Geo log i cal Quar terly, 2005, 49 (2): 235–242
The sul phur and ox y gen iso to pic com po si tion of Lower Cam brian an hyd rites in East Si be ria
Tadeusz M. PERYT, Stanis³aw HA£AS, Volodymyr M. KOVALEVYCH, Oleh Y. PETRYCHENKO and Nodar M. DZHINORIDZE
Peryt T. M., Ha³as S., Kovalevych V. M., Petrychenko O. Y. and Dzhinoridze N. M. (2005) — The sul phur and ox y gen iso to pic com po si - tion of Lower Cam brian an hyd rites in East Si be ria. Geol. Quart., 49 (2): 235–242. Warszawa.
Pub lished sul phur and ox y gen iso tope age curves for the late Neoproterozoic–Early Cam brian time in ter val have been based on stud ies of sul phate in ter vals of the East Si be rian salt gi ant. We re port here on sul phur and ox y gen mea sure ments for sul phate dis persed in, or form ing laminae in, the rock salt de pos its in all Lower Cam brian bas ins of East Si be ria. Sul phur iso tope data for 26 sam ples of Lower Cam brian an hyd rites from East Si be ria range from +22.6 to +34.5‰. No dif fer ence was ob served be tween dif fer ent suites and be tween sam ples taken from anhydrite in ter ca la tions in rock salt and from wa ter-in sol u ble res i due in rock salt. Ox y gen iso tope data for 25 anhydrite sam ples range from +12.4 to +17.8‰, and thus d18O val ues have a smaller range of vari a tion (5.5‰) than d34S (11.8‰) over the en tire set of Lower Cam brian an hyd rites. The great d34S vari abil ity ob served in the Lower Cam brian of Si be ria seems to re flect mix - ing of sulphates com ing from the ocean and due to the riverine in put. The low est d18O val ues may in di cate the in put val ues from both the sources, whilst the high est value may re sult from iso tope ex change be tween SO42-
and wa ter. Our re sults com bined with data pro vided by pre vi ous work ers could in di cate a clear strati graphic trend in d34S val ues, with a re mark able fall of ca. 9‰ in d34S value dur ing the ear li - est Cam brian and then a slight rise in d34S val ues in the youn ger part of Early Cam brian. How ever, if only the high est val ues are taken, the mea sured val ues are com pat i ble with sea wa ter d34S³30‰ dur ing the en tire Early Cam brian. Sul phur iso to pic com po si tion of sul phate min er als did not be come heavier from the sul phate stage to ward the chlo ride stage.
Tadeusz Marek Peryt and Volodymyr M. Kovalevych, Pol ish Geo log i cal Institute, Rakowiecka 4, PL-00-975 Warszawa, Po land, e-mail:
Tadeusz.Peryt@pgi.gov.pl; Stanis³aw Ha³as, In sti tute of Phys ics, Maria Cu rie-Sklodowska Uni ver sity, PL-20-031 Lublin, Po land, e-mail: halas@tytan.umcs.lublin.pl; Volodymyr M. Kovalevych and Oleh Y. Petrychenko, In sti tute of Ge ol ogy and Geo chem is try, Na - tional Acad emy of Sci ences of Ukraine, Naukova 3a, 79053 Lviv, Ukraine, e-mail: igggk@ah.ipm.lviv.ua; Nodar M. Dzhinoridze,VNIIG Stock Co., Sankt Pe ters burg, Rus sia (re ceived: No vem ber 10, 2004; ac cepted: Feb ru ary 7, 2005).
Key words: Si be ria, Lower Cam brian, evaporites, sul phur iso topes, ox y gen iso topes.
INTRODUCTION
A sharp in crease in d34S val ues oc curred in ma rine sulphates some time dur ing the late Neoproterozoic, which was sus tained un til the end of Early Cam brian (Claypool et al., 1980), with the max i mum val ues known from the late Neoproterozoic (Vinogradov et al., 1994; Strauss et al., 2001).
Sim i lar high d34S val ues have been re ported from phosphorites from the Pre cam brian-Cam brian bound ary sec tion in Meishucun, China (Shields et al., 1999) and from the up per Neoproterozoic Doushantuo For ma tion, South China (Shields et al., 2004). In con trast, ox y gen iso tope data for this time in ter - val show no ma jor changes (Claypool et al., 1980).
Pub lished sul phur and ox y gen iso tope age curves have been based, in large part as far as the late Neoprote - rozoic–Early Cam brian time in ter val is con cerned, on stud ies of the East ierian salt gi ant (Claypool et al., 1980), al though the mea sured set of d18O val ues was lim ited (6 re sults).
Claypool et al. (1980) and Pisarchik and Golubchina (1975) sam pled sul phate in ter vals, and re sults re ported by Pustylnikov (1976) re fer to both anhydrite and rock salt in ter - vals of the evaporite se quence. We re port here on sul phur and ox y gen mea sure ments for sul phate dis persed in, or form ing laminae in, the rock salt de pos its in all Lower Cam brian bas - ins of East Si be ria, aim ing to ex plain re corded vari a tions in d34S and d18O in the Lower Cam brian of Si be ria.
GEOLOGICAL SETTING AND SAMPLE MATERIAL
Salt de pos its of late Vendian to Early Cam brian age in East Si be ria cover an ex ten sive ter ri tory (ca. 2 mil lion km2) lo cated to the north-west of Lake Baikal (Fig. 1). The thick ness of the up - per Vendian–Lower Cam brian suc ces sion is 2.0–2.5 km in the south ern, west ern, and cen tral parts of the ba sin, and 1.3–1.5 km in the NE part (Nepa-Vilyui). This sa line gi ant (to tal vol ume of up per Vendian–Lower Cam brian evaporites is 785.000 km3 — Zharkov, 1984) is char ac ter ized by the oc cur rence of four teen re gional marker car bon ate units and 15 salt units (Chechel et al., 1977; Zharkov, 1984, with ref er ences therein). Five ma jor phases of salt de po si tion can be dis tin guished, in the late Vendian (Danilovo) and Early Cam brian (Usolye, Belsk, Angara, and Litvintsevo) bas ins (Fig. 2) Chechel et al. (1977), Zharkov (1984), Kuznetsov et al. (2000). Pre vi ously (Chechel et al., 1977; Zharkov, 1984) the lat ter ba sin was con sid ered to be of Mid dle Cam brian age (Amgan) but now it is ac cepted as be long - ing to the mid dle Toyonian (Kuznetsov et al., 2000).
The area oc cu pied by par tic u lar bas ins as well as the av er - age thick ness of evaporite de pos its de creased with time. The area of the old est, Usolye salt ba sin was al most 2 mil lion km2, and the av er age thick ness of de pos ited salt 200 m (Zharkov, 1981), while the area of the youn gest, Litvintsevo salt ba sin on a 0.5 mil lion km2 and the av er age thick ness of its evaporite de - pos its (rock salt and anhydrite) 50 m (Zharkov, 1984). De po si - tion took place in a deep wa ter ba sin: Petrichenko (1988, ta ble 13) eval u ated that at the ter mi na tion of ha lite de po si tion the depth was 50–260 m, and at the on set of pot ash de po si tion it was 10–50 m. It should be men tioned that Pustylnikov (1976) as sumes that the Cam brian evaporite ba sin of Si be ria was rel a - tively shal low, but for him shal low means a hun dred me tres or less (Pustylnikov, 1976, p. 58).
Our sam ples come from all four of the Early Cam brian bas - ins al though the larg est data set is from the Angara suite (Ta - ble 1). The sam ples from the Angara Suite are from the mid dle part of the Suite (Zhigalovo, Bratsk and Nepa ar eas) and the up per part (Taseyevo and Mirnyi ar eas).
METHODS
Most sam ples were taken from anhydrite in ter ca la tions (laminae) in rock salt and from anhydrite-dom i nat ing wa ter in sol u ble res i due in rock salt. One sam ple was taken from gyp sum cap rock, and one from an anhydrite-ce lest ite nest in car bon - ate rock. The sam ples were pow dered in an ag ate mor tar, then ca. 100 mg of the pow der was dis solved in dis tilled wa ter acid i fied with HCl to pH = 1. The dis so lu tion was per formed in 250 mL glass beak ers filled to ca. 1/3 of their vol ume. The beak ers were cov ered by watch glasses, and stored in an ex haust un der a fume hood over sev eral days, they were and stirred sev eral times a day. Af ter dis so lu tion of sulphates the sol - utes were fil tered to small glass beak ers and BaSO4 was pre cip i tated by means of acid i fied (with HCl) so lu tion of BaCl. The pre cip i tate was washed by dis tilled wa ter sev eral times un til dis ap pear ance of the chlo ride ion, which was tested in the re - main ing fil trate us ing by 10% AgNO3 so - lu tion. Clean BaSO4 re main ing in small beak ers was dried in an oven at 100°C and then sub jected to the pro ce dures for quan ti - ta tive ex trac tion of sul phur and ox y gen for iso tope anal y sis. Un der the con di tions as de scribed no in flu ence of iso tope ex change be tween sul phate ion and wa ter was ob - served due to low am bi ent tem per a ture (16 to 18°C) and the es cape of a ma jor frac tion of HCl from the beak ers within a few hours to the at mo sphere.
Fig. 1. Lo ca tion map show ing the stud ied bore holes
Black quad ran gle N of Bratsk area in di cates the lo ca tion of bore holes sam pled by Claypool et al. (1980)
The iso to pic com po si tions, d34S and d18O, were an a lyzed by a dual in let and tri ple col lec tor mass spec trom e ter on SO2 and CO2 gases, re spec - tively. SO2 was ex tracted by the method de vel oped in the Lublin lab o ra tory (Halas and Szaran, 2001, 2004), whereas CO2 was pre pared by the method de scribed by Mizutani (1971). We used typ i cally 8 to 12 mg of BaSO4 in each prep a ra tion, how ever, where nec es sary we were able to an a lyze 1 mg BaSO4. The reproducibility of both anal y ses (2 stan dard de vi a tions), ob tained on the ba sis of rep - li cated SO2 ex trac tions, was about 0.16‰. Delta val ues were nor mal ized to the CDT and the VSMOW scales by anal y sis of the NBS-127 stan - dard, for which we as sumed d34 S = 21.14‰
(Halas and Szaran, 2001) and d18O = 9.91‰ ac - cord ing to our re cent cal i bra tion per formed vs.
VSMOW wa ter stan dard.
The sulphur and oxygen isotopic composition of Lower Cambrian anhydrites in East Siberia 237
Fig. 2. Stra tig ra phy of the up per Vendian–Mid dle Cam brian de pos its of East Si be ria (af ter Kuznetsov et al., 2000 and Khomentovsky and Karlova, 2002)
T a b l e 1 Sul phur and ox y gen iso tope re sults for Lower Cam brian sulphates of East Si be ria
RESULTS
Sul phur iso tope data for Lower Cam brian an hyd rites (Ta - ble 1) ranged from +22.6 to +34.5‰ ex cept for one very low value (+7.3‰) re corded in a sam ple from the Usolye Suite.
No sig nif i cant dif fer ences were ob served be tween the over all ranges of the iso to pic val ues from dif fer ent suites (Fig. 3), al - though the sam ples from the Belsk Suite show d34S val ues close to the lower limit of the range. Sim i larly, there are no sig nif i cant dif fer ences be tween sam ples taken from anhydrite in ter ca la tion in rock salt and from wa ter-in sol u ble res i due in rock salt. The ranges of d34S val ues for sam ples from the mid - dle part of the Angara Suite (+22.8 to +34.0‰) and from the up per part of the suite (+26.0 to +32.3‰) do not dif fer much, but the av er age d34S val ues do dif fer sub stan tially for anhydrite from the mid dle and up per part of the Angara Suite (+27.5‰ and +30.8‰, re spec tively). d34S value for gyp sum from the Angara Suite is +21.6‰, and for ce lest ite +32.8‰.
Ox y gen iso tope data for Lower Cam brian an hyd rites (Ta - ble 1) range from +12.5 to +17.8‰ ex cept for one sam ple with lower value (+11.9‰) from the Usolye Suite show ing very low d34S (this value is not shown in Fig ure 3). Other sam ples from the Usolye Suite show low d18O val ues, and there is no es sen tial dif fer ence be tween ranges of d18O val ues among other suites (Fig. 3). The av er age d18O value for the mid dle part
of the Angara Suite is +16.1‰ and for the up per part +15.7‰.
d18O value for the Angara gyp sum sam ple is +13.4‰, and for the ce lest ite +15.0‰.
INTERPRETATION AND DISCUSSION
Most our sam ples come from the Angara Suite. The range of d34S vari a tion, and the av er age d34S value, in our data set from the Angara Suite are sim i lar to those re corded by Claypool et al. (1980) (Fig. 4) al though our sam ples de rive from the chlo - ride fa cies whereas the sam ples an a lyzed by Claypool et al.
(1980) are from the sul phate fa cies. The cal cu lated T-test value for both data sets is 0.70 whilst the cut-off value at 0.05 prob a - bil ity level is 1.96, there fore the dif fer ence be tween the two av - er ages is sta tis ti cally in sig nif i cant. Ac cord ingly, there is no trend sug gest ing that the sul phur iso to pic com po si tion of sul - phate min er als be comes heavier from the sul phate stage to ward the chlo ride stage, as it was re corded in the De vo nian Prypiac’
Ba sin of Belarus (Makhnach et al., 2000). It should be noted that both the De vo nian Prypiac’ Ba sin of Belarus (Petrychenko and Peryt, 2004) and the Lower Cam brian ba sin of East Si be ria (Kovalevich et al., 1998, Kovalevych et al., 2003) were char ac - ter ized by the same, Ca2+-rich, SO42--poor sea wa ter, and there - fore their dif fer ent be hav iours can not be at trib uted to the dif fer - ent chem i cal com po si tion of par ent seawaters.
The only sam ple from the Litvintsevo Suite (Ta ble 1) yielded d34S value very close to our and Claypool et al. (1980) av er age val ues for the Angara Suite. It should be noted that the av er age val ues of d34S given by Pisarchik and Golubchina (1975) and Pustylnikov (1976) for the Angara Suite are clearly lower than ours (Fig. 4) due to a shift of range of d34S vari a tion to wards the lower val ues (Fig. 4). Pustylnikov (1976) no ticed that in the up per part of the Angara Suite, d34S val ues are lower than in the mid dle part (by about 4–5‰) and ex plained this by re lat ing it to the in creas ing brine con cen tra tion. A sim i lar gen - eral trend is also ap par ent from data given by Claypool et al.
(1980). How ever, our data set does not con firm this trend.
Sparse d34S val ues given by Pisarchik and Golubchina (1975) and by us for the Belsk Suite are within our range of d34S vari a tion for the Angara Suite (Fig. 4). d34S val ues for the Usolye Suite are sim i lar to val ues char ac ter is tic for the Angara Suite (Fig. 4), and the range of our two val ues is sim i lar to that re ported by Pustylnikov (1976). One (of two) val ues re ported by Pisarchik and Golubchina (1975) is within the range of d34S vari a tion for the Usolye Suite given by Pustylnikov (1976) whereas the sec ond value is lower.
We did not an a lyze sam ples from the late Vendian evaporite ba sin of East Si be ria, Danilovo one, but con sid er ing the data re ported by Vinogradov et al. (1994, ta ble 3 and fig. 11), the anhydrite sam ples from do lo mite com plexes show d34S val ues of +33.5 to +35.7‰. Tak ing into ac count those data in ad di tion to our data, d34S val ues for the up per Ven - dian-Lower Cam brian an hyd rites of East Si be ria show a large range (13‰). Sim i lar large ranges have been found for the mid - dle and up per Vendian of East Si be ria (Vinogradov et al., 1994), and con sid er ing our re sults as well as data of pre vi ous
Fig. 3. Plot of d18O and d34S val ues in stud ied sam ples C — ce lest ite, G — gyp sum, no let ter — anhydrite
The sulphur and oxygen isotopic composition of Lower Cambrian anhydrites in East Siberia 239
work ers it can be con cluded that there is a clear strati graphic trend for par tic u lar suites (Fig. 4), with a re mark able fall of ca.
9‰ in d34S value dur ing the ear li est Cam brian (see ranges and av er age val ues for Usolye and Danilovo Suites), and then a slight rise in d34S val ues in the Belsk, Angara and Litvintsevo Suites (Fig. 4). How ever, the sta tis ti cal con strains of the above-men tioned trend is weak due to a small num ber of sam - ples. In ad di tion, if one takes high est val ues only for bas ins with lower out li ers, then mea sured val ues are com pat i ble with sea wa ter d34S ³ 30‰ dur ing the en tire Early Cam brian.
Sim i lar large ranges in d34S val ues were rec og nized in ter mi - nal Neoproterozoic to Lower Cam brian evaporite se quences of Hormuz For ma tion, Iran (Hought on, 1980) and Hanseran For - ma tion, NW In dia (Strauss et al., 2001). De spite the ap par ent het er o ge ne ity in the en tire set of the d34S val ues for the Hanseran evaporites, Strauss et al. (2001) rec og nized a clear strati graphic trend for the dif fer ent drill cores and in ter preted it as due to sec u - lar vari a tion in sea wa ter iso to pic com po si tion. Their data in di - cate that in par tic u lar cy cles, sulphates from ha lite units show clearly higher d34S val ues com pared to those re corded in non-ha -
lite in ter vals. This could in di cate closed sys tem con di tions with im por tant role played by bac te rial sul phate re duc tion (Strauss et al., 2001) in a ba sin partly sep a rated from the open ocean. As men tioned ear lier, our data in di cate that in the Lower Cam brian of East Si be ria there is no such shift to wards more pos i tive val - ues with in creas ing brine con cen tra tion. There fore, such a great d34S vari abil ity as ob served in the Lower Cam brian of Si be ria seems to be mostly re lated to the strong bac te rial sul phate re duc - tion con tem po ra ne ous with evaporite de po si tion as well as to the in flux of riverine sulphates re sult ing from con ti nen tal weath er - ing (cf. Strauss et al., 2001). The lat ter fac tor was of ma jor im - por tance dur ing for ma tion of sulphates of the Up per Lena Se ries which over lies the Litvitsevo Suite as in di cated by d34S val ues rang ing from 5.4 to 9.75‰ (Pisarchik et al., 1977), and one sam - ple from the Usolye Suite show ing d34S value of 7.30‰ seems to re flect the in flux of riverine sul phate.
The range of d18O (SO4) vari a tion re corded by us is greater than that given by Claypool et al. (1980) (Fig. 4). At the same time, av er age d18O in our data set is ca. 3‰ higher than that re - corded by Claypool et al. (1980). In their study of mod ern salt
Fig. 4. Sul phur iso to pic com po si tion of Lower Cam brian sulphates of East Si be ria and some other up per Neoproterozoic and Lower Cam brian evaporites and phosphorites
The cur rent strati graphic po si tion of sam ples from Aus tra lia (Sol o mon et al., 1971) af ter Weste (1994); the num - ber above each seg ment in di cates the num ber of sam ples mea sured by each au thor
pans in Slovenia, Pezdiè et al. (1998) re corded that the high est d18O value was char ac ter is tic for a me dium evap o ra tion stage (35–160‰ of sa lin ity) and thus the dif fer ence can not be ex - plained by that Claypool et al. (1980) used sam ples from the gyp sum fa cies whereas we used sam ples mostly from the ha lite fa cies. Ac cord ingly, we in ter pret the dis crep ancy be tween our data sets as due to a smaller data set of d18O val ues given by Claypool et al. (1980). On the other hand, d18O val ues have a smaller range of vari a tion (5.5‰) than d34S (11.8‰) when the en tire set of Lower Cam brian an hyd rites is con cerned (Fig. 3).
Lu et al. (2001) con cluded that re dox re ac tions could sig nif i - cantly change d34S and d18O val ues for nor mal ma rine dis solved sul phate be fore they pre cip i tated solid sul phate. In the deeper-wa ter ba sin both d34S and d18O of dis solved sul phate can have large vari a tions, and in the shal low wa ter pan en vi ron ment, d34S and d18O vari a tion is small, and the d34S vari a tion is greater than that of d18O (SO4) (Lu et al., 2001). Our data in di cate that both d34S and d18O can vary greatly and that the d34S vari a tion is greater than that of d18O, al though the depth of the Early Cam - brian salt ba sin was 50–260 m as sug gested by the cor re spond ing pres sure in fluid in clu sions (Petrichenko, 1988, p. 42).
An other rea son of high d18O val ues re corded in the in ves ti - gated evaporites seems to be the ox y gen iso tope ex change re ac - tion be tween sul phate ion and wa ter, prior to CaSO4 pre cip i ta - tion. The re ac tion rate may be en hanced by rel a tively high tem - per a ture and low pH of wa ter (Kusakabe and Rob in son, 1977).
Re cently Ha³as and Pluta (2000) pub lished the fol low ing em - pir i cal “iso tope ther mom e ter” for low tem per a ture brines:
103ln a = 2.41× 106/T2–5.77
where: a =( / )
/ )
18 16
16
O O
( O O
sulphate
18 water
For the com plete iso tope ex change re ac tion this ther mom e - ter yields a sen si ble range for 103ln a be tween sul phate ion and wa ter at tem per a tures 10 to 40°C.
The ob served d18O in the anhydrite is higher by about 3.5‰ than in the mother so lu tion due to iso tope frac tion - ation dur ing crys tal li za tion (Claypool et al., 1980). There - fore, ac cord ing to the Ta ble 2, the com plete iso tope ex - change at 40°C re quires as sump tion of ca. –5‰ for d18O of the ba sin wa ter. As sum ing tem per a ture of sea wa ter <30°C, the com plete ex change re quires wa ter with d val ues be tween –6 and –10‰ in the ba sin, which seems to be un re al is tic. For this rea son we pos tu late that the iso tope ex change was rather in com plete, i.e. the iso tope equi lib rium was not at tained, but the pro cess was likely much more ad vanced than it is en - coun tered in the mod ern salt pans.
CONCLUSIONS
Sul phur iso tope data for 26 sam ples of Lower Cam brian an - hyd rites from East Si be ria range from +22.6 to +34.5‰ (ex cept for one very low value). No dif fer ence was ob served be tween dif fer ent suites and be tween sam ples taken from anhydrite in - ter ca la tions in rock salt and from wa ter-in sol u ble res i due in rock salt. Ox y gen iso tope data for 25 anhydrite sam ples range from +12.4 to +17.8‰ (ex cept for one lower value), and thus d18O val ues have a smaller range of vari a tion (5.5‰) than d34S (11.8‰) over the en tire set of Lower Cam brian an hyd rites.
Those re sults com bined with data pro vided by pre vi ous work ers in di cate a clear strati graphic trend in d34S val ues, with a re mark able fall of ca. 9‰ in d34S value dur ing the ear li - est Cam brian and then a slight rise in d34S val ues in the Belsk, Angara and Litvintsevo Suites. It is con cluded that in the Early Cam brian salt ba sin of East Si be ria sul phur iso to pic com po si tion of sul phate min er als did not be come heavier from the sul phate stage to ward the chlo ride stage. The great d34S vari abil ity ob served in the Lower Cam brian of Si be ria seems to re flect mix ing of sulphates com ing from two sources: 1 — the ocean, were a ma jor frac tion was sub ject to bac te rial re duc tion yield ing very high val ues, and 2 — the riverine in put yield ing iso to pi cally light sulphates re sult ing from con ti nen tal weath er ing.
d18O val ues in the in ves ti gated evaporitic sulphates are uni - formly dis trib uted from 12.5 to 18‰. The low est value re flects d18O of the in put sul phate ions (ei ther oce anic or riverine) whereas the high est value cor re sponds to the ions with the high est pos si ble de gree of the iso tope ex change.
Ac knowl edge ments. The study re sulted from the Pol ish State Com mit tee on Sci en tific Re search re search grant No. 3 P04D 010 22 (to V. Kovalevych). G. A. Shields read the first draft of the pa per and of fered many use ful com ments, and the fi nal manu script bene fited from crit i cism and sug ges tions by the jour nal re view ers A. Longinelli and G. A. Shields.
T
[oC] 103 ln a
10 24.29
20 22.27
30 20.45
40 18.81
T a b l e 2 Ox y gen iso tope frac tion ation be tween sul phate ion and wa ter for equi lib rium
at low tem per a tures
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