两种测定海洋沉积物中碳酸盐含量的非器测方法对比分析*

doi:10.11978/2025108

Abstract

Abstract:

Carbonates constitute a critical component of marine sediments, and accurate determination of their content is fundamental to understanding global shifts in carbonate deposition and dissolution within the oceans, as well as the influence of carbonate system evolution on climate change. The gasometric method and the weight-loss method are typical non-instrumental approaches to carbonate quantification; however, their precision and reliability in the analysis of marine sediment carbonates remain insufficiently evaluated. This study first investigates the solubility of carbon dioxide (CO₂) gas in hydrochloric acid (HCl) solutions, and finds that under typical temperature and pressure conditions, the solubility of CO₂ gas in the ~18% HCl solution (20 mL) within the gasometric device ranges from 0.3% to 21.5%, with an average of 9%. Subsequently, using both the gasometric method and an improved weight-loss method, we conducted a comparative analysis of carbonate content in prepared samples with varying calcium carbonate concentrations and in deep-sea sedimentary sequence samples. The experimental results reveal that, due to CO₂ dissolution in HCl, the gasometric method induces an absolute error in carbonate concentration analysis ranging from 0.3% to 18.2% (mean = 4.4%), with a standard deviation of 5.4%. In contrast, the improved weight-loss method yields errors of only 0.2% to 2.4% (mean = 1.0%) and a substantially lower standard deviation of 1.2%. These findings demonstrate that the accuracy and stability of the improved weight-loss method for carbonate quantification are superior to those of the gasometric method. Moreover, a comparison of carbonate content results for samples derived from IODP (International Ocean Discovery Program) Site U1553, obtained by both methods in this study and by coulometric titration, reveals that the improved weight-loss method more accurately reproduces the carbonate content variations observed at Site U1553, further validating its reliability and applicability for determining carbonate content in deep-sea sediments.

Key words: carbonate, gasometric method, weight-loss method, measurement error, deep-sea sediments

CLC Number:

P736.21

ZHANG Qiang, ZHAO Zhongwei, SU Xiang, ZHAO Xuan, LI Wei. A comparison of two non-instrumental methodologies for determining carbonate content in marine sediments^*[J].Journal of Tropical Oceanography, 2026, 45(3): 25-38.

Figures/Tables 8

Fig. 1

Appendix Tab. 1

Determination of carbonate content and its error in different prepared samples by the gasometric method (standard sample)"

样品号	碳酸钙重量/g	黏土重量/g	碳酸钙含量真实值%	碳酸钙标样重量/g	实验室温度/°C	盐酸与样品反应前滴定读数/mL	盐酸与样品反应后滴定读数 /mL	生成的CO₂体积/mL	碳酸钙重量测量值/g	碳酸钙含量测量值/%	测量绝对误差值/%
标准				0.0981	26	11.4	33.7	22.3
1	0.0043	0.1446	2.89			10.2	10.6	0.4	0.0018	1.18	1.71
2	0.0091	0.1391	6.14			16	17.6	1.6	0.0070	4.75	1.39
3	0.0158	0.1353	10.46			24	28.6	4.6	0.0202	13.39	2.94
4	0.0207	0.1235	14.36			12.8	16.9	4.1	0.0180	12.51	1.85
标准				0.0957	26	9.5	31.7	22.2
5	0.0255	0.1258	16.85			10.2	15.4	5.2	0.0212	14.00	2.86
6	0.031	0.1274	19.57			23	31.3	8.3	0.0338	21.34	1.77
7	0.0362	0.1157	23.83			7.3	14.2	6.9	0.0281	18.50	5.33
8	0.0396	0.1122	26.09			21.5	30	8.5	0.0346	22.80	3.28
标准				0.0977	26	12.5	34.5	22
9	0.0456	0.105	30.28			10.3	20.2	9.9	0.0417	27.68	2.60
10	0.0504	0.1009	33.31			25.6	35.8	10.2	0.0430	28.39	4.92
11	0.0559	0.0931	37.52			5.9	18.9	13	0.0547	36.74	0.77
12	0.0612	0.0893	40.66			22.1	37.9	15.8	0.0665	44.21	3.55
标准				0.0981	26	9.6	31.4	21.8
13	0.0663	0.0846	43.94			10.3	26.3	16	0.0720	47.71	3.78
14	0.0718	0.0799	47.33			7.7	23.9	16.2	0.0729	48.06	0.73
15	0.0746	0.0745	50.03			10.7	29.8	19.1	0.0860	57.65	7.61
16	0.0795	0.0713	52.72			8.6	27.1	18.5	0.0833	55.21	2.49
标准				0.1037	26	5.1	28.5	23.4
17	0.0852	0.0653	56.61			6.9	24.5	17.6	0.0797	52.96	3.65
18	0.091	0.0582	60.99			7.1	24.5	17.4	0.0788	52.81	8.18
19	0.0967	0.0548	63.83			8.2	29.2	21	0.0951	62.77	1.06
20	0.1022	0.0491	67.55			9.4	30.6	21.2	0.0960	63.45	4.10
标准				0.1015	26	10.7	31.5	20.8
21	0.106	0.0457	69.87			7.6	26.9	19.3	0.0942	62.08	7.79
22	0.1105	0.0404	73.23			7.3	29.3	22	0.1074	71.14	2.08
23	0.1152	0.0359	76.24			11.5	36.8	25.3	0.1235	81.71	5.47
24	0.1224	0.0286	81.06			8.9	35	26.1	0.1274	84.35	3.29
25	0.1253	0.0255	83.09			5.3	36.6	31.3	0.1527	101.29	18.19
标准				0.102	26	8.5	30.1	21.6
26	0.1308	0.0183	87.73			8.5	35.8	27.3	0.1266	84.89	2.84
27	0.1347	0.014	90.59			10.3	36.2	25.9	0.1201	80.75	9.83
28	0.1401	0.0083	94.41			7.6	35.9	28.3	0.1312	88.42	5.99
29	0.1445	0.0066	95.63			8.2	37.2	29	0.1345	88.98	6.65
30	0.151	0	100			6.5	40.7	34.2	0.1586	105.01	5.01

Appendix Tab. 1

Appendix Tab. 2

Determination of carbonate content and its error in different prepared samples by the weight-loss method"

离心管号	离心管重量/g	碳酸钙重量/g	黏土重量/g	碳酸钙含量真实值/%	离心管与样品总重/g	去离子水洗盐烘干后离心管+ 样品总重量/g	盐酸反应、洗盐、烘干后离心管+ 样品总重量/g	碳酸钙重量测量值/g	碳酸钙含量测量值/%	测量绝对误差值/%
1	10.2252	0.0057	0.2961	1.89	10.5270	10.5101	10.4983	0.0118	3.91	2.02
2	10.1821	0.0147	0.2799	4.99	10.4767	10.4653	10.4434	0.0219	7.43	2.44
3	10.1873	0.0251	0.2733	8.41	10.4857	10.4672	10.4487	0.0185	6.20	2.21
4	10.1678	0.0362	0.2636	12.07	10.4676	10.4514	10.4102	0.0412	13.74	1.67
5	10.1734	0.0453	0.2537	15.15	10.4724	10.4551	10.4167	0.0384	12.84	2.31
6	10.1856	0.0555	0.2471	18.34	10.4882	10.4792	10.4287	0.0505	16.69	1.65
7	10.1757	0.0692	0.2331	22.89	10.4780	10.4658	10.4040	0.0618	20.44	2.45
8	10.2331	0.0811	0.2136	27.52	10.5278	10.5178	10.4341	0.0837	28.40	0.88
9	10.2444	0.0916	0.2087	30.50	10.5447	10.5367	10.4419	0.0948	31.57	1.07
10	10.1261	0.1019	0.1993	33.83	10.4273	10.4191	10.3149	0.1042	34.59	0.76
11	10.1281	0.1105	0.1910	36.65	10.4296	10.4219	10.3086	0.1133	37.58	0.93
12	10.1800	0.1210	0.1774	40.55	10.4784	10.4702	10.3477	0.1225	41.05	0.50
13	10.2163	0.1298	0.1707	43.19	10.5168	10.5088	10.3813	0.1275	42.43	0.77
14	10.1821	0.1402	0.1588	46.89	10.4811	10.4743	10.3326	0.1417	47.39	0.50
15	10.2582	0.1511	0.148	50.52	10.5573	10.5501	10.3997	0.1504	50.28	0.23
16	10.2682	0.1607	0.1399	53.46	10.5688	10.5596	10.3976	0.1620	53.89	0.43
17	10.1072	0.1705	0.1301	56.72	10.4078	10.4015	10.2298	0.1717	57.12	0.40
18	10.1569	0.1808	0.1196	60.19	10.4573	10.4499	10.2670	0.1829	60.89	0.70
19	10.2122	0.1902	0.1087	63.63	10.5111	10.5049	10.3115	0.1934	64.70	1.07
20	10.1136	0.2017	0.0973	67.46	10.4126	10.4093	10.2058	0.2035	68.06	0.60
21	10.2207	0.2101	0.0892	70.20	10.5200	10.5159	10.3052	0.2107	70.40	0.20
22	10.2739	0.2202	0.0793	73.52	10.5734	10.5702	10.3516	0.2186	72.99	0.53
23	10.1204	0.2300	0.0689	76.95	10.4193	10.4152	10.1831	0.2321	77.65	0.70
24	10.2065	0.2398	0.0587	80.34	10.505	10.5015	10.2596	0.2419	81.04	0.70
25	10.1543	0.2514	0.0488	83.74	10.4545	10.4522	10.1981	0.2541	84.64	0.90
26	10.2031	0.2611	0.0385	87.15	10.5027	10.5017	10.2384	0.2633	87.88	0.73
27	10.1908	0.2707	0.0281	90.60	10.4896	10.4887	10.2167	0.2720	91.03	0.44
28	10.1537	0.2803	0.0207	93.12	10.4547	10.4539	10.1726	0.2813	93.46	0.33
29	10.2082	0.2915	0.0090	97.00	10.5087	10.5081	10.2158	0.2923	97.27	0.27
30	10.1455	0.3016	0	100.00	10.4471	10.4463	10.1465	0.2998	99.40	0.60

Appendix Tab. 2

Fig. 2

Fig. 3

Fig. 4

Appendix Tab. 3

Tab. 1

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序号	碳酸钙标样重量/g	反应前滴管中液面读数/mL	反应后滴管中液面读数/mL	CO₂气体体积/mL
1	0.0300	5.6	12.9	7.3
2	0.0670	10.4	25.4	15.0
3	0.0988	7.8	29.1	21.3
4	0.1300	9.2	39.1	29.9
5	0.1680	7.8	42.9	35.1

测量方法	绝对误差范围/%	平均误差/%	标准偏差/%
气量法-标准曲线	0.3~12.5	4.7	5.7
气量法-标准样品	0.8~18.2	4.4	5.4
质量损失法	0.2~2.4	1.0	1.2

A comparison of two non-instrumental methodologies for determining carbonate content in marine sediments^*

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A comparison of two non-instrumental methodologies for determining carbonate content in marine sediments*

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A comparison of two non-instrumental methodologies for determining carbonate content in marine sediments^*