₃）/ %	NiO		WO₃		P₂O₅
编号	w（MO₃）/ %	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps
1	8.80	4.03	504.22	11.40	505.78	5.04	80.00
2	11.74	4.03	489.39	11.40	504.39	5.04	90.51
3	13.69	4.03	480.29	11.40	500.37	5.04	92.87

编号	w（WO₃）/ %	NiO		MO₃		P₂O₅
编号	w（WO₃）/ %	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps
1	8.81	4.03	504.21	11.74	435.85	5.04	90.85
2	11.40	4.03	489.39	11.74	385.26	5.04	90.51
3	14.50	4.03	447.87	11.74	336.14	5.04	82.62

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Determination of Ni, Mo, W and P in hydrofining catalysts by X-ray fluorescence spectrometry

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编号	w（P₂O₅）/ %	NiO		MO₃		WO₃
编号	w（P₂O₅）/ %	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps	质量分数/%	强度/ kcps
1	2.04	4.03	510.45	11.74	381.62	11.40	481.93
2	5.04	4.03	489.39	11.74	385.26	11.40	504.39
3	6.96	4.03	472.54	11.74	381.64	11.40	506.11

待测元素	线性范围/%	校准曲线方程	相关系数
Ni	1.92~7.1	I=3.21e^-3 C-0.21	0.999 9
Mo	8.80~13.69	I=7.18e^-3 C-0.55	0.999 5
W	8.81~14.50	I=1.36e^-2 C-2.28	0.999 1
P	2.04~6.96	I=4.36e^-2 C-0.034	0.999 0

样品质量/g	w（NiO）/%	w（MoO₃）/%	w（WO₃）/%	w（P₂O₅）/%
2.5	7.10	8.72	14.50	2.03
2.6	7.10	8.76	14.50	2.04
2.8	7.10	8.78	14.50	2.04
3.0	7.10	8.80	14.50	2.04
3.2	7.10	8.80	14.50	2.05
3.4	7.11	8.80	14.50	2.04
3.5	7.10	8.80	14.50	2.04

标样编号	待测元素	标准值	本方法测定值	标样编号	待测元素	标准值	本方法测定值
1	w（NiO）	1.92	1.90	6	w（WO₃）	14.50	14.65
	w（MoO₃）	13.69	13.41	6	w（P₂O₅）	2.04	2.03
	w（WO₃）	8.81	8.76	13	w（NiO）	4.03	4.02
	w（P₂O₅）	6.96	6.90		w（MoO₃）	11.74	11.72
6	w（NiO）	7.10	7.09		w（WO₃）	11.40	11.22
6	w（MoO₃）	8.80	8.68		w（P₂O₅）	6.96	6.99

样品名称	待测元素	本方法测定值	ICP法测定值	样品名称	待测元素	本方法测定值	ICP法测定值
RHYC-1	w（NiO）	5.17	5.04	RHYC-2	w（WO₃）	12.35	11.89
	w（MoO₃）	9.54	9.17	RHYC-2	w（P₂O₅）	2.49	2.36
	w（WO₃）	10.43	10.12	RHYC-3	w（NiO）	5.19	5.06
	w（P₂O₅）	2.38	2.16		w（MoO₃）	9.83	9.65
RHYC-2	w（NiO）	4.86	4.99		w（WO₃）	11.85	11.32
RHYC-2	w（MoO₃）	10.78	10.51		w（P₂O₅）	2.58	2.21

标样编号	待测元素	标准值	加标量	测定值	回收率
3	NiO	4.03	1.57	5.58	98.72
	MoO₃	11.74	1.60	13.30	97.50
	WO₃	11.40	1.70	13.15	102.94
	P₂O₅	5.04	1.20	6.28	103.33
4	NiO	4.99	1.57	6.53	98.09
	MoO₃	10.76	1.60	12.41	103.13
	WO₃	12.43	1.70	14.10	98.24
	P₂O₅	3.96	1.20	5.18	101.67

组分	X_r	X_R	S_r	S_R	RSD_r	RSD_R
NiO	7.104	7.102	0.68	0.95	0.10	0.13
MoO₃	8.806	8.802	0.98	1.03	0.11	0.12
WO₃	14.504	14.503	1.00	1.16	0.07	0.08
P₂O₅	2.041	2.043	0.76	0.83	0.37	0.41

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