海洋沉积物陆源碎屑粒度分析预处理方法研究

doi:10.11867/j.issn.1001-8166.2017.07.0769

如何有效去除海洋沉积物中的非陆源物质,同时又能完好保存陆源碎屑,是获得陆源碎屑粒度变化信息的先决条件。利用南海MD190航次的深海岩芯沉积物样品,进行了不同预处理条件下的生源物质去除效果和陆源碎屑粒度分析结果的对比研究。结合显微镜和扫描电镜观察,获得了海洋沉积物陆源碎屑粒度分析预处理方法的新认识。结果显示,对于海洋沉积物中的有机质、碳酸盐和生物硅3种生源组分,依次使用浓度为30%的H₂O₂水浴60 ℃震荡3 h,0.5%的HCl充分反应1 h,2 mol/L的Na₂CO₃水浴85 ℃震荡5 h,可以有效去除,并能兼顾去除效率以及相对完好地保存陆源碎屑。研究认为,针对不同类型的沉积物样品进行陆源碎屑粒度分析时,应考虑生源碎屑对粒度结果的实际影响,从而选择合适的预处理方案。即在确保陆源碎屑的粒度分析结果更接近真实分布的情况下,沉积物样品的预处理步骤越少越好,并非一定要去除所有的生源成分。如当生物硅含量低于2%时,其对陆源碎屑粒度分析结果的影响很小,可不用去除。另外,超声可导致部分陆源碎屑的破碎,在粒度分析预处理过程中全程不宜使用。

关键词: 陆源碎屑, 粒度分析, 预处理方法, 生源碎屑, 超声

The prerequisite for obtaining variations of terrigenous grain-size of marine sediments is how to effectively remove non-terrigenous matters and preserve terrigenous particles synchronously. Combined with observations under biological microscope and scanning electron microscope, a comparative study of biogenic debris removal effect and terrigenous grain-size analysis under different pretreatment condition was performed on core sediments, which were retrieved in the South China Sea during the MD190 cruise. Our new results showed that the main three biogenic particles, namely, organic matter, carbonate, and opal in marine sediments could be removed effectively by 30% H₂O₂ in a stirring water bath at 60 ℃ for 3 h, 0.5% HCl for 1 h, and 2 mol/L Na₂CO₃ in a stirring water bath at 85 ℃ for 5 h, in turn. Such pretreatments achieved the goals of biogenic debris removal efficiency and relatively well-preserved terrigenous particles. Prior to selecting an appropriate pretreatment method, this study suggested that the actual effects of biogenic detritus on grain-size results of diverse marine sediment samples should be taken into account. If the laboratory data are ensured to be closer to the natural grain-size distribution of terrigenous particles, the removals of all biogenic debris are not always needed, and the less pretreatment processes the better. For example, opal particles have little effect on terrigenous grain-size distribution when their percentage is lower than 2%. Thus, there is no use to remove them from marine sediments before laboratory grain-size analysis of terrigenous particles. Additionally, ultrasonic is not suggested through the whole process of terrigenous grain-size analysis because the strong energy of ultrasonic can lead to the fragmentation of some fragile terrigenous particles.

Key words: Terrigenous particle, Grain-size analysis, Pretreatment method, Biogenic debris, Ultrasonic.

中图分类号:

P736.21

表1 南海及世界其他海域沉积物粒度分析预处理方法总结

Table 1 A review of pretreatment methods of sediment grain-size analysis in the South China Sea and other regions

编号	研究材料	时间属性	生源颗粒是否去除			是否超声	参考文献
编号	研究材料	时间属性	有机质			碳酸盐	蛋白石
1	MD05-2900 MD05-2901 MD05-2904 MD05-2897	方法研究 450 ka 260 ka 486 ka	是	是	是	是	[13] [17] [18]
2	MD05-2905 表层沉积物 DS97-2P^a GeoB7920^b SO120-289KL^c	36 ka 现代 MIS 3 120 ka 80 ka	是	是	是	否	[19] [20] [10] [14] [16]
3	ODP 1146 KNG-5	20 Ma 17.5 ka	是	是	否	是	[21] [22]
4	MD01-2393 ODP 1144 ODP 1143 ODP 1144 ODP 1123^d PS67等^e	190 ka 1.1 Ma 1.8 Ma 1.5~0.4 Ma 15.5~12.5 Ma 30 ka	否	是	是	否	[7] [6] [23] [15] [4]
5	17937-2 17938-2 17939-2 17940-1/2 GHE27L SL112^f SL148^f	末次冰期 21 ka 26 ka 21 ka	是	是	否	否	[8] [8] [8] [8] [24] [25]
6	ODP 1144 ODP 1143 MD05-2895 NIOP469^c ODP 984^a	140 ka MIS 3 20 ka 25 ka	否	是	否	否	[5] [26] [27] [9] [11]
7	ODP 1144	14 ka	否	否	否	是	[12]
8	NS93-5 NIOP468等^c	200 ka 15 ka	否	否	否	否	[28] [9]

表1 南海及世界其他海域沉积物粒度分析预处理方法总结

Table 1 A review of pretreatment methods of sediment grain-size analysis in the South China Sea and other regions

编号	研究材料	时间属性	生源颗粒是否去除			是否超声	参考文献
编号	研究材料	时间属性	有机质			碳酸盐	蛋白石
1	MD05-2900 MD05-2901 MD05-2904 MD05-2897	方法研究 450 ka 260 ka 486 ka	是	是	是	是	[13] [17] [18]
2	MD05-2905 表层沉积物 DS97-2P^a GeoB7920^b SO120-289KL^c	36 ka 现代 MIS 3 120 ka 80 ka	是	是	是	否	[19] [20] [10] [14] [16]
3	ODP 1146 KNG-5	20 Ma 17.5 ka	是	是	否	是	[21] [22]
4	MD01-2393 ODP 1144 ODP 1143 ODP 1144 ODP 1123^d PS67等^e	190 ka 1.1 Ma 1.8 Ma 1.5~0.4 Ma 15.5~12.5 Ma 30 ka	否	是	是	否	[7] [6] [23] [15] [4]
5	17937-2 17938-2 17939-2 17940-1/2 GHE27L SL112^f SL148^f	末次冰期 21 ka 26 ka 21 ka	是	是	否	否	[8] [8] [8] [8] [24] [25]
6	ODP 1144 ODP 1143 MD05-2895 NIOP469^c ODP 984^a	140 ka MIS 3 20 ka 25 ka	否	是	否	否	[5] [26] [27] [9] [11]
7	ODP 1144	14 ka	否	否	否	是	[12]
8	NS93-5 NIOP468等^c	200 ka 15 ka	否	否	否	否	[28] [9]

图1 扫描电镜及生物显微镜下的陆源碎屑颗粒及生物碎屑
(a)MD12-3428岩芯沉积物去除生源碎屑后生物显微镜下陆源碎屑颗粒;(b)MD12-3428岩芯沉积物中生物硅和陆源碎屑颗粒生物显微镜下的大小比较;(c)和(d)MD12-3434岩芯沉积物中生物硅和陆源碎屑扫描电镜下的大小比较

Fig.1 Terrigenous and biogenic particles under biological microscope and scanning electron microscope
(a) Terrigenous particles of core MD12-3428 after removed biogenic particles under biological microscope; (b) Terrigenous VS. opal particles of Core MD12-3428 under biological microscope; (c) and (d) Terrigenous VS. opal particles of Core MD12-3434 under scanning electron microscope

表2 MD12-3428岩芯陆源碎屑粒度分析试验样品沉积物组成

Table 2 Sediment compositions of selected samples from Core MD12-3428 for grain-size analysis

样品层位/cm	100	200	300	500	700
碳酸盐/%	24	20	22	26	29
生物硅/%	1.6	2.0	1.8	2.0	2.0
有机质/%	0.9	0.9	0.9	0.8	1.0
陆源碎屑/%	74	78	76	71	68

表2 MD12-3428岩芯陆源碎屑粒度分析试验样品沉积物组成

Table 2 Sediment compositions of selected samples from Core MD12-3428 for grain-size analysis

样品层位/cm	100	200	300	500	700
碳酸盐/%	24	20	22	26	29
生物硅/%	1.6	2.0	1.8	2.0	2.0
有机质/%	0.9	0.9	0.9	0.8	1.0
陆源碎屑/%	74	78	76	71	68

表3 MD12-3434岩芯陆源碎屑粒度分析试验样品沉积物组成

Table 3 Sediment compositions of selected samples from Core MD12-3434 for grain-size analysis

样品层位/cm	0	200	400	600	800
碳酸盐/%	20	12	15	17	11
生物硅/%	4.9	6.5	4.9	5.7	3.8
有机质/%	0.9	1.3	1.2	1.0	0.7
陆源碎屑/%	74	81	79	76	85

表3 MD12-3434岩芯陆源碎屑粒度分析试验样品沉积物组成

Table 3 Sediment compositions of selected samples from Core MD12-3434 for grain-size analysis

样品层位/cm	0	200	400	600	800
碳酸盐/%	20	12	15	17	11
生物硅/%	4.9	6.5	4.9	5.7	3.8
有机质/%	0.9	1.3	1.2	1.0	0.7
陆源碎屑/%	74	81	79	76	85

表4 MD12-3428岩芯沉积物样品去除有机质后残留样品烧失量随反应时间的变化及试验过程记录

Table 4 Temporal variations of loss on ignition of residual sediments at Core MD12-3428 after removing organic matter under different reaction time and the procedure record

反应时间/h		1	2	3	4	5
样品1	坩埚重/g	11.7741	13.5706	13.3905	14.4166	13.5602
	坩埚+样品重/g	11.9661	13.7237	13.5974	14.6316	13.7109
	490 ℃烧2 h后/g	11.9523	13.7123	13.5814	14.6149	13.6993
	烧失量/%	7.19	7.45	7.73	7.77	7.70
样品2	坩埚重/g	11.5332	12.7334	13.0958	14.3292	11.4270
	坩埚+样品重/g	11.6963	12.9267	13.2655	14.5265	11.6083
	490 ℃烧2 h后/g	11.6861	12.9133	13.2534	14.5125	11.5971
	烧失量/%	6.25	6.93	7.13	7.10	6.18 ?

表4 MD12-3428岩芯沉积物样品去除有机质后残留样品烧失量随反应时间的变化及试验过程记录

Table 4 Temporal variations of loss on ignition of residual sediments at Core MD12-3428 after removing organic matter under different reaction time and the procedure record

反应时间/h		1	2	3	4	5
样品1	坩埚重/g	11.7741	13.5706	13.3905	14.4166	13.5602
	坩埚+样品重/g	11.9661	13.7237	13.5974	14.6316	13.7109
	490 ℃烧2 h后/g	11.9523	13.7123	13.5814	14.6149	13.6993
	烧失量/%	7.19	7.45	7.73	7.77	7.70
样品2	坩埚重/g	11.5332	12.7334	13.0958	14.3292	11.4270
	坩埚+样品重/g	11.6963	12.9267	13.2655	14.5265	11.6083
	490 ℃烧2 h后/g	11.6861	12.9133	13.2534	14.5125	11.5971
	烧失量/%	6.25	6.93	7.13	7.10	6.18 ?

图2 MD12-3428岩芯样品去除有机质后残留样品烧失量的时间序列变化

Fig.2 Temporal variations of loss on ignition of residual sediments at Core MD12-3428 after removing organic matter under different reaction time

图3 MD12-3428岩芯陆源碎屑不同预处理方法粒度分析结果

Fig.3 Results of terrigenous grain-size analysis under different pretreatment procedure at Core MD12-3428

图4 MD12-3434岩芯陆源碎屑不同预处理方法粒度分析结果

Fig.4 Results of terrigenous grain-size analysis under different pretreatment procedures at Core MD12-3434

表5 MD12-3434岩芯沉积物中生物硅除与不除陆源碎屑粒度分析结果对比

Table 5 Comparison between grain-size analysis results of opal-free and opal-within terrigenous particles at Core MD12-3434

粒度参数	预处理方法	样品层位/cm
粒度参数	预处理方法	0	200	400	600	800
平均粒径/μm	去除有机质+碳酸盐	12.11	12.41	14.33	17.45	14.56
平均粒径/μm	去除所有生源颗粒	7.51	7.83	8.06	9.89	8.90
中值粒径/μm	去除有机质+碳酸盐	5.43	7.19	7.25	8.01	6.52
中值粒径/μm	去除所有生源颗粒	5.31	5.12	5.75	7.24	6.29
黏土含量对比/%	去除有机质+碳酸盐	59	47	47	43	52
黏土含量对比/%	去除所有生源颗粒	61	62	57	47	53
粉砂含量对比/%	去除有机质+碳酸盐	38	50	49	51	44
粉砂含量对比/%	去除所有生源颗粒	39	38	42	53	47

表5 MD12-3434岩芯沉积物中生物硅除与不除陆源碎屑粒度分析结果对比

Table 5 Comparison between grain-size analysis results of opal-free and opal-within terrigenous particles at Core MD12-3434

粒度参数	预处理方法	样品层位/cm
粒度参数	预处理方法	0	200	400	600	800
平均粒径/μm	去除有机质+碳酸盐	12.11	12.41	14.33	17.45	14.56
平均粒径/μm	去除所有生源颗粒	7.51	7.83	8.06	9.89	8.90
中值粒径/μm	去除有机质+碳酸盐	5.43	7.19	7.25	8.01	6.52
中值粒径/μm	去除所有生源颗粒	5.31	5.12	5.75	7.24	6.29
黏土含量对比/%	去除有机质+碳酸盐	59	47	47	43	52
黏土含量对比/%	去除所有生源颗粒	61	62	57	47	53
粉砂含量对比/%	去除有机质+碳酸盐	38	50	49	51	44
粉砂含量对比/%	去除所有生源颗粒	39	38	42	53	47

表6 超声对MD12-3428岩芯沉积物陆源碎屑粒度分析结果的影响

Table 6 Effect of ultrasound on grain size analysis of terrigenous particles at Core MD12-3428

粒度参数	是否超声	样品层位/cm								平均值
粒度参数	是否超声	80		82		84	86	88	90	92
平均粒径/μm	是	12.09	13.88		12.71	12.36	12.43	12.04	12.88	12.59
平均粒径/μm	否	18.67	14.89		17.40	18.34	15.47	16.36	16.10	16.75
中值粒径/μm	是	6.98	6.68		6.75	6.74	6.84	6.64	6.67	6.77
中值粒径/μm	否	10.72	9.57		11.10	10.15	10.85	11.01	10.88	10.61
中值/平均粒径比	是	0.58	0.48		0.53	0.55	0.55	0.55	0.52	0.54
中值/平均粒径比	否	0.57	0.64		0.64	0.55	0.70	0.67	0.68	0.63

表6 超声对MD12-3428岩芯沉积物陆源碎屑粒度分析结果的影响

Table 6 Effect of ultrasound on grain size analysis of terrigenous particles at Core MD12-3428

粒度参数	是否超声	样品层位/cm								平均值
粒度参数	是否超声	80		82		84	86	88	90	92
平均粒径/μm	是	12.09	13.88		12.71	12.36	12.43	12.04	12.88	12.59
平均粒径/μm	否	18.67	14.89		17.40	18.34	15.47	16.36	16.10	16.75
中值粒径/μm	是	6.98	6.68		6.75	6.74	6.84	6.64	6.67	6.77
中值粒径/μm	否	10.72	9.57		11.10	10.15	10.85	11.01	10.88	10.61
中值/平均粒径比	是	0.58	0.48		0.53	0.55	0.55	0.55	0.52	0.54
中值/平均粒径比	否	0.57	0.64		0.64	0.55	0.70	0.67	0.68	0.63

图5 MD12-3428岩芯陆源碎屑超声后与不超声粒度分析结果

Fig.5 Results of terrigenous grain-size analysis under ultrasonic or without ultrasonic at Core MD12-3428

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A Study of Pretreatment Methods for Terrigenous Grain-Size Analysis of Marine Sediments