WDXRF WDXRF a b c a Analysis of Chemical Species of Water-Insoluble Sulfur Compounds in Rime Ice and Snow and Long-range Transfer Mechanism of Coal Bu
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1 WDXRF a b c a Analysis of Chemical Species of Water-Insoluble Sulfur Compounds in Rime Ice and Snow and Long-range Transfer Mechanism of Coal Burning Emissions under Winter Monsoon Conditions Shoji IMAI a*, Takeshi KAMIMURA b, Kenji KODAMA c and Yuhei YAMAMOTO a a Division of Chemistry, Institute of Natural Science, Graduate School of Technology, Industrial and Social Sciences, Tokushima University 2-1 Minamijosanjima-cho, Tokushima , Japan b Hitachi High-Technologies Corporation 3-31, Miyahara 3-chome, Yodogawa, Osaka , Japan c X-ray Instrument Division, Rigaku Corporation 14-8 Akaoji-cho, Takatsuki, Osaka , Japan (Received 22 January 2018, Accepted 23 January 2018) We have conducted the analysis of chemical species of water-insoluble sulfur compounds in rime ice and snow and used the analysis to propose a long-range transport mechanism for coal-burning emissions in East Asia under winter monsoon conditions. Thin films of insoluble substances included in rime ice and snow on a 0.45 μm pore size membrane filter were analyzed by wavelength-dispersive X-ray fluorescence spectrometry with single dispersive crystal. Using this approach, we could analyze the sulfur-containing chemical species by examining the chemical shift of the S-Kα line. The chemical species containing sulfur were analyzed exclusively from the Ca and S concentrations in the residues of rime ice and snow. Singleparticle analysis of the thin film on the membrane filter was performed for particles with size below 3 μm using a tabletop low-vacuum scanning electron microscopy with energy dispersive X-ray spectroscopy instrument. Particles were classified into six categories according to their compositions. Five major categories of spider chart distribution patterns were identified, and we proposed that they depended on the 24-hour back trajectory, such as Huabei, China, Northeast a shoji.imai@tokushima-u.ac.jp b c X Adv. X-Ray. Chem. Anal., Japan 49, pp (2018) 125
2 China, Korea Peninsula, Heilongjiang-Russia, and Japan types. We could assign the generating area of the air pollutants using the mole ratios of water-soluble Cd, Pb, and nss-so 4 2 species. These categories corresponded with the areas in China based on the isotope ratio of sulfur in Chinese coal and the isotope ratio of Pb collected in Japan. [key words] Sulfur speciation, Inorganic small sphere, Coal, Long-range transfer, Rime, Snow S-Kα X SEM-EDX 5 24 h Cd Pb PM 2.5 PM Cd Pb As SO
3 web PM 2.5 PM 2.5 web Pb// 206 Pb- 207 Pb/ 206 Pb 8 34 S Fig AREA-A AREA-B AREA-B 2 AREA-C AREA-D 1.2 pyrite S VI XRF XPS XAFS XANES X S-Kβ Fig.1 Classification based on isotope ratio of 208 Pb (Group 1 5) 6) and 34 S ; distribution of coal deposits in China 8) and Pb emissions in kg km 2 y 1 9). 127
4 a b Fig.2 (a)back trajectory. (b) PM2.5 in Beijing and Tokushima City X WDXRF S-Kα 28 WDXRF S-Kα 29 S-Kα S VI Ca 1.3 PM 2.5 Jan NOAA HYSPLITS 30 Fig.2 a PM 2.5 Fig.2 b AEROS Fig.2 PM 2.5 PM μg m 3 PM μg m 3 10 μg m 3 1/7 1/8 PM km 1700 km 1/20 PM Vol
5 WDXRF による樹氷と雪の中の非水溶性イオウ化合物の化学形態別分析と東アジアの石炭燃焼排出物の冬期モンスーン下での長距離輸送機構 Fig. 3 Scanning electron microscopy (SEM) image of insoluble species on a membrane filter and a photograph of the membrane filter. 29 ) Fig.3 Scanning electron (SEM) of insoluble species a membrane (a), rime 500 g at Feb. 19, 2013microscopy ( 5000, 3000); (b)image rime 500 g at Feb. 23, 2013 ( on5000, 3000); (c)filter snowand 498agphotograph and (d) rime of 106 g at Jan. 22, 2 29) the6000). membrane filter. (a), rime 500 g at Feb. 19, 2013 ( 5000, 3000); (b) rime 500 g at Feb. 23, 2013 ( 5000, ( 3000); (c) snow 498 g and (d) rime 106 g at Jan. 22, 2014 ( 6000). Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. 本報の 樹氷 とは 気象学的な真の 樹氷 やさえぎり効果 μm による大気エアロ rime を意味する 樹氷は 気温 5 程度で大 ゾル粒子の沈着を誘発する これらの沈着現象 気中の過冷却水が地物に直接接触して風上方向 において表面積の大きな樹氷の沈着効率は 滑 へ生長する氷の結晶の塊であり外見として折り らかな表面をもつ粗氷のそれよりはるかに効率 重なった エビの尻尾 の外観を有する 気温が 的である 大気中のススが効率的に沈着して 黒 10 になると地物に衝突した過冷却水滴は い樹氷 も生成する 4 日間寒気にさらされた 透明な氷として風上へ生長する粗氷を生成す 樹氷への粒子の取り込みを観測した Fig.3 る 樹氷や粗氷に凝結核として取り込む粒子状 四国の山岳における樹氷は Fig.4 に示すよ 物質のサイズは PM2.5 に属する蓄積モード 0.1 うに中国山地に雪を降らせた寒気が再び樹氷を 1 μm の粒子である 樹氷や粗氷が接触する 形成する特徴がある この特徴は 蔵王山系で 寒気を濾過することで慣性衝突効果 3 μm の樹氷の形成過程に類似する Ｘ線分析の進歩
6 Fig.4 Model of formation of rime and snow in Shikoku island. St m m m 20 PM m Cd-Pb m Fig m 130
7 Fig.5 Locations of sampling site m 500 m m PM Black Acid Rime Ice 1990 SEM-EDS Black Acid Rime Ice Black Snow 2013 Black Acid Rime Ice 5. WD-XRF S VI XPS XAFS XANES WDXRF S-Kβ 131
8 WDXR WD-XRF Fig.6 Fig.6 WDXRF spectrum of insoluble substance in rime at Feb. 21, ). Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. Fig.7 Plots of the concentrations of various elements vs. the aluminum concentration in the insoluble fraction of wet depositions 29)., snow ;, rime on No.1;, hard rime on No.1;, rime on No.2;, coal flys ash. Solid line, regression curve for snow; dotted line, regression curve for rime. Reprinted with permission from S. Imai et al.: Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. 132
9 WDXRF による樹氷と雪の中の非水溶性イオウ化合物の化学形態別分析と東アジアの石炭燃焼排出物の冬期モンスーン下での長距離輸送機構 のアルミニウム濃度に対して 鉱物成分には正 の相関関係 Fig.7-Si が得られる Si Mg Na 5.2 S-Kα 線の化学シフト法 児玉ら 5 29 は リガク製 ZSX PrimusII を用い K Ti では強い正の相関関係が得られたが Fe ての高分解モードと高感度モードで測定した Ca P Mn Zn As Pb では相関係数が小さかっ S-Kα 線のピークシフトを利用した冬季湿性沈 た 相関性が低いことは 鉱物質以外の化学種 着中の S VI と S II のスペシエーションの の存在を示す イオウにおいては 二つの正の 可能性を報告した Fig.8 A に示した通り標準 相関関係 Fig.7-S が得られた Ca 濃度とイオ サンプル中の S-Kα 線のピークシフト 化学シ ウ濃度の相関性を利用して有機体と無機態を分 フト を求めた Table 1 の結果が得られた 別定量できた 樹氷では 鉱物質でないが Al Fig.8 B に示したイオウ元素の平均酸化数と と類似の起源をもつイオウ化合物の存在を示唆 の相関関係から濾過物中のイオウの平均酸化数 する 特異的である 有機イオウ化合物である が次式によって求められる と推察される Fig.8 Wavelength Dispersive X-ray Fluorescence data for the insoluble substances in snow and rime together with standard samples29). (A) S-Kα spectrum: a, Na2SO4; b, NaHSO4; c, Na2SO3; d, NaHSO4; e, cystine, f, rime sample at Feb. 21, Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. Ｘ線分析の進歩
10 Table 1 X-Ray spectral chemical shift ( ) of S-Kα peak in standard sustrates. / ev S VI S IV S II S 0 S II Imai 29) Na 2 SO 4 Na 2 SO 3 Na 2 S 2 O 3 Cystine NaHSO 4 NaHSO Kavčič 34) (NH 4 ) 2 SO 4 Na 2 SO 3 TiS ± ±0.04 Fe 2 (SO 4 ) ±0.04 Wenqi 35) inorg.-s VI S IV S 0 inorg.-s' II ~ ~ ~ org.-s VI FeS org.-s II 0.153~ ~ Ito 36) NaHSO 4 NaHSO 3 HOCH 2 SO 2 Na 2H 2 O Sulfer HOCH 2 SO 2 Na 2H 2 O 0.3 [Observed oxidation number] = r 2 = S VI S II Fig.8 C S VI S II f [S(VI)]% = r 2 = f [S( II)]% = 100 f [S(VI)]% 3 XRF Fig.9 Fig.9 Chemical shift (δ) of the standard sample; emission from the incomplete combustion of coal, snow, hard rime, and rime 29). Standar samples: S(VI), Na 2SO 4; S(VI), Na 2SO 3; S(II), NaHSO 4; S( II), cystine. Average,, ±S.D. Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. 134
11 S VI Fig Ca S VI S-Kα Fig.9 Ca S VI [ crustal-s(vi) Ca] rime = [ crustal-ca] rime 4 [ noncrustal-s( II) Ca] rime = [ total-s] rime [ crustal-s(vi) Ca] rime 5 [ total-s] rime [ crustal-ca] rime S Ca [ crustal-s(vi) Ca] rime S VI [ noncrustal-s( II) Ca] rime S II μmol L 1 crust.-s VI S II % f [ crustal-s(vi) M] rime % f [ noncrustal-s( II) M] rime % f [ crustal-s(vi)] rime % = [ crustal-s(vi)] rime /[S] rime f [ noncrustal-s( II)] rime % = [ noncrustal-s( II)] rime /[S] rime Fig.10 S VI Ca Fig.10 Plots of [M] vs. [S] in rime and snow collected in a one-day accumulation in Table 6 in the reference 29). (A), Ca; (B), Si; (C), Al. Solid line is a ratio of [ obs.m] vs.[ obs.s] in the hard rime., snow;, rime;, hard rime at No.1 site., snow at various sites in Japan. Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. Table 2 Mole fraction in percent (%) of S(VI) and S( II) based on the chemical shift of S-Kα and the [M] in hard rime at No.1 site 29). Date σ / ev [Ca] S VI / % S II / % S VI / % S II / % Dec. 24, Jan. 22, Feb. 16, Feb. 21, Average±SD 32.3± ± ± ±
12 Fig.11 Fraction of S(VI) and S( II) of insoluble sulfur 29). Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. Table 2 Ca Fig SEM-EDX ADVANTECH 0.45 μm SEM-EDX 3 μm SEM-EDX SEM TM3000 TM kv 30.0 s EDX-SwiftED3000 EDX Fig.12 Fe Al Si Ca Mg Na K Cr Ni 1 Fe Si Al Ca Mg Na K FA 2 Ti FA FTi 3 Fe Si Al Na K P 1 4 Fe Si Al Ca Mg P 2 5 Fe Si Al Si P 3 6 Fe UPFe Fig.13 ISP inorganic sphere particulate h FA FTi AREA-A P 1 AREA-B AREA-B 2 P 3 AREA-C UPFe AREA-D 5 Fig
13 Fig.12 SEM image and energy dispersive X-ray spectra of small inorganic spherical particles in the residues of rime. Reprinted with permission from S. Imai et al. Anal. Sci., 34, accepted for publication (2018). Copyright (2018) Japan Society for Analytical Chemistry. Fig.13 Hexagonal diagram models of distribution of inorganic small spherical particles in winter wet depositions collected at the summit of Mt. Kajigamori (St.1) and aerosol in Tokushima City, Japan 10, 11). Cited with backtrajectry Hexagonal chart pattern: (A) Huabei chart, (B) Dongbei chart, (B 2) Korea Peninsula chart, (C) Heilongjiang- Primorsk Russia chart, (D) Japan urban chart. 137
14 Fig.14 Locations of the regions of origin of atmospheric aerosols containing inorganic small spherical particles reported in previous works 10). Categories: A, Hebei, China; B, south area of North East China; B 2, Korea Peninsula; C, north area of North East China and Maritime Province in Russia; D, Japan. Reprinted with permission from S. Imai et al.: Bunseki Kagaku, 67, 95 (2018). Copyright (2018) Japan Society for Analytical Chemistry. 6.2 Pb-Cd Pb Cd Pb/Cd Pb/Cd Pb/Cd Pb/Cd = Pb Cd Fig.15 ISP AREA AREA-C Pb Cd AREA-C Pb Cd Pb/Cd ISP 138
15 5.0 (c) [Pb] / µg L a 1.0 b [Cd] / µg L -1 Fig.15 (a), (b) Plots of [Pb] vs. [Cd ] of rime ( ) and snow ( ) samples collected on Mt. Kajigamori 37). (a) data of the same day collection of rime and snow. S 1: Dec. 24, 2013 ; S 2: Feb. 19, (b) all data in 2014 y. ~2008 y. Line1: [Pb]=32.56 [Cd] 1.0 (r 2 =0.9008); Line 2: [Pb]= [Cd] (r 2 =0.9676). Reprinted with permission from S. Imai et al.: Bunseki Kagaku, 66, 95, (2017). Copyright (2018) Japan Society for Analytical Chemistry. (c) Plots of Pb and Cd shown in Table 1 in the reference 38). Categories:, AREA-C;, AREA-D. Correlation curve: Line a for of AREA-C, Line b for of AREA-D. Regression line obtained in remote area: Line 1, AREA-A; Line 2, AREA-B; Line-3, AREA-B 2. Reprinted with permission from S. Imai et al. Bunseki Kagaku, 67, 95 (2018). Copyright (2018) Japan Society for Analytical Chemistry. ISP AREA-A Pb/ Cd AREA-B 2 72 h AREA-B 48 h AREA-A 24 h AREA-B M Cd Pb SO Fig.16 [Pb] [nss-so 2 4 ] [Cd] [nss-so 2 4 ] [Pb] [nss-so 2 4 ] Fig.16 a Dec Dec Jan Jan Pb Feb P 1 Feb P 2 nss-so 2 4 Fig.16 b rime Pb [Pb] = 1.60 [nss-so 2 4 ] r 2 = rime Pb s-rich: [Pb] = [nss-so 2 4 ]
16 Fig.16 Plots of [Pb] vs. [nss-so 2 4 ] and [Cd] vs. [nss-so 2 4 ] in rime and snow 37). (a), (c) snow: 2014, 2013, 2012; 2011, 2010, 2009, 2008, same day sampling of rime and snow. (b) rime: 1. Jan. 22, 2014; 2. Feb. 9, 2012; 3. Jan. 23, 2013; 4. Feb. 16, 2012; 5. Feb. 29, 2012; 6. Dec. 28, 2013; 7. Feb. 16, 2014; (d) rime: 1. Jan. 5, 2014 ; 2. Jan. 22, 2014; 3. Jan. 23, 2013; 4. Feb. 9, Jan. 29, 2012; 6. Feb. 16, 2013; 7. Mar. 14, 2013; 8. Dec. 28, (a), (c): line 1, regression line (solid) of same day sampling group (?) with standard error (dotted). (b), (d): line 1 and line 2 for regression line (solid) of the sample with standard error (dotted). Reprinted with permission from S. Imai et al.: Bunseki Kagaku, 66, 95 (2017). Copyright (2018) Japan Society for Analytical Chemistry. r 2 = rime Pb line 1 rime Pb s-rich line 2 nss-so 2 4 nss-so 2 4 line 2 [Cd] [nss-so 2 4 ] Fig.16 c Cd nss-so 2 4 Fig.16 d rime Cd [Cd] = [nss-so 2 4 ] r 2 = rime Cds-rich: [Cd] = [nss-so 2 4 ] r 2 = rime Cd rime Cd s-rich nss-so 2 4 line 2 nss- 140
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