Comparing Methods for Extracting Heavy Metals from Histosols for Establishing Quality Reference Values

Lima, Erica Souto Abreu; Amaral, Nelson Moura Brasil do; Pérez, Daniel Vidal; Coutinho, Izabella Bezerra

doi:10.1590/18069657rbcs20150097

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Division 2 - Soil Processes and Properties • Rev. Bras. Ciênc. Solo 40 (0) • 2016 • https://doi.org/10.1590/18069657rbcs20150097 copy

Comparing Methods for Extracting Heavy Metals from Histosols for Establishing Quality Reference Values

Authorship SCIMAGO INSTITUTIONS RANKINGS

ABSTRACT

The diversity of methods for heavy metal extraction from soils complicates comparison of results used by environmental agencies to establish quality reference values. The aim of this study was to evaluate three soil digestion methods regarding the solubilizing capacity of Ba, Cr, Cu, Fe, Mn, Ni, Pb and Zn, and to propose a standard method to establish Quality Reference Values (QRVs) for Brazilian Histosols. Twenty soil samples were selected to evaluate the USEPA 3051, USEPA 3051A and Aqua Regia methods in a closed system. The methods tested were statistically similar regarding Cu, Fe and Mn extraction from soils. However, the methods can not be considered similar for Ba, Cr, Ni, Pb and Zn; Aqua Regia recorded the highest levels, except for Ba. The Aqua Regia method proved suitable for metal extraction from soils with organic characteristics and can be used to establish QRVs.

organic horizons; pseudo-total content; soil digestion methods

Sample	Location/ Horizon	pH(H₂O)	P	K⁺	Ca²⁺	Mg²⁺	SB	Al³⁺	H+Al	CEC	MM	OM	C	C-HAF	C-FAF	C-HUM
			mg dm^-3	------------------ cmol_c dm^-3 ------------------							%	------------------ g kg^-1 ------------------
1	BA02/ Hdoj3	2.5	0.0	0.1	3.8	4.2	8.2	8.5	88.6	96.9	26.0	740.0	369.9	189.5	16.7	175.8
2	BA03/ Hdopj1	3.6	54.0	0.4	5.9	5.7	12.3	1.6	44.9	57.2	19.0	807.0	387.6	159.5	36.5	184.3
3	BA03/ Hdopj2	3.5	0.0	0.1	1.7	3.1	5.2	2.6	43.6	48.7	6.0	939.0	555.4	198.9	16.2	281.1
4	MA05/ Hdo1	4.3	15.0	1.3	9.0	9.2	20.3	2.7	19.3	39.6	64.0	355.0	154.1	34.2	12.7	96.5
5	MA05/ Hdo2	4.4	14.0	1.0	7.1	7.9	16.4	5.0	28.9	45.3	79.0	208.0	110.4	23.5	9.0	64.5
6	MG01/ Hd	4.6	13.0	0.1	3.2	1.6	5.8	1.9	45.5	51.3	59.0	412.0	213.7	95.5	23.6	77.6
7	MG01/ Hdo	4.5	1.0	0.4	0.6	0.9	3.0	7.9	29.9	32.9	38.0	615.0	279.0	65.9	40.0	147.4
8	PR02/ Hdp1	4.4	40.0	0.4	5.6	3.3	9.4	0.7	34.8	44.2	72.0	279.0	144.1	89.5	13.1	36.5
9	PR02/ Hdp2	4.1	7.0	0.2	3.5	1.8	5.6	4.5	63.2	68.8	62.0	376.0	192.8	143.4	10.0	30.7
10	RJ02/ Ho1	4.1	5.0	0.3	3.4	4.8	10.3	4.4	51.2	61.5	16.0	837.0	426.1	87.1	11.6	335.0
11	RJ03/ 2Hbd	4.8	41.0	0.2	4.5	2.2	7.1	1.5	25.4	32.5	66.0	335.0	178.2	50.5	14.3	78.8
12	RJ03/ Hdo1	5.3	2.0	0.3	12.1	14.8	27.8	1.1	20.0	47.7	28.0	718.0	314.9	121.2	42.6	139.2
13	RJ03/ Hdp2	4.9	31.0	0.2	5.7	2.8	9.4	1.4	18.2	27.6	75.0	254.0	125.9	43.8	14.1	54.1
14	RJ 04/ Hdp1	5.5	23.0	0.1	2.5	4.7	7.6	0.1	20.3	27.9	81.0	186.0	91.7	30.5	15.6	20.9
15	RS 04/ Hdj	3.5	27.0	0.2	4.5	13.4	18.2	3.8	70.3	88.5	32.0	678.0	482.2	153.7	16.6	240.1
16	RS 05/ Hdj	3.5	27.0	0.1	4.0	6.0	10.2	2.2	47.2	57.4	51.0	488.0	291.6	134.0	24.4	111.4
17	SC 01/ H2	4.6	N.D	0.7	13.9	8.6	23.3	0.6	16.4	39.7	N.D	N.D	N.D	108.5	26.0	224.5
18	SC 02/ Hdoj2	3.3	6.0	0.2	4.4	3.1	7.9	2.1	44.2	52.1	6.0	940.0	528.1	188.4	24.5	260.3
19	SP 01/ Hp1	5.2	4.0	0.5	0.6	1.5	3.2	0.4	58.2	61.4	61.0	391.0	207.4	112.8	23.7	53.7
20	SP 01/ Hp2	5.1	1.0	0.1	0.3	1.1	1.5	0.3	41.7	43.3	69.0	313.0	144.4	95.1	13.2	17.7

Digestion	Method	Proportion (v/v)	System
Pseudo - Total	Aqua Regia (AR)	1 HNO₃: 3 HCl	Closed system (microwave)
	EPA 3051 (NIT)	HNO₃
	EPA 3051A (RAR)	3 HNO₃: 1 HCl

Sample NIST	Certified value	Leach Recovery NIST	EPA 3051		EPA 3051A		Aqua Regia

			Determined value	Recovery (determined)⁽¹⁾	Determined value	Recovery (determined)⁽¹⁾	Determined value	Recovery (determined)⁽¹⁾
	mg kg^-1	%	mg kg^-1	%	mg kg^-1	%	mg kg^-1	%
	Zn
2709	106±3	94	91.6	86	98.5	99	104.4	105
2782	1254±196	93	1183	101	1290	111	1125	96
	Fe
2709	35000±1100	86	28270	94	33157	111	40205	134
2782	269000±7000	94	320939	126	304219	120	278927	110
	Mn
2709	538±17	87	417.1	89	468.9	100	467.1	100
2782	300	86	197.1	76	245.0	95	246.1	96
	Cu
2709	34.6±0.7	92	34.4	108	33.3	104	31.0	97
2782	2594±52	94	2429	100	2439	100	2327	96
	Ni
2709	88±5	89	72.7	93	78.1	100	75.3	96
2782	154.1±3.1	62	109.9	115	117.5	122	101.8	106
	Pb
2709	18.9±0.5	69	5.5	42	8.6	66	14.5	112
2782	574±11	97	482.5	87	500.5	90	551.5	100
	Cr
2709	130±4	61	48.5	61	54.7	69	66.7	84
2782	109±6.0	61	50.1	76	58.5	89	72.0	109
	Ba
2709	968±40	41	460.5	116	376.2	95	343.8	86
2782	254±24	60	170.5	112	168.7	111	146.8	97

y	x	a	b	Confidence interval (1 %)

				a		b

				Upper	Lower	Upper	Lower
		Zn
RAR	HNO₃	0.22	0.94	-3.12	3.56	0.86	1.02
AR	HNO₃	-4.50	1.20	-12.89	3.91	1.01	1.39
AR	RAR	-5.01	1.28	-11.14	1.11	1.13	1.43
		Mn
RAR	HNO₃	3.53	0.96	-3.74	10.80	0.89	1.02
AR	HNO₃	-0.89	1.05	-19.07	17.29	0.88	1.22
AR	RAR	-4.02	1.09	-23.46	15.41	0.90	1.27
		Fe
RAR	HNO₃	-152.71	1.08	-1836	1530.26	0.89	1.26
AR	HNO₃	2183.79	1.02	-3040	7407.91	0.46	1.59
AR	RAR	2436.55	0.94	-2513	7386.38	0.44	1.43
		Cu
RAR	HNO₃	-1.15	0.97	-4.04	1.73	0.89	1.05
AR	HNO₃	0.46	1.02	-5.18	6.11	0.87	1.18
AR	RAR	1.58	1.05	-2.55	5.71	0.93	1.18
		Ni
RAR	HNO₃	-0.13	0.99	-1.06	0.80	0.89	1.09
AR	HNO₃	1.41	1.57	-2.49	5.32	1.15	1.98
AR	RAR	1.61	1.59	-1.91	5.13	1.20	1.97
		Pb
RAR	HNO₃	3.44	0.85	1.81	5.07	0.76	0.93
AR	HNO₃	3.83	1.05	0.03	7.63	0.85	1.25
AR	RAR	-0.57	1.25	-3.85	2.70	1.07	1.42
		Cr
RAR	HNO₃	3.36	0.96	1.63	5.09	0.89	1.04
AR	HNO₃	5.74	1.01	-3.03	14.51	0.64	1.39
AR	RAR	2.13	1.06	-7.29	11.54	0.68	1.42
		Ba
RAR	HNO₃	14.91	0.79	-19.07	48.88	0.67	0.91
AR	HNO₃	3.56	0.55	-13.80	20.92	0.49	0.61
AR	RAR	0.47	0.65	-32.96	33.91	0.51	0.80

Sample	Zn			Ni			Pb			Cr			Ba

	RAR: NIT	AR: NIT	AR: RAR	RAR: NIT	AR: NIT	AR: RAR	RAR: NIT	AR: NIT	AR: RAR	RAR: NIT	AR: NIT	AR: RAR	RAR: NIT	AR: NIT	AR: RAR
	-------------- % --------------
1	-6	-29	-25	-36	28	99	136	186	21	34	-13	-35	11	-65	-69
2	-11	10	24	-20	39	74	-11	18	33	-1	9	10	-22	-49	-34
3	0	5	5	-25	109	179	3	48	44	7	14	7	63	38	-15
4	-8	-17	-9	5	140	129	8	15	7	17	35	16	-7	22	32
5	-4	15	20	1	53	52	114	186	33	38	231	140	-13	-43	-35
6	2	2	0	-10	-21	-12	11	20	9	124	113	-5	-18	-28	-13
7	-5	2	8	-11	111	136	-7	2	10	5	25	19	-4	-47	-45
8	7	-6	-12	-23	69	119	350	417	15	57	32	-16	145	-91	-96
9	1	45	43	-16	301	377	10	28	16	17	22	4	-17	8	31
10	-34	-47	-19	52	112	40	-6	9	16	0	-4	-4	52	-58	-72
11	2	10	8	3	57	51	4	29	24	15	23	6	-26	-48	-30
12	-1	-5	-4	-11	22	38	-6	4	10	13	1	-10	-15	-45	-36
13	-11	0	12	-4	43	50	0	15	15	20	-2	-18	-19	-51	-39
14	5	-9	-13	-12	31	48	44	72	19	88	83	-2	-28	-55	-38
15	-6	-22	-17	13	32	16	320	160	-38	585	445	-20	-30	-37	-10
16	-1	-11	-10	0	80	80	11	24	12	5	17	11	37	67	22
17	19	36	14	3	65	60	8	31	22	89	119	16	-30	-46	-22
18	-4	48	54	12	195	163	229	343	35	381	230	-31	197	14	-62
19	-2	33	36	1	80	78	7	30	21	7	151	135	-14	-41	-32
20	-10	19	32	26	239	168	37	117	59	6	18	12	-1	40	42
Mean⁽¹⁾	7	19	18	14	91	98	66	88	23	75	79	26	37	45	39
Max⁽¹⁾	34	48	54	52	301	377	350	417	59	585	445	140	197	91	96
Min⁽¹⁾	0	0	0	0	21	12	0	2	7	0	1	2	1	8	10
SD⁽¹⁾	8	16	14	13	76	82	109	117	14	147	112	39	49	19	22

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[1] *Corresponding author: E-mail: ericaabreulima@gmail.com