Development of Analytical Method for Determination of Inorganic Constituents in Powder Refreshment Using Dilute Mineral Acids and Detection by ICP OES

Santos, Samir H.; Costa, Silvânio S. L.; Souza, Sidnei O.; Garcia, Karina S.; Soares, Sarah A. R.; Garcia, Carlos A. B.; Almeida, Tarcísio S.; Araujo, Rennan G. O.

doi:10.21577/0103-5053.20210034

Samir H. Santos

Instituto de Química, Universidade Federal da Bahia, Campus Universitário Ondina, 40170-115 Salvador-BA, Brazil

Silvânio S. L. Costa

Instituto de Química, Universidade Federal da Bahia, Campus Universitário Ondina, 40170-115 Salvador-BA, Brazil

Núcleo de Petróleo, Gás e Biocombustíveis, Universidade Federal de Sergipe, Campus São Cristóvão, 49100-000 São Cristóvão-SE, Brazil

Sidnei O. Souza

Instituto de Química, Universidade Federal da Bahia, Campus Universitário Ondina, 40170-115 Salvador-BA, Brazil

Universidade Federal de Sergipe, Campus Lagarto, 49400-000 Lagarto-SE, Brazil

Karina S. Garcia

Instituto de Geociências, Universidade Federal da Bahia, 40170-115 Salvador-BA, Brazil

Sarah A. R. Soares

Instituto de Geociências, Universidade Federal da Bahia, 40170-115 Salvador-BA, Brazil

Carlos A. B. Garcia

Departamento de Química, Universidade Federal de Sergipe, Campus São Cristóvão, 40100-000 São Cristóvão-SE, Brazil

Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador-BA, Brazil

Tarcísio S. Almeida

Instituto de Química, Universidade Federal da Bahia, Campus Universitário Ondina, 40170-115 Salvador-BA, Brazil

Departamento de Ciências Exatas, Universidade Estadual de Feira de Santana, 44036-900 Feira Santana-BA, Brazil

Rennan G. O. Araujo ^**e-mail: rgoa01@terra.com.br, rennan@ufba.br

Instituto de Química, Universidade Federal da Bahia, Campus Universitário Ondina, 40170-115 Salvador-BA, Brazil

Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador-BA, Brazil

https://orcid.org/0000-0001-6955-8115

*e-mail: rgoa01@terra.com.br, rennan@ufba.br

Author Contributions

Samir H. Santos was responsible for the conceptualization, formal analysis, investigation, methodology, validation, and writing original draft; Silvanio S. L. Costa for the conceptualization, formal analysis, methodology and validation; Sidnei O. Souza for the methodology, validation and software; Karina S. Garcia for methodology and supervision; Sarah A. R. Soares for the methodology, supervision, and writing original draft; Carlos A. B. Garcia for the methodology and supervision; Tarcísio S. Almeida for the supervision, writing review and editing; Rennan G. O. Araujo for the writing review and editing, supervision and project administration.

Experiment	Coded (real value)					Concentration value											MR
Experiment	[HNO₃] / (mol L^-1)	[H₂O₂] / (% m m^-1)	HF / (mol L^-1)	Temperature / °C	time / min	Na / %	Al / (µg g^-1)	Ba / (µg g^-1)	K / (µg g^-1)	Ca / (µg g^-1)	Zn / (µg g^-1)	Ti / (µg g^-1)	Sr / (µg g^-1)	Mn / (µg g^-1)	Mg / (µg g^-1)	Fe / (µg g^-1)	MR
1	-1 (1.0)	-1 (1.0)	-1 (0.0)	-1 (150)	+1 (120)	19.6	6.03	14.7	307	3366	0.413	0.00	6.02	0.536	202	302	7.23
2	+1 (3.0)	-1 (1.0)	-1 (0.0)	-1 (150)	-1 (60)	20.9	7.77	15.7	309	3375	0.221	0.00	5.87	0.500	204	309	7.21
3	-1 (1.0)	+1 (4.0)	-1 (0.0)	-1 (150)	-1 (60)	20.1	8.57	15.8	354	3553	0.147	0.00	6.38	0.414	207	262	7.17
4	+1 (3.0)	+1 (4.0)	-1 (0.0)	-1 (150)	+1 (120)	19.1	8.94	15.1	307	3450	0.294	0.00	6.14	0.497	204	303	7.23
5	-1 (1.0)	-1 (1.0)	+1 (2.74)	-1 (150)	-1 (60)	18.1	29.82	14.7	320	3667	0.791	57.8	6.57	0.521	218	304	9.46
6	+1 (3.0)	-1 (1.0)	+1 (2.74)	-1 (150)	+1 (120)	18.9	26.52	15.1	314	3630	0.583	59.9	6.60	0.902	219	356	9.82
7	-1 (1.0)	+1 (4.0)	+1 (2.74)	-1 (150)	+1 (120)	18.8	29.97	15.5	338	3878	0.781	62.2	6.93	0.518	223	285	9.73
8	+1 (3.0)	+1 (4.0)	+1 (2.74)	-1 (150)	-1 (60)	21.1	28.46	15.8	323	3759	0.846	57.9	6.62	0.580	217	331	9.85
9	-1 (1.0)	-1 (1.0)	-1 (0.0)	+1 (190)	-1 (60)	21.4	20.67	17.4	357	3911	0.458	0.00	6.77	0.596	224	313	8.57
10	+1 (3.0)	-1 (1.0)	-1 (0.0)	+1 (190)	+1 (120)	20.8	13.52	15.8	324	3595	0.877	0.00	6.44	0.492	207	305	8.15
11	-1 (1.0)	+1 (4.0)	-1 (0.0)	+1 (190)	+1 (120)	22.1	9.58	16.5	327	3503	0.472	0.00	6.36	0.587	205	265	7.72
12	+1 (3.0)	+1 (4.0)	-1 (0.0)	+1 (190)	-1 (60)	18.3	11.42	16.5	277	3445	0.557	0.00	6.01	0.456	196	260	7.29
13	-1 (1.0)	-1 (1.0)	+1 (2.74)	+1 (190)	+1 (120)	21.8	11.47	15.9	305	3580	0.559	57.7	4.50	0.376	188	221	8.00
14	+1 (3.0)	-1 (1.0)	+1 (2.74)	+1 (190)	-1 (60)	20.3	22.09	15.1	301	3427	0.570	49.2	6.20	0.534	201	315	8.80
15	-1 (1.0)	+1 (4.0)	+1 (2.74)	+1 (190)	-1 (60)	19.5	22.94	14.8	305	3317	0.477	47.2	5.88	0.411	198	278	8.34
16	+1 (3.0)	+1 (4.0)	+1 (2.74)	+1 (190)	+1 (120)	19.1	24.59	14.3	287	3266	0.950	50.2	5.80	0.468	196	299	8.86
17	0 (2.0)	0 (2.5)	0 (1.37)	0 (170)	0 (90)	18.7	28.04	14.0	283	3357	0.821	58.5	5.70	0.365	202	250	8.73
18	0 (2.0)	0 (2.5)	0 (1.37)	0 (170)	0 (90)	18.3	20.85	14.1	297	3126	0.796	54.8	5.48	0.406	192	255	8.35
19	0 (2.0)	0 (2.5)	0 (1.37)	0 (170)	0 (90)	18.3	19.91	13.9	282	3135	0.789	48.3	5.48	0.383	198	268	8.20

Element	LOD / (µg g^-1)	LOQ / (µg g^-1)	Recovery / %	Element	LOD / (µg g^-1)	LOQ / (µg g^-1)	Recovery / %
Al	3.7	12	(80.0 ± 0.9)-(112 ± 2)	Mg	0.40	1.2	(100 ± 3)-(105 ± 1)
As	0.90	3.0	(105 ± 1)-(118 ± 4)	Mn	0.030	0.10	(92 ± 2)-(103 ± 2)
Ba	0.010	0.020	(92 ± 2)-(102 ± 3)	Na	1.1	3.8	(85 ± 5)-(109 ± 4)
Be	0.010	0.020	(100 ± 2)-(108 ± 1)	Ni	0.10	0.30	(96 ± 2)-(105.4 ± 0.6)
Bi	0.50	1.7	(92 ± 4)-(100 ± 4)	P	0.80	2.7	(92 ± 6)-(114 ± 2)
Ca	1.6	5.2	(81 ± 3)-(108 ± 3)	Pb	0.70	2.2	(93.9 ± 0.8)-(104.6 ± 0.3)
Cd	0.10	0.20	(106 ± 2)-(116 ± 1)	S	2.8	9.4	(98 ± 3)-(115 ± 4)
Co	0.050	0.20	(89 ± 2)-(95 ± 1)	Sn	0.70	2.4	(94 ± 2)-(101 ± 1)
Cr	0.10	0.20	(98 ± 2)-(108 ± 2)	Sr	0.10	0.40	(100 ± 2)-(111.2 ± 0.4)
Cu	0.20	0.60	(97 ± 1)-(106 ± 1)	Ti	0.10	0.30	(106 ± 11)-(119 ± 3)
Fe	0.46	1.5	(95 ± 8)-(109 ± 5)	V	0.030	0.10	(96 ± 2)-(104.4 ± 0.8)
K	11	36	(85 ± 1)-(105 ± 4)	Zn	0.20	0.80	(102 ± 2)-(113 ± 1)

CRM	Element	Certified value / (µg g^-1)	Found value / (µg g^-1)	Agreement / %	Element	Certified value / (µg g^-1)	Found value / (µg g^-1)	Agreement / %
NIST 1515	Al	284.5 ± 5.8	239 ± 25	84.0 ± 8.8	Mn	54.1 ± 1.1	44.4 ± 1.3	82.1 ± 2.4
	Ba	48.8 ± 2.3	46.9 ± 2.9	96.1 ± 5.9	Ni	0.936 ± 0.094	0.95 ± 0.02	101.5 ± 2.1
	Ca	15250 ± 100	14682 ± 300	96.3 ± 2.0	P	1593 ± 68	1423 ± 38.4	89.3 ± 2.4
	Fe	82.7 ± 2.6	95 ± 1.5	115 ± 1.8	S	(1800)	1883 ± 145	104.6 ± 8.0
	K	16080 ± 210	16676 ± 451	103.7 ± 2.8	Zn	12.45 ± 0.43	12.2 ± 0.7	98.0 ± 5.6
	Mg	2710 ± 120	2437 ± 53	89.9 ± 2.0
NIST 1547	Al	248.9 ± 6.5	292 ± 60	117 ± 24	K	24330 ± 380	20120 ± 67	82.7 ± 0.3
	Ba	123.7 ± 5.5	107 ± 11	86.5 ± 8.9	Mg	4320 ± 150	4016 ± 287	93.0 ± 6.6
	Ca	15590 ± 160	13354 ± 38	85.6 ± 0.2	Mn	97.8 ± 1.8	84.8 ± 5.5	86.7 ± 5.6
	Cd	0.0261 ± 0.0022	< 0.2	n.d.	Ni	0.689 ± 0.095	0.64 ± 0.03	92.8 ± 4.3
	Cr	(1.00)	1.1 ± 0.01	110 ± 1.0	P	1371 ± 82	1304 ± 37	95.1 ± 2.7
	Cu	3.75 ± 0.37	3.18 ± 0.05	84.8 ± 1.3	S	(2000)	1830 ± 153	91.5 ± 7.6
	Fe	219.8 ± 6.8	204 ± 7.3	92.8 ± 3.3	Zn	17.97 ± 0.53	16.5 ± 0.7	91.8 ± 3.9
CRM-Agro C100-3a	As	19.0 ± 2.8	15.3 ± 0.04	80.5 ± 0.2	Mn	470 ± 69	408 ± 8.4	86.8 ± 1.8
	Cd	26.6 ± 2.1	28.2 ± 0.86	106.0 ± 3.2	Na	2710 ± 840	3071 ± 226	113 ± 8.3
	Cr	6.7 ± 1.5	6.25 ± 0.1	93.3 ± 1.5	Ni	3.16 ± 0.87	3.16 ± 0.18	100 ± 5.7
	Cu	1130 ± 140	1003 ± 32	88.8 ± 2.8	P	4370 ± 740	4779 ± 134	109.4 ± 3.0
	Fe	1120 ± 190	1041 ± 16	92.9 ± 1.4	Zn	37.5 ± 5.0	36.2 ± 1.5	96.5 ± 4.0
	Mg	4110 ± 360	3769 ± 120	91.7 ± 2.9
NCS DC 73351	Al	(0.3%)	(0.220 ± 0.001)	73.3 ± 0.3	K	(1.66 ± 0.12)	(1.62 ± 0.02)	97.6 ± 1.2
	Ba	58 ± 6	54.6 ± 1.3	94.1 ± 2.2	Mg	(0.17 ± 0.02)	(0.16 ± 0.002)	94.1 ± 1.2
	Ca	0.43 ± 0.04%	0.400 ± 0.005%	93.0 ± 1.2	Mn	1240 ± 70	1096 ± 26	88.4 ± 2.1
	Cd	0.057 ± 0.010	< 0.2	n.d.	Ni	4.6 ± 0.5	4.10 ± 0.1	89.1 ± 2.2
	Cr	0.80 ± 0.03	0.78 ± 0.02	97.5 ± 2.5	P	2840 ± 90	2760 ± 77	97.2 ± 2.7
	Cu	17.3 ± 1.8	14.0 ± 0.1	81.0 ± 0.6	S	(0.245 ± 0.022)	(0.254 ± 0.002)	103.7 ± 0.8
	Fe	264 ± 15	238 ± 5.4	90.2 ± 2.0	Zn	26.3 ± 2.0	26.6 ± 0.6	101.1 ± 2.3

Sample	Ca / %	Cu / (µg g^-1)	Fe / (µg g^-1)	K / %	Mg / (µg g^-1)	Mn / (µg g^-1)	Na / %	P / %	S / %	Sr / (µg g^-1)	Ti / %	V / (µg g^-1)
A / grape	0.370 ± 0.003	0.63 ± 0.060	350 ± 6	0.053 ± 0.001	32.7 ± 1.8	2.76 ± 0.01	0.45 ± 0.02	0.170 ± 0.001	0.310 ± 0.002	1.87 ± 0.10	< 0.3 µg g^-1	< 0.1
B / strawberry	0.410 ± 0.011	0.65 ± 0.060	361 ± 19	0.042 ± 0.003	86.3 ± 1.0	1.50 ± 0.02	0.94 ± 0.05	0.230 ± 0.007	0.110 ± 0.004	7.80 ± 0.20	0.041 ± 0.001	0.33 ± 0.03
C / passion fruit	0.0980 ± 0.002	< 0.6	< 1.5	0.015 ± 0.001	170.0 ± 1.0	0.39 ± 0.01	0.39 ± 0.01	0.054 ± 0.001	0.050 ± 0.001	3.21 ± 0.10	0.400 ± 0.008	3.61 ± 0.02
D / grape	0.880 ± 0.007	2.86 ± 0.18	< 1.5	1.42 ± 0.02	91.9 ± 1.2	1.28 ± 0.02	0.27 ± 0.01	0.700 ± 0.007	0.410 ± 0.003	5.88 ± 0.40	0.033 ± 0.0003	0.240 ± 0.004
E / tangerine	0.730 ± 0.004	1.52 ± 0.09	440 ± 21	0.068 ± 0.001	445.0 ± 3.4	1.92 ± 0.04	0.49 ± 0.01	0.380 ± 0.001	0.100 ± 0.001	14.0 ± 0.10	0.064 ± 0.0003	0.500 ± 0.004
F / strawberry	0.720 ± 0.003	1.88 ± 0.21	428 ± 21	0.049 ± 0.001	176.0 ± 1.2	1.68 ± 0.06	0.89 ± 0.03	0.420 ± 0.004	0.110 ± 0.001	23.4 ± 0.40	0.091 ± 0.0021	0.77 ± 0.05
G / mango	0.570 ± 0.010	< 0.6	456 ± 14	0.037 ± 0.002	36.8 ± 1.4	4.73 ± 0.44	0.64 ± 0.04	< 2.7 µg g^-1	< 9.4 µg g^-1	< 0.4	0.210 ± 0.009	< 0.1
H / tangerine	0.0350 ± 0.001	< 0.6	< 1.5	0.021 ± 0.002	13.4 ± 0.9	< 0.1	0.49 ± 0.02	< 2.7 µg g^-1	< 9.4 µg g^-1	< 0.4	0.051 ± 0.001	< 0.1
I / pineapple	0.0750 ± 0.008	< 0.6	< 1.5	0.034 ± 0.003	14.2 ± 0.8	0.40 ± 0.04	0.81 ± 0.01	< 2.7 µg g^-1	< 9.4 µg g^-1	< 0.4	0.083 ± 0.003	< 0.1
J / pineapple	0.630 ± 0.024	< 0.6	< 1.5	0.033 ± 0.002	126.0 ± 6.9	0.61 ± 0.04	0.44 ± 0.02	< 2.7 µg g^-1	< 9.4 µg g^-1	< 0.4	0.200 ± 0.015	< 0.1
K / orange	0.480 ± 0.001	< 0.6	< 1.5	< 36 µg g^-1	140.0 ± 8.0	< 0.1	0.47 ± 0.01	0.210 ± 0.0004	0.180 ± 0.001	< 0.4	0.130 ± 0.007	< 0.1
L / orange with lemon	0.220 ± 0.001	< 0.6	< 1.5	0.042 ± 0.001	71.2 ± 1.1	< 0.1	0.10 ± 0.01	0.090 ± 0.001	0.072 ± 0.001	< 0.4	< 0.3 µg g^-1	< 0.1
M / pineapple	0.300 ± 0.002	< 0.6	< 1.5	< 36 µg g^-1	68.6 ± 5.0	< 0.1	0.22 ± 0.01	0.140 ± 0.0002	0.110 ± 0.004	< 0.4	0.042 ± 0.001	< 0.1
N / mango	0.350 ± 0.005	< 0.6	< 1.5	< 36 µg g^-1	33.2 ± 1.7	< 0.1	0.45 ± 0.02	0.140 ± 0.001	0.150 ± 0.009	< 0.4	0.150 ± 0.003	< 0.1
O / lemon	0.320 ± 0.024	< 0.6	< 1.5	< 36 µg g^-1	122.0 ± 4.9	< 0.1	0.16 ± 0.02	0.180 ± 0.011	0.130 ± 0.007	< 0.4	< 0.3 µg g^-1	< 0.1
P / strawberry	0.240 ± 0.004	< 0.6	< 1.5	< 36 µg g^-1	58.8 ± 1.6	< 0.1	0.20 ± 0.01	0.120 ± 0.005	0.070 ± 0.006	< 0.4	0.015 ± 0.001	< 0.1
Q / tangerine	0.250 ± 0.004	< 0.6	< 1.5	0.030 ± 0.003	46.5 ± 0.9	< 0.1	0.10 ± 0.01	0.140 ± 0.008	0.083 ± 0.0004	< 0.4	0.032 ± 0.002	< 0.1
R / orange	0.250 ± 0.007	< 0.6	< 1.5	0.350 ± 0.002	104.0 ± 1.0	< 0.1	< 3.8 µg g^-1	0.140 ± 0.002	0.120 ± 0.001	< 0.4	0.045 ± 0.002	< 0.1
S / passion fruit	0.150 ± 0.007	< 0.6	138 ± 2	< 36 µg g^-1	16.0 ± 1.6	< 0.1	0.15 ± 0.01	0.061 ± 0.003	0.100 ± 0.002	< 0.4	0.030 ± 0.003	< 0.1
T / orange	0.190 ± 0.008	< 0.6	208 ± 12	< 36 µg g^-1	53.2 ± 2.9	< 0.1	0.12 ± 0.01	0.083 ± 0.004	0.110 ± 0.004	< 0.4	0.050 ± 0.002	< 0.1
Minimum	0.0350	< 0.6	< 1.5	< 36	13.4	< 0.1	< 3.8	< 2.7	< 9.4	< 0.4	< 0.3	< 0.1
Maximum	0.880	2.86	456	1.42	445	4.73	0.94	0.700	0.410	23.4	0.400	3.61
Number of samples	20	05	07	13	20	10	19	16	16	06	17	05
Average	0.363	1.51	340	0.169	95.3	1.70	0.41	0.204	0.138	9.36	0.098	1.09
Standard deviation	0.231	0.83	113	0.371	93.7	1.30	0.26	0.162	0.091	7.38	0.095	1.27
^a a Recommended values by ANVISA, Resolution No. 55,871, 1965, March 26.12 Results expressed as average ± standard deviation (SD, n = 3). n.d.: not determined. ANVISA / (µg g^-1)	n.d.	5.00	n.d.	n.d.	n.d.	n.d.	n.d.	n.d.	n.d.	n.d.	n.d.	n.d.

[1] *e-mail: rgoa01@terra.com.br, rennan@ufba.br

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Development of Analytical Method for Determination of Inorganic Constituents in Powder Refreshment Using Dilute Mineral Acids and Detection by ICP OES