AJAC  Vol.6 No.7 , June 2015
Methods Development for the Optical Determination of the Black Carbon Content of Loess Samples
Abstract: We evaluate the applicability of an optical transmission measurement method commonly used for the analysis of the Black Carbon (BC) content of aerosol sample, to determine the BC content of loess sediments. A number of different sample pretreatment procedures are developed and compared, leading to an optimum preparation process. The results include: 1) Subtraction of the optical attenuation values before and after heating of the sample filters (“ΔATN”) varies linearly with the sample mass. The slope of the regression line provides the best determination of BC concentration. 2) When the sample mass is small, (NaPO3)6 pretreatment is best for BC measurement, and the BC concentration results are given by the slope of the regression between ΔATN and sample mass, for a series of samples of varying mass. 3) HF pretreatment accompanied by centrifugation and rinsing may produce a negative bias on the result. 4) Replicate measurements of BC for loess samples showed a maximum deviation less than 5.6%, suggesting that measurements of the BC concentration of a sequence of loess samples could determine variations to this degree of significance. 5) The overall trends of BC concentration in loess section sequences were similar for all chemical pretreatments. The BC concentration result for replicate samples is comparable when pretreated by the same procedure.
Cite this paper: Mu, Y. , Qin, X. , Liu, J. and Yin, Z. (2015) Methods Development for the Optical Determination of the Black Carbon Content of Loess Samples. American Journal of Analytical Chemistry, 6, 585-603. doi: 10.4236/ajac.2015.67057.

[1]   Ahmed, T., Dutkiewicz, V.A. and Shareef, A. (2009) Measurement of Black Carbon (BC) by an Optical Method and a thermal-Optical Method: Intercomparison for Four Sites. Atmospheric Environment, 43, 6305-6311.

[2]   Poot, A., Quik, J.T.K., Veld, H. and Koelmans, A.A. (2009) Quantification Methods of Black Carbon: Comparison of Rock-Eval Analysis with Traditional Methods. Journal of Chromatography A, 1216, 613-622.

[3]   Masiello, C.A. and Druffel, E.R.M. (1998) Black Carbon in Deep-Sea Sediments. Science, 280, 1911-1913.

[4]   Wang, G.C., Bai, J.H., Kong, Q.X. and Emilenko, A. (2005) Black Carbon Particles in the Urban Atmosphere in Beijing. Advances in Atmospheric Sciences, 22, 640-646.

[5]   Preston, C.M. and Schmidt, M.W.I. (2006) Black (Pyrogenic) Carbon: A Synthesis of Current Knowledge and Uncertainties with Special Consideration of Boreal Regions. Biogeosciences, 3, 397-420.

[6]   Hsieh, Y.P. and Bugna, G.C. (2008) Analysis of Black Carbon in Sediments and Soils Using Multi-Element Scanning Thermal Analysis (MESTA). Organic Geochemistry, 39, 1562-1571.

[7]   Gelinas, Y., Prentice, K.M., Bladock, J.A. and Hedges, J.I. (2001) An Improved Thermal Oxidation Method for the Quantification of Soot/Graphitic Black Carbon in Sediments and Soils. Environmental Science & Technology, 35, 3519-3525.

[8]   Elmquist, M., Gustafsson, O. and Andersson, P. (2004) Quantification of Sedimentary Black Carbon Using the Chemothermal Oxidation Method: An Evaluation of Ex Situ Pretreatments and Standard Additions Approaches. Limnology and Oceanography: Methods, 2, 417-427.

[9]   Schmidt, M.W.I. and Noack, A.G. (2000) Black Carbon in Soils and Sediments: Analysis, Distribution, Implications, and Current Challenges. Global Biogeochemical Cycles, 14, 777-793.

[10]   Bird, M.I.J. and Cali, A. (1998) A Million-Year Record of Fire in Sub-Saharan Africa. Nature, 394, 767-769.

[11]   Lim, B. and Cachier, H. (1996) Determination of Black Carbon by Chemical Oxidation and Thermal Treatment in Recent Marine and Lake Sediments and Cretaceous-Tertiary Clays. Chemical Geology, 131, 143-154.

[12]   Muri, G., Cermelj, B., Faganeli, J. and Brancelj, A. (2002) Black Carbon in Slovenian Alpine Lacustrine Sediments. Chemosphere, 46, 1225-1234.

[13]   Seiler, W. and Crutzen, P.J. (1980) Estimates of Gross and Net Fluxes of Carbon between the Biosphere and the Atmosphere from Biomass Burning. Climatic Change, 2, 207-247.

[14]   Kuhlbusch, T.A.J. and Crutzen, P.J. (1995) Toward a Global Estimate of Black Carbon in Residues of Vegetation Fires Representing a Sink of Atmospheric CO2 and a Source of O2. Global Biogeochemical Cycles, 9, 491-501.

[15]   Trumbore, S.E., Chadwick, O.A. and Amundson, R. (1996) Rapid Exchange between Soil Carbon and Atmospheric Carbon Dioxide Driven by Temperature Change. Science, 272, 392-396.

[16]   Middelburg, J.J., Nieuwenhuize, J. and van Breugel, P. (1999) Black Carbon in Marine Sediments. Marine Chemistry, 65, 245-252.

[17]   Simpson, M.J. and Hatcher, P.G. (2004) Overestimates of Black Carbon in Soils and Sediments. Naturwissenschaften, 91, 436-440.

[18]   Sun, X.S., Peng, P.A., Song, J.Z., Zhang, G. and Hu, J.F. (2008) Sedimentary Record of Black Carbon in the Pearl River Estuary and Adjacent Northern South China Sea. Applied Geochemistry, 23, 3464-3472.

[19]   Schmidt, M.W.I., Masiello, C.A. and Skjemstad, J.O. (2003) Final Recommendations for Reference Materials in Black Carbon Analysis. Eos, Transactions American Geophysical Union, 52, 582-583.

[20]   Schmidt, M.W.I., Skjemstad, J.O., Czimczik, C.I., Glaser, B., Prentice, K.M., Gelinas, Y. and Kuhlbusch, T.A.J. (2001) Comparative Analysis of Blank Carbon in Soils. Global Biogeochemical Cycles, 15, 163-167.

[21]   Gustafsson, O., Bucheli, T.D., Kukulska, Z., Andersson, M., Largeau, C., Rouzaud, J.-N., et al. (2001) Evaluation of a Protocol for the Quantification of Black Carbon in Sediments. Global Biogeochemical Cycles, 15, 881-890.

[22]   Hammes, K., Schmidt, M.W.I., Smernik, R.J., Currie, L.A., Ball, W.P., Nguyen, T.H., et al. (2007) Comparison of Quantification Methods to Measure Fire-Derived (Black/Elemental) Carbon in Soils and Sediments Using Reference Materials from Soil, Water, Sediment and the Atmosphere. Global Biogeochemical Cycles, 21.

[23]   Nguyen, T.H., Brown, R.A. and Ball, W.P. (2004) An Evaluation of Thermal Resistance as a Measure of Black Carbon Content in Diesel Soot, Wood Char, and Sediment. Organic Geochemistry, 35, 217-234.

[24]   Gustafsson, O., Haghseta, F., Chan, C., Macfarlane, J. and Gschwend, P.M. (1997) Quantification of the Dilute Sedimentary Soot Phase: Implications for PAH Speciation and Bioavailability. Environmental Science & Technology, 31, 203-209.

[25]   Allen, G.A., Lawrence, J. and Koutrakis, P. (1998) Field Validation of a Semi-Continuous Method for Aerosol Black Carbon (Aethalometer) and Temporal Patterns of Summertime Hourly Black Carbon Measurements in Southwestern PA. Atmospheric Environment, 33, 817-823.

[26]   Chow, J.C., Watson, J.G., Pritchett, L.C., Pierson, W.R., Frazier, C.A. and Purcell, R.G. (1993) The Dri Thermal/Optical Reflectance Carbon Analysis System: Description, Evaluation and Applications in US Air Quality Studies. Atmospheric Environment, 27, 1185-1201.

[27]   Chow, J.C., Watson, J.G., Chen, L.W.A., Arnott, W.P. and Moosmuller, H. (2004) Equivalence of Elemental Carbon by Thermal/Optical Reflectance and Transmittance with Different Temperature Protocols. Environmental Science Technology, 38, 4414-4422.

[28]   Watson, J.G., Chow, J.C. and Chen, L.W.A. (2005) Summary of Organic and Elemental Carbon/Black Carbon Analysis Methods and Intercomparisons. Aerosol and Air Quality Research, 5, 65-102.

[29]   Han, Y.M., Cao, J.J., An, Z.S., Chow, J.C., Watson, J.G., Jin, Z.D., Fung, K. and Liu, S.X. (2007) Evaluation of the Thermal/Optical Reflectance Method for Quantification of Elemental Carbon in Sediments. Chemosphere, 69, 526-533.

[30]   Han, Y.M., Cao, J.J., Chow, J.C., Watson, J.G., An, Z.S., Jin, Z.D., Fung, K. and Liu, S.X. (2007) Evaluation of the Thermal/Optical Reflectance Method for Discrimination between Char- and Soot-EC. Chemosphere, 69, 569-574.

[31]   Han, Y.M., Han, Z.W., Cao, J.J., Chow, J.C., Watson, J.G., An, Z.S., Liu, S.X. and Zhang, R.J. (2008) Distribution and Origin of Carbonaceous Aerosol over a Rural High-Mountain Lake Area, Northern China and Its Transport Significance. Atmospheric Environment, 42, 2405-2414.

[32]   Han, Y.M., Cao, J.J., Posmentier, E.S., Chow, J.C., Watson, J.G., Fung, K.K., Jin, Z.D., Liu, S.X. and An, Z.S. (2008) The Effect of Acidification on the Determination of Elemental Carbon, Char-, and Soot-Elemental Carbon in Soils and Sediments. Chemosphere, 75, 92-99.

[33]   Glaser, B., Haumaier, L., Guggenberger, G. and Zech, W. (1998) Black Carbon in Soils: The Use of Benzenecarboxylic Acids as Specific Markers. Organic Geochemistry, 29, 811-819.

[34]   Qiu, J., Gao, R., Yang, Y.S., Yin, Y.F., Ma, H.L. and Li, Y.F. (2009) Advances on Research of Black Carbon in Soil. Journal of Subtropical Resources and Environment, 4, 88-94. (In Chinese)

[35]   Zhang, X.D., Liang, C., Ge, Y.P., Jiang, Y., Xie, H.T., He, H.B. and Wang, J. (2003) Roles of Black Carbon in the Biogeochemical Cycles of Soil Organic Carbon. Chinese Journal of Soil Science, 34, 349-355. (In Chinese)

[36]   Currie, L.A., Benner, B.A., Kessler, J.D., Klindinst, D.B., Kloda, G.A., Marolf, J.V., Slater, J.F., Wise, S.A., Cachier, H., Cary, R., Chow, J.C., Watson, J., Druffel, E.R.M., Masiello, C.A., Eglinton, T.I., Pearson, A., Reddy, C.M., Gustafsson, O., Quinn, J.G., Hartmann, P.C., Hedges, J.I., Prentice, K.M., Kirchstetter, T.W., Novakov, T., Puxbaum, H. and Schmid, H.A. (2002) Critical Evaluation of Interlaboratory Data on Total, Elemental, and Isotopic Carbon in the Carbonaceous Particle Reference Material, NIST SRM 1649a. Journal of Research of the National Institute of Standards and Technology, 107, 279-298.

[37]   Han, Y.M., Cao, J.J., Chow, J.C., Watson, J.G., An, Z.S. and Liu, S.X. (2009) Elemental Carbon in Urban Soils and Road Dusts in Xi’an, China and Its Implication for Air Pollution. Atmospheric Environment, 43, 2464-2470.

[38]   Hansen, A.D.A., Rosen, H. and Novakov, T. (1984) The Aethalometer—An Instrument for the Real-Time Measurement of Optical Absorption by Aerosol Particles. Science of The Total Environment, 36, 191-196.

[39]   Hansen, A.D.A., Kapustin, V.N., Kopeikin, V.M., Gillette, D.A. and Bodhaine, B.A. (1993) Optical Absorption by Aerosol Black Carbon and Dust in Desert Region of Central Asia. Atmospheric Environment, 27, 2527-2531.

[40]   Liu, T.S. (1985) Loess and the Environment. Science Press, Beijing. (In Chinese)

[41]   Wang, X., Peng, P.A. and Ding, Z.L. (2005) Black Carbon Records in Chinese Loess Plateau over the Last Two Glacial Cycles and Implications for Paleofires. Palaeogeography, Palaeoclimatology, Palaeoecology, 223, 9-19.

[42]   Liu, J.Q , Chen, T.M., Nie, G.Y., Song, C.Y., Guo, Z.T., Li, K., Gao, S.J., Qiao, Y.L. and Ma, Z.B. (1994) Dating and Reconstruction of the High Resolution Time Series in the Weinan Loess Section of the Last 150 ka B.P. Quaternary Sciences, 3, 193-202. (In Chinese)

[43]   Qin, X.G., Cai, B.G. and Liu, T.S. (2005) Loess Record of the Aerodynamic Environment in the East Asia Monsoon Area since 60000 before Present. Journal of Geophysical Research, 29, 1-16.

[44]   Qin, X.Q., Mu, Y., Ning, B. and Yin, Z.Q. (2008) Climate Effect of Dust Aerosol in Southern Chinese Loess Plateau over the Last 140,000 Years. Geophysical Research Letters, 36, Article ID: L02707.

[45]   Gundel, L.A., Dod, R.L., Rosen, H. and Novakov, T. (1984) The Relationship between Optical Attenuation and Black Carbon Concentration for Ambient and Source Particles. Science of the Total Environment, 36, 197-202.