海洋沉积物不同相态中Sr、Nd同位素提取方法研究

张颖; 张辉; 王小静; 刘季花; 汪虹敏; 朱爱美; 胡宁静

doi:10.3969/j.issn.0253-4193.2020.02.016

海洋沉积物不同相态中Sr、Nd同位素提取方法研究

doi: 10.3969/j.issn.0253-4193.2020.02.016

张颖^{1, 2, 3,},
张辉^{1, 2, 3},
王小静^{1, 2, 3},
刘季花^{1, 2, 3, ,},
汪虹敏^{1, 2, 3},
朱爱美^{1, 2, 3},
胡宁静^{1, 2, 3}

1.
自然资源部第一海洋研究所，山东青岛 266061
2.
海洋沉积与环境地质自然资源部重点实验室，山东青岛 266061
3.
青岛海洋科学与技术试点国家实验室海洋地质过程与环境功能实验室，山东青岛 266237

基金项目: 国际海域资源调查与开发“十三五”规划项目（DY135-R2-1-01，DY135-R2-1-03）；国家自然科学基金项目（41676053）；国家自然科学基金青年科学基金项（41706068，41606075）。

详细信息

作者简介:
张颖（1986—），女，山西省晋中县人，助理工程师，主要从事海洋沉积物元素与同位素分析研究。E-mail：zhangyinghj@163.com

通讯作者:
刘季花（1965—），女，研究员，主要从事海洋沉积地球化学方面研究。E-mail：jihliu@fio.org.cn

中图分类号: P736.41
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出版历程
- 收稿日期: 2019-01-29
- 修回日期: 2019-04-09
- 网络出版日期: 2020-11-18
- 刊出日期: 2020-02-25

Sequential extraction of Sr and Nd isotope from Fe–Mn oxyhydroxide and detrital in marine sediments

Zhang Ying^{1, 2, 3
,},
Zhang Hui^{1, 2, 3},
Wang Xiaojing^{1, 2, 3},
Liu Jihua^{1, 2, 3
, ,},
Wang Hongmin^{1, 2, 3},
Zhu Aimei^{1, 2, 3},
Hu Ningjing^{1, 2, 3}

1.
First Institute of Oceanography, Minisitry Natural Resources, Qingdao 266061, China
2.
Key Laboratory of Marine Sedimentology and Environmental Geology, Minisitry Natural Resources, Qingdao 266061, China
3.
Laboratory for Marine Geology and Environment, Pilot National Laboratory for Marine Science and Technology (Qingdao), Qingdao 266237, China

摘要

摘要: 海洋沉积物中Fe-Mn氧化物相和残渣态的Sr、Nd同位素组成能够敏感地指示洋流循环及物质来源，但实验室对沉积物中上述相态的Sr和Nd同位素的提取易产生过量或提取不完全，进而影响同位素测定结果的准确性，因此制定有效的提取流程显得非常重要。本文采用不同浓度盐酸羟胺(Hydroxylamine Hydrochloride，HH)与醋酸(Acetic Acid，HAc)混合溶液对中印度洋海盆深海沸石黏土、北极半深海沉积物以及安达曼海近海沉积物的Fe-Mn氧化物相进行提取，残渣态用HNO₃-HF高压密闭消解法溶融，测定了各相态的主微量元素含量及Sr、Nd同位素组成，通过分析不同实验条件下得到的Fe-Mn氧化物相与残渣态的稀土元素(REE)配分模式、Al/Nd含量比值及Sr、Nd同位素组成，建立了3种不同成因类型海洋沉积物不同相态的化学提取方法。提取深海沸石黏土中Fe-Mn氧化物相的理想试剂条件为0.25 mol/L HH和15% HAc，北极半深海沉积物和安达曼海近海沉积物的试剂条件为0.5 mol/L HH和15% HAc。该方法可以准确获得沉积物中Fe-Mn氧化物相与残渣态的Sr、Nd同位素组成信息，为古海洋学的研究提供方法支持。
- 海洋沉积物 /
- 相态提取 /
- 铁锰氧化物 /
- 残渣态 /
- ⁸⁷Sr/⁸⁶Sr /
- ¹⁴³Nd/¹⁴⁴Nd
Abstract: The radiogenic isotope composition of neodymium (Nd) and strontium (Sr) extracted from Fe-Mn oxyhydroxide and detrital in marine sediments indicated potential for investigate present and past oceanic circulation or input of terrigenous material. However, the isotope compositions of elements obtained from the Fe-Mn oxyhydroxide fraction and detrital are easily disturbed by each other originating from the extraction process, will affect the isotope composition of these fractions. Therefore, it is very important to establish a rigorous leaching procedure that can be used to separate both Fe-Mn oxyhydroxide and the detrital fraction from the same marine sediment sample for Nd and Sr isotopic analysis. In this study, the mixture reagent of hydroxylamine hydrochloride (HH) and acetic acid (HAc) at 12 different concentrations were used to extract Fe-Mn oxyhydroxide fraction and detrital from zeolite clay of the Central Indian Ocean Basin, bathyal sediment of Arctic and offshore marine sediment of the Andaman Sea. Detrital was dissolved by HF-HNO₃ system with high-pressure closed digestion method. Elements concentration and Sr and Nd isotope ratios in these fractions were measured. To corroborate the reliability of the extracting methods, REE patterns, Al/Ca ratios, as well as Sr and Nd isotope compositions were applied to assess the absence of detrital contributions to the extracted solutions and to support the seawater origin of the Nd isotope ratios in the Fe-Mn oxyhydroxide fraction. The result showed that different genetic types of sediments have different extraction reagents. The ideal reagent concentration for extraction of Fe-Mn oxyhydroxide fraction from zeolite clay is 0.25 mol/L HH in 15% acetic acid, for bathyal sediment of Greenland Sea and offshore marine sediment is 0.5 mol/L HH in 15% acetic acid. This method can accurately obtain the Sr and Nd isotopic composition of Fe-Mn oxyhydroxide and residue state in marine sediments, providing method support for the study of paleoceanography.
- marine sediment /
- extraction /
- Fe-Mn oxyhydroxide /
- detritus /
- ⁸⁷Sr/⁸⁶Sr /
- ¹⁴³Nd/¹⁴⁴Nd

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图 1 连续相态提取实验流程

Fig. 1 Flowchart of the procedures for sequential extraction experiment

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图 2 不同实验条件下Sr、Nd同位素结果

Fig. 2 Sr and Nd isotope results from experimental investigations

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图 3 3种类型沉积物中Fe-Mn氧化物相和残渣态的稀土元素后太古宙澳大利亚页岩标准化模式图

Fig. 3 Normalized REE with Post-Archean Australian Shale Composite of both Fe-Mn fraction and residue from three types of sediments

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图 4 3个样品Fe-Mn氧化物相和残渣态中元素Al/Nd的比值

Fig. 4 Element ratios (Al/Nd) for Fe-Mn fraction and residue of the three samples presented

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表 1 3个沉积物样品采样信息和特征

Tab. 1 Sample locations and characteristics of sediments analyzed in this study

实验编号	样品号	海区	纬度	经度	水深/m	粒级组分/%			沉积物类型
实验编号	样品号	海区	纬度	经度	水深/m	砂	粉砂	黏土	沉积物类型
A	GC19	中印度洋海盆	3°53′S	8°55′E	4 643	0.03	68.84	31.16	深海黏土（含有铁锰微结核）
B	IS4C	格陵兰海	68°42′N	14°48’W	1 595	5.36	61.98	32.66	黏土质粉砂
C	ADM-S18	安达曼海	6°57’S	97°55′E	335	20.05	71.09	8.88	砂质粉砂

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表 2 3个样品中主、微量元素及稀土元素含量(主量元素单位:%, 微量元素单位:10^-6)

Tab. 2 Contents of major(%), trace and rare earth elements(10^-6) of 3 samples from different areas

样品	Al₂O₃	CaO	Fe₂O₃	K₂O	MgO	MnO	Na₂O	P₂O₅	TiO₂	SiO2	Ba	Sr	Zn	Zr	Cr	Co	Ni
A	11.38	4.14	13.22	2.68	3.12	3.76	5.02	2.59	0.59	38.32	404	322	243	200	43	249	765
B	10.34	16.52	5.99	1.87	2.28	0.21	3.55	0.21	0.86	38.37	593	654	77	132	60	23	35
C	10.86	7.49	3.63	1.85	2.05	0.04	3.22	0.13	0.49	50.71	217	317	75	190	54	9	27

样品	Cu	Y	La	Ce	Pr	Nd	Sm	Eu	Gd	Tb	Dy	Ho	Er	Tm	Yb	Lu	ΣREE
A	680	434	271	212	65.6	281	60.72	14.50	56.8	10.61	66.9	13.04	37.25	5.51	33.67	5.53	1 133
B	30	23	28	57	6.7	25	4.95	1.35	4.46	0.74	4.57	0.85	2.38	0.38	2.33	0.35	139
C	18	24	31	63	7.1	26	5.04	0.91	4.30	0.73	4.40	0.83	2.44	0.39	2.47	0.39	149

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表 3 不同浓度盐酸羟氨（C_H·H）与不同质量百分比浓度醋酸（C_HAc）混合溶液条件

Tab. 3 The mixture of hydroxylamine hydrochloride and acetic acid at different concentrations

编号	C_H·H/mol·L⁻¹	C_HAc/%	编号	C_H·H /mol·L⁻¹	C_HAc/%
a1	2.00	15	b1	2.00	25
a2	1.00	15	b2	1.00	25
a3	0.50	15	b3	0.50	25
a4	0.25	15	b4	0.25	25
a5	0.10	15	b5	0.10	25
a6	0.04	15	b6	0.04	25

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表 4 ICP-OES标准溶液浓度

Tab. 4 Concentrations of standard solutions measured by ICP-OES

溶液	混合标液编号
溶液	空白	STD 1	STD 2	STD 3	STD 4
多元素混合标准溶液1/μg·mL⁻¹	0.000	0.025	0.125	0.250	1.250
多元素混合标准溶液 2/μg·mL⁻¹	0.000	0.100	0.500	1.000	5.000
多元素混合标准溶液4/μg·mL⁻¹	0.000	0.025	0.125	0.250	1.250

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表 5 ICP-MS标准溶液浓度

Tab. 5 Concentrations of standard solutions measured by ICP-MS

溶液	混合标液编号
溶液	空白	STD 1	STD 2	STD 3	STD 4	STD 5
多元素混合标准溶液 1/ng·mL⁻¹	0.00	0.50	2.50	5.00	25.00	50.00
多元素混合标准溶液 2/ng·mL⁻¹	0.00	1.00	5.00	10.00	50.00	100.00
多元素混合标准溶液 4/ng·mL⁻¹	0.00	1.00	5.00	10.00	50.00	100.00

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表 6 不同提取条件下Fe-Mn氧化物相和残渣态元素在全样中的百分含量(%)

Tab. 6 Percentage of representative elements in different chemical phase from leaching tests(%)

样品	Al		Ca		Fe		Mn		Sr		Nd
样品	Fe-Mn 氧化物相	残渣态	Fe-Mn 氧化物相	残渣态	Fe-Mn 氧化物相	残渣态	Fe-Mn 氧化物相	残渣态	Fe-Mn 氧化物相	残渣态	Fe-Mn 氧化物相	残渣态
Aa1	3.85	74.41	20.97	6.41	18.90	64.47	69.27	1.63	24.21	13.39	89.25	8.47
Aa2	2.94	79.29	24.00	11.30	16.58	70.33	70.85	2.32	29.31	15.40	78.94	22.18
Aa3	2.57	79.77	22.98	15.31	15.20	70.27	71.23	2.97	29.66	17.18	68.01	32.84
Aa4	2.35	82.31	20.80	16.27	15.44	73.57	74.84	3.77	29.64	18.30	55.01	39.24
Aa5	2.02	80.89	17.34	19.02	13.42	74.22	72.81	4.46	26.41	20.05	41.92	47.78
Aa6	2.12	77.81	13.15	16.17	9.75	77.66	68.83	5.68	20.08	19.55	39.32	43.71
Ab1	4.16	78.86	28.71	7.82	20.03	65.61	70.54	1.46	31.83	14.17	87.82	13.71
Ab2	3.51	79.27	29.08	10.59	17.72	68.76	73.57	2.02	34.78	15.26	83.04	20.81
Ab3	3.04	78.96	23.05	15.16	15.60	71.30	71.89	2.63	30.16	16.87	63.51	32.52
Ab4	2.90	78.48	18.52	14.73	14.89	68.84	72.13	2.86	26.81	17.34	56.14	32.85
Ab5	2.61	77.94	18.22	23.32	12.98	71.60	70.41	3.53	27.50	20.75	41.00	54.47
Ab6	2.56	78.16	13.89	24.33	10.29	78.28	67.42	5.12	21.92	22.25	35.13	55.45
Ba1	2.79	73.04	1.39	7.15	13.52	72.17	57.92	17.40	2.57	15.25	21.03	60.89
Ba2	3.02	74.83	1.51	8.39	13.52	74.87	60.79	20.02	2.78	16.24	20.63	62.41
Ba3	2.82	76.16	1.49	7.18	11.84	75.14	60.94	20.97	2.75	16.00	17.30	62.84
Ba4	2.75	74.39	1.54	9.27	11.17	74.63	61.72	21.79	2.74	17.38	15.87	68.06
Ba5	2.41	69.88	1.81	9.07	9.34	70.64	61.47	21.37	2.66	16.89	12.58	69.46
Ba6	2.13	75.66	1.56	9.90	7.68	77.46	60.13	23.73	2.50	18.38	10.42	74.77
Bb1	3.15	74.53	1.52	9.27	15.02	70.18	61.09	20.08	2.69	17.72	22.40	61.46
Bb2	2.96	72.56	1.41	9.60	13.05	70.72	59.34	20.70	2.60	17.52	19.92	65.92
Bb3	3.19	71.04	1.53	8.94	13.18	71.29	60.97	20.10	2.71	16.88	18.42	66.93
Bb4	2.49	74.03	1.23	9.68	9.81	74.43	52.69	21.77	2.22	17.78	12.97	64.60
Bb5	2.40	73.56	1.31	9.75	9.38	73.72	57.13	21.94	2.25	18.19	12.19	72.92
Bb6	2.32	70.02	1.37	9.24	8.57	74.95	57.32	21.81	2.30	16.73	10.57	70.51
Ca1	2.76	76.38	3.50	1.48	20.46	63.62	19.54	25.69	3.70	9.26	25.14	54.90
Ca2	2.42	76.86	3.38	1.44	18.36	65.49	18.50	26.84	3.56	9.35	20.27	60.77
Ca3	1.98	78.41	3.30	1.46	16.31	68.99	16.74	27.80	3.44	9.51	16.99	65.14
Ca4	1.50	88.44	3.45	1.27	14.22	84.72	15.98	31.54	3.58	9.27	11.81	73.32
Ca5	1.11	84.03	3.18	1.47	12.66	80.19	14.61	30.73	3.34	9.29	8.23	72.85
Ca6	0.85	77.62	3.13	1.81	10.33	77.92	26.23	30.76	3.16	9.46	5.37	75.11
Cb1	3.07	79.39	3.27	1.28	22.11	65.14	19.26	24.99	3.37	8.99	23.97	56.20
Cb2	2.54	80.61	2.95	1.54	18.05	68.60	18.62	26.52	3.16	9.28	20.08	59.01
Cb3	1.94	74.29	2.71	1.50	14.67	65.01	15.75	26.52	2.86	9.23	14.27	59.30
Cb4	2.28	97.25	3.10	0.90	19.03	94.02	18.13	30.04	3.28	9.01	15.04	70.71
Cb5	1.29	74.53	3.12	1.71	13.34	67.18	15.25	28.49	3.17	9.34	8.69	65.65
Cb6	0.89	68.32	3.04	1.97	10.58	63.13	13.41	27.92	3.06	9.53	5.89	68.85

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表 7 不同提取条件下Fe-Mn氧化物相和残渣态中元素浓度及Sr、Nd同位素比值

Tab. 7 Al, Sr and Nd concentration and Sr, Nd isotope ratios of Fe-Mn oxyhydroxide leaching phases and the respective detrital fraction

样品	Fe-Mn 氧化物相							样品	残渣态
	Al/%	Sr/10⁻⁶	Nd/10⁻⁶	⁸⁷Sr/⁸⁶Sr	¹⁴³Nd/¹⁴⁴Nd	ε_Nd	Al/Nd		Al/%	Sr/10⁻⁶	Nd/10⁻⁶	⁸⁷Sr/⁸⁶Sr	¹⁴³Nd/¹⁴⁴Nd	ε_Nd	Al/Nd
				±0.000 02	±0.000 014	±0.27						±0.000 02	±0.000 014	±0.27
Aa1	0.29	97	290	0.709 63	0.512 285	−6.9	9.9	Aa1	6.59	63	39	0.719 05	0.512 207	−8.4	1 671
Aa2	0.21	113	239	0.710 11	0.512 278	−7.0	8.8	Aa2	6.69	69	98	0.717 95	0.512 249	−7.6	680
Aa3	0.18	114	205	0.70925	0.512 279	−7.0	9.0	Aa3	6.63	76	143	0.716 95	0.512 265	−7.3	462
Aa4	0.17	116	181	0.70925	0.512 279	−7.0	9.5	Aa4	6.72	80	168	0.717 28	0.512 267	−7.2	399
Aa5	0.15	102	136	0.70979	0.512 282	−6.9	10.7	Aa5	6.58	87	204	0.716 10	0.512 264	−7.3	322
Aa6	0.16	80	134	0.709 91	0.512 274	−7.1	11.9	Aa6	6.49	87	192	0.716 37	0.512 267	−7.2	339
Ab1	0.30	121	286	0.710 70	0.512 275	−7.1	10.4	Ab1	6.69	64	61	0.718 85	0.512 230	−8.0	1 094
Ab2	0.25	133	265	0.709 38	0.512 274	−7.1	9.5	Ab2	6.68	69	92	0.718 14	0.512 254	−7.5	725
Ab3	0.22	115	204	0.709 24	0.512 284	−6.9	10.6	Ab3	6.55	75	142	0.717 25	0.512 270	−7.2	462
Ab4	0.21	106	185	0.709 72	0.512 272	−7.1	11.5	Ab4	6.58	78	145	0.716 97	0.512 258	−7.4	455
Ab5	0.19	109	134	0.70961	0.512 271	−7.2	14.4	Ab5	6.53	93	240	0.715 63	0.512 267	−7.2	272
Ab6	0.18	85	112	0.709 21	0.512 277	−7.0	16.5	Ab6	6.38	97	238	0.716 12	0.512 271	−7.2	268
Ba1	0.25	27	8.32	0.709 04	0.512 443	−3.8	296	Ba1	6.56	164	29	0.711 93	0.512 232	−7.9	2 294
Ba2	0.26	28	7.99	0.708 63	0.512 457	−3.5	324	Ba2	6.67	173	29	0.711 46	0.512 311	−6.4	2 293
Ba3	0.24	29	6.72	0.708 68	0.512 461	−3.5	363	Ba3	6.83	172	29	0.711 71	0.512 277	−7.1	2 318
Ba4	0.24	28	6.18	0.70858	0.512 449	−3.7	387	Ba4	6.62	185	32	0.710 99	0.512 357	−5.5	2 090
Ba5	0.21	27	4.80	0.70854	0.512 443	−3.8	429	Ba5	6.20	179	32	0.710 72	0.512 366	−5.3	1 924
Ba6	0.18	26	4.07	0.708 53	0.512 436	−3.9	450	Ba6	6.62	192	34	0.710 71	0.512 356	−5.5	1 935
Bb1	0.27	28	8.67	0.708 70	0.512 453	−3.6	313	Bb1	6.69	190	29	0.710 90	0.512 320	−6.2	2 319
Bb2	0.25	27	7.59	0.708 70	0.512 456	−3.6	335	Bb2	6.52	188	31	0.710 80	0.512 326	−6.1	2 105
Bb3	0.28	28	7.30	0.708 62	0.512 447	−3.7	381	Bb3	6.38	181	31	0.711 01	0.512 344	−5.7	2 030
Bb4	0.22	23	5.09	0.708 59	0.512447	−3.7	423	Bb4	6.57	189	30	0.710 82	0.512 355	−5.5	2 191
Bb5	0.21	23	4.65	0.708 57	0.512 444	−3.8	447	Bb5	6.52	193	34	0.710 68	0.512 327	−6.1	1 929
Bb6	0.20	24	4.15	0.708 52	0.512 444	−3.8	491	Bb6	6.21	177	33	0.710 94	0.512 340	−5.8	1 899
Ca1	0.20	15	8.21	0.709 62	0.512 127	−10.0	249	Ca1	5.93	40	22	0.727 62	0.511 989	−12.7	2 723
Ca2	0.18	15	6.73	0.709 62	0.512 131	−9.9	266	Ca2	5.96	40	24	0.727 64	0.511 977	−12.9	2 476
Ca3	0.14	14	5.46	0.709 55	0.512 136	−9.8	264	Ca3	6.01	40	26	0.727 42	0.511 992	−12.6	2 356
Ca4	0.11	15	3.73	0.709 37	0.512 142	−9.7	296	Ca4	6.78	39	29	0.726 80	0.512 017	−12.1	2 362
Ca5	0.08	14	2.64	0.709 39	0.512 149	−9.5	311	Ca5	6.46	39	29	0.727 45	0.512 025	−12.0	2 258
Ca6	0.06	13	1.73	0.709 33	0.512 137	−9.8	358	Ca6	5.94	40	29	0.726 41	0.512 001	−12.4	2 023
Cb1	0.23	14	7.77	0.709 39	0.512 144	−9.6	290	Cb1	6.14	38	22	0.728 08	0.511 960	−13.2	2 765
Cb2	0.19	13	6.50	0.709 67	0.512 124	−10.0	285	Cb2	6.18	39	23	0.727 32	0.511 991	−12.6	2 674
Cb3	0.14	12	4.60	0.709 46	0.512 136	−9.8	308	Cb3	5.64	39	23	0.727 56	0.511 967	−13.1	2 453
Cb4	0.17	13	4.84	0.709 44	0.512 141	−9.7	347	Cb4	7.50	38	28	0.726 75	0.512 021	−12.0	2 692
Cb5	0.10	13	2.86	0.709 44	0.512 136	−9.8	339	Cb5	5.79	40	26	0.727 38	0.512 026	−11.9	2 223
Cb6	0.07	12	1.92	0.709 36	0.512 131	−9.9	340	Cb6	5.16	40	27	0.726 55	0.512 005	−12.4	1 942

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