Determination of Phosphorus in Welding Flux by Inductively Coupled Plasma Atomic Emission Spectrometry With Ultrasonic Assisted Hydrochloric Acid Extraction

Pan LIU; Jing-bin LI; Jian-hao ZHANG; Yi ZHANG; Guo-liang CHANG; Peng-fei HE; Bin-bin ZHANG; Xin-yao ZHANG

doi:10.3964/j.issn.1000-0593(2022)09-2824-06

Journals >Spectroscopy and Spectral Analysis >Volume 42 >Issue 9 >Page 2824 > Article

Spectroscopy and Spectral Analysis
Vol. 42, Issue 9, 2824 (2022)

Determination of Phosphorus in Welding Flux by Inductively Coupled Plasma Atomic Emission Spectrometry With Ultrasonic Assisted Hydrochloric Acid Extraction

Pan LIU^{1; 2;}, Jing-bin LI^1;, Jian-hao ZHANG^1;, Yi ZHANG^1;, Guo-liang CHANG^1;, Peng-fei HE^1;, Bin-bin ZHANG^1;, and Xin-yao ZHANG^{1; 3;}

Author Affiliations

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

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DOI: 10.3964/j.issn.1000-0593(2022)09-2824-06 Cite this Article

Pan LIU, Jing-bin LI, Jian-hao ZHANG, Yi ZHANG, Guo-liang CHANG, Peng-fei HE, Bin-bin ZHANG, Xin-yao ZHANG. Determination of Phosphorus in Welding Flux by Inductively Coupled Plasma Atomic Emission Spectrometry With Ultrasonic Assisted Hydrochloric Acid Extraction[J]. Spectroscopy and Spectral Analysis, 2022, 42(9): 2824 Copy Citation Text

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Fig. 1. Effect of spectral parameters on intensity
(a): Radio frequency power; (b): Nebulization gas flow; (c): Auxiliary gas flow; (d) Plasma gas flow

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Fig. 2. Typical analytical spectrum of calibration solution (a) and actual sample solution (b)

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波长/nm	强度	干扰元素	备注
213.618	1 550.9	Cu 213.598 nm, W 213.639 nm, Mo 213.606 nm	-
214.914	504.1	Ni 214.780 nm, W 214.917 nm, Fe 214.919 nm	-
178.222	285.7	-	紫外区, 需惰性气体高速吹扫
177.434	436.5	Ni 177.341 nm	紫外区, 需惰性气体高速吹扫

Table 1. Analytical lines of phosphorus

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编号	测定值/%(n=6~10)	平均值 /%	RSD /%	参考值 /%	偏倚 /%
WF804	0.012 3, 0.012 8, 0.012 4, 0.012 0, 0.012 2, 0.012 4, 0.012 8, 0.012 7, 0.013 0, 0.012 8	0.012 5	2.6	0.012^a	0.000
CHF-105R(1^#)	0.014 7, 0.014 0, 0.014 5, 0.014 7, 0.014 3, 0.014 4, 0.014 3, 0.014 4, 0.014 8, 0.014 8	0.014 5	1.8	0.014^a	0.000
705-ch(1^#)	0.021 1, 0.021 2, 0.022 2, 0.020 3, 0.020 5, 0.020 4, 0.020 5, 0.020 5, 0.019 9, 0.020 5	0.020 7	3.1	0.020^a	+0.001
705-ch(2^#)	0.012 8, 0.012 3, 0.011 7, 0.011 3, 0.013 0, 0.012 1, 0.012 7, 0.012 9, 0.012 5, 0.012 9	0.012 4	4.6	0.011^a	+0.001
焊条药皮8080	0.002 8, 0.002 5, 0.002 8, 0.002 5, 0.002 6, 0.003 0, 0.002 6, 0.003 1, 0.003 0, 0.002 8	0.002 8	7.1	0.003 1^a	-0.000 3
705-ch(7^#)	0.011 4, 0.011 0, 0.010 9, 0.011 7, 0.011 0, 0.012 0, 0.012 0, 0.012 6, 0.011 9, 0.012 1	0.011 7	4.9	0.010^a	+0.002
705-ch(4^#)	0.016 1, 0.017 2, 0.015 6, 0.016 8, 0.017 3, 0.017 2, 0.017 3, 0.018 0, 0.014 9, 0.018 9	0.016 9	6.8	0.016^a	+0.001
705-ch(6^#)	0.016 0, 0.016 9, 0.016 4, 0.015 6, 0.015 8, 0.016 7, 0.015 9, 0.016 4, 0.016 9, 0.014 7	0.016 1	4.2	0.018^a	-0.002
CHF-105R(2^#)	0.013 8, 0.013 8, 0.013 8, 0.013 9, 0.013 8, 0.013 9, 0.014 2, 0.013 6, 0.014 2, 0.014 2	0.013 9	1.5	0.015^a	-0.001
SJ208DR	0.004 8, 0.005 0, 0.004 9, 0.004 6, 0.004 8, 0.004 7, 0.005 1, 0.004 9, 0.005 0, 0.004 8	0.004 9	3.1	0.003 2^a	+0.001 7
SJ101DR	0.025 6, 0.025 8, 0.025 5, 0.026 1, 0.026 0, 0.025 5, 0.025 8, 0.025 9, 0.025 9, 0.025 6	0.025 8	0.8	0.028^a	-0.002
GSBJ33003—92	0.022 1, 0.021 6, 0.021 5, 0.021 4, 0.021 2, 0.022 0, 0.021 5, 0.021 8, 0.021 8, 0.022 1	0.021 7	1.4	0.022^b	0.000
GSBJ33001—92	0.023 2, 0.023 0, 0.023 1, 0.022 7, 0.023 0, 0.022 8, 0.022 8, 0.022 7	0.022 9	0.8	0.024^b	-0.001
YSBC11801—2006	0.005 0, 0.005 1, 0.004 7, 0.005 0, 0.004 6, 0.005 0	0.004 9	4.1	0.005 2^b	-0.000 3
YSBC11802—2006	0.002 8, 0.002 6, 0.002 8, 0.003 0, 0.002 6, 0.002 8	0.002 8	5.4	0.003 2^b	-0.000 4

Table 2. Determination results of phosphorus in actual sample and certified reference materials of welding fluxes

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编号	本底量/μg	加标量/μg	测得总量/μg	回收量/μg	回收率/%
705-ch(1^#)	10.86	5.00	15.83, 16.13, 15.75, 15.83	4.97, 5.27, 4.89, 4.97	99.4, 105.4, 97.9, 99.4
705-ch(2^#)	6.38	5.00	11.25, 11.48, 11.33, 11.40	4.87, 5.09, 4.94, 5.02	97.3, 101.8, 98.8, 100.3
CHF-105R(1^#)	7.36	5.00	12.60, 12.60, 12.83, 12.53	5.24, 5.24, 5.46, 5.16	104.7, 104.7, 109.2, 103.2
WF804	6.44	5.00	11.85, 11.63, 11.48, 11.48	5.41, 5.18, 5.03, 5.03	108.1, 103.6, 100.6, 100.6
GSBJ33003—92	10.87	5.00	16.35, 16.20, 16.35, 16.28	5.48, 5.33, 5.48, 5.40	109.6, 106.6, 109.6, 108.1
YSBC11801—2006	2.44	5.00	7.65, 7.58, 7.50, 7.65	5.21, 5.14, 5.06, 5.21	104.2, 102.7, 101.2, 104.2
YSBC11802—2006	2.09	5.00	6.75, 6.83, 7.05, 6.90	4.66, 4.73, 4.96, 4.81	93.2, 94.7, 99.2, 96.2

Table 3. Recovery rate test results

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