TCVN 4920:2007

ISO 925:1997
NHIN LIU KHONG RN - XC NH HM LNG CACBON CACBONAT - PHNG PHP
KHI LNG
Solid mineral fuels - Determination of carbonate carbon content - Gravimetric method

Li ni u
TCVN 4920:2007 thay th TCVN 4920:1989.
TCVN 4920:2007 hon ton tng ng vi ISO 925:1997.
TCVN 4920:2007 do Tiu ban K thut Tiu chun TCVN/TC27/SC3 Nhin liu khong rn - Than
bin son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc v Cng ngh cng b.

NHIN LIU KHONG RN - XC NH HM LNG CACBON CACBONAT - PHNG PHP

KHI LNG
Solid mineral fuels - Determination of carbonate carbon content - Gravimetric method
1. Phm vi p dng
Tiu chun ny quy nh phng php khi lng xc nh cacbon trong cacbonat khong lin kt vi
nhin liu khong rn.
CH THCH Kt qu thu c bao gm c cacbon t cacbon dioxit kh quyn c nhin liu hp
th.
2. Ti liu vin dn
Cc ti liu vin dn sau l cn thit khi p dng tiu chun ny. i vi cc ti liu vin dn ghi nm
ban hnh th p dng bn c nu. i vi cc ti liu vin dn khng ghi nm ban hnh th p dng
phin bn mi nht, bao gm c cc bn sa i (nu c).
TCVN 318 (ISO 1170) Than v cc - Tnh kt qu phn tch trn nhng c s khc nhau.
TCVN 1693 (ISO 1988) Than - Ly mu.
TCVN 4919 (ISO 687) Cc - Xc nh m trong mu phn tch.
ISO 1015:1992 Brown coal and lignites - Determination of moisture content - Direct volumetric method
(Than nu v than non - Xc nh hm lng m - Phng php th tch trc tip).
ISO 2309:1980 Coke - Sampling (Cc - Ly mu).
ISO 5068:1983 Brown coal and lignites - Determination of moisture content - Indirect gravimetric
method (Than nu v than non - Xc nh hm lng m - Phng php khi lng gin tip).
ISO 5069-2:1983 Brown coal and lignites - Principles of sampling - Part 2: Sample preparation for
determination of moisture content and for general analysis. (Than nu v than non - Nguyn tc ly
mu - Phn 2: Chun b mu xc nh hm lng m v phn tch chung).
ISO 9411-1:1994 Solid mineral fuels - Mechanical sampling from moving streams - Part 1: Coal.
(Nhin liu khong rn - Ly mu c hc trn dng vn chuyn - Phn 1: Than).
ISO 9411-2 1994 Solid mineral fuels - Mechanical sampling from moving streams - Part 2: Coke.
(Nhin liu khong rn - Ly mu c hc trn dng vn chuyn - Phn 2: Cc).
3. Nguyn tc
Mu c khi lng bit c x l bng axit clohydric, axit clohydric phn ng vi cacbonat c
trong mu gii phng cacbon dioxit. Cacbon dioxit thu c t s phn hy ca cacbonat c
hp th v cn.
4. Thuc th
CNH BO Phi cn thn khi tip xc vi thuc th, v nhiu thuc th c tnh c v n mn.
Trong qu trnh phn tch, nu khng c quy nh khc, ch dng ha cht loi tinh khit phn tch v
ch dng nc ct hoc nc c tinh khit tng ng.
CH THCH C th loi b cacbon ioxit trong nc ct bng cch un si nh trong vng 15 pht.
4.1. Axit clohydric, khong 3 mol/lit
4.2. Cht hp th hydro sunfua
Bt c cht no trong s cc cht sau:
a) ng (II) phosphat, dng ht, kch thc ht t 1,2 mm n 0,7 mm;
CH THCH 1 ng (II) phosphat dng ht c th chun b nh sau:
Trn thuc th bt ng (II) phosphat vi 1 % dung dch h tinh bt thnh hn hp qunh. p hn hp
qua l kim loi c t l ng knh khong 1 mm. Sy kh vt liu n ra nhit 110 oC v sng
c kch thc yu cu.
b) ng (II) sulfat, c mang trn nn cht mang l bt nghin;
CH THCH 2 Cht hp th thch hp, da trn ng (II) sulfat, c th c chun b nh sau:
Chun b bt bng cch p v sng nhn c cp ht t 2,8 mm n 0,7 mm. Chuyn
khong 60 gam bt chun b vo mt cho lm kh, ph ln bng dung dch ng (II) sulfat bo
ha, lm bay hi n kh c khuy u, ri gia nhit nhit 150 oC n 160oC trong 3 gi n 4
gi. Lm ngui trong bnh ht m v bo qun trong chai thy tinh nt nhm.
c) bc sunfat, dng ht.
4.3. Magie perclorat, khan, kch thc ht t 1,2 mm n 0,7 mm.
CNH BO Khi loi b magie perclorat L kit, phi lm theo quy nh k thut. Khng c
c gng ti sinh magie perclorat, do c nguy him n.
4.4. Natri hydroxit, bo qun trong mi trng tr, tt nht l loi th, v d 1,7 mm n 1,2 mm, v
tt nht l loi t ch th.
4.5. Cht thm t, ph hp s dng trong dung dch axit
Ch thch Tc nhn thm nc dng lng nng 100 ml/l hoc etanol (95 % th tch) l ph hp.
4.6. Thuc th cho php th kim tra
S dng mt trong hai loi sau
a) natri cacbonat khan;
b) canxi cacbonat khan.
5. Thit b, dng c
5.1. Cn phn tch, c kh nng cn chnh xc n 0,1 mg.
5.2. Dng c bng thy tinh c chia , ph hp cc yu cu i vi loi A trong Tiu chun tng
ng v: Dng c thy tinh dng cho phng th nghim v cc thit b lin quan.
5.3. ng lc, gm ng hp th1) cha natri hyroxit bo qun trong mi trng tr (4.4).
5.4. Cm bnh phn ng, gm mt bnh tht c y trn 300 ml lp vi phu c van, mt ng sinh
hn hai lp v mt ng c bu.
5.5. Cc ng hp th, gm 3 ng hp th a), b) v c) nhi ln lt cc cht sau:
a) magie perclorat (4.3) lm kh kh;
b) cht hp th hydro sunfit (4.2) tip theo l lp bo v magie perclorat (4.3). Kt ni t ng ny n
ng c) phi c lp ti u thot ra ca ng bng mt van hoc thit b ng kn khc;
c) natri hydroxit bo qun trong mi trng tr (4.4) hp th cacbon dioxit sinh ra trong bnh phn
ng, tip theo l lp bo v magie perclorat (4.3) hp th nc to ra trong phn ng gia cacbon
dioxit v natri hydroxit. ng ny phi c lp vi kha van hoc thit b ng kn khc ti u vo
hoc u ra.
5.6. Thit b lu thng khng kh
Bm ht c kh nng rt khng kh vi tc 50 ml/pht qua thit b, ni qua mt lu lng k n
mt ng ni ch T c kha van (l thng khng kh).
5.7. Ngun nhit, dng cho bnh phn ng
Bp in hoc bp ga nh cung cp nhit cho bnh dung tch 300 ml.
V d v mt b dng c lp rp ph hp c minh ha trn Hnh 1.

1)
ng hp th c th l ng hnh ch U hoc ng Midvale (loi gim p lc ngc v do , nguy
him r r) Pha trn ca ct thuc th phi c y bng np bng thy tinh trnh s xm nhp
ca ht bi nh ngoi khng kh.
 Hnh 1 - B dng c lp rp ph hp
6. Chun b mu th
Mu th l mu phn tch c chun b ph hp vi TCVN 1693 (ISO 1988), ISO 2309, ISO 5069-2,
ISO 9411-1 hoc ISO 9411-2 tng ng. Phi m bo hm lng m ca mu cn bng vi mi
trng phng th nghim, nu cn ri mu thnh lp mng trong khong thi gian ngn nht t
c cn bng.
Trc khi bt u xc nh, trn u mu th cn bng t nht l mt pht, tt nht l trn bng
my.
Nu cc kt qu c tnh ton khc vi trng thi kh khng kh (xem iu 8) th, s dng phn khc
ca mu th (xem 7.2) xc nh hm lng m theo phng php m t trong ISO 687, ISO 1015
hoc ISO 5068 tng ng.
7. Cch tin hnh
7.1. Php th kim tra
Kim tra kn khng kh ca thit b v trng thi ca cc thuc th bng cch tin hnh mt php
th theo quy trnh m t trong 7.2, nhng s dng khong 60 mg thuc th kim tra (4.6), cn chnh
xc n 0,1 mg, thay cho mu th.
Tnh khi lng l thuyt ca cacbon ioxit (xem A.2), d kin c gii phng t phn mu kim tra,
v so snh vi gi tr o c. Php th l tha ng nu gi tr o c nm trong khong 10 % gi
tr l thuyt; nu khng th kim tra thit b cn thn bt kn mi s r r v/hoc nhi li thuc th.
Th li cho n khi t c kt qu tha ng.
Tin hnh cc php th kim tra sau khi lp t thit b ban u, sau khi c bt k thay i no ca
thit b hoc ca thuc th v trc khi tin hnh mt php th hoc mt lot php th.
7.2. Php xc nh
7.2.1. Chun b
Cn 5 gam mu chnh xc n 0,01 g, cho vo bnh phn ng ri thm 5 git cht thm t (4.5) v
100 ml nc. ng kn bng nt cao su v lc mnh lm t mu. Tho nt v ra sch mu bm
nt tr li bnh. Lp rp thit b nh ch dn Hnh 1, ng kn l thng kh
CH THCH i vi loi nhin liu c hm lng cacbon cacbonat ln hn 0,5 % th khi lng mu
c th gim theo t l, n ti thiu l 0,5 g.
7.2.2. Chun b iu kin th
Thi khng kh qua thit b vi tc 50 ml/pht trong khong 10 pht. Ngng lu thng khng kh ri
nt kn cc u ca ng hp th cacbon ioxit v u ra ca ng hp th hyro sunfit ni vi n.
Tho ng hp th cacbon ioxit v lau sch ng hp th bng vi sch kh khng x.
CH THCH 1 iu kin m nht nh, vic lau cc b hp th bng vi c th gy ra tch tnh
in, v nu ng k c th nh hng n vic cn. Do cn xem xt vic s dng thit b loi b
tnh in.
ng ngui n bng vi nhit phng v cn li ng sau 10 pht cho ti khi t c khi lng
khng i, tc l cc lng cn k tip chnh lch khng qu 1 mg.
CH THCH 2 Cc ng dng hp th cacbon ioxit, c th l ng Midvale, c php lm ngui
t t trong 60 pht trc khi cn. Khi khng ni vi thit b, cc ng phi bo v khi b nhim bn
mi trng bng cch nt kn vi v lp ng cao su c nt bt chn. Thng cn ng hp th khng
c nt bt sau khi lau.
7.2.3. Phn ng v kt thc
Lp li ng hp th vo thit b ri m kha hoc cc nt kn khc trong chui hp th. Rt 25 ml axit
clohydric (4.1) vo phu c kha, m l thng kh ri cho axit vo bnh phn ng. Nt l thng kh v
ht khng kh qua h thng vi tc khong 50 ml/pht. Nng dn nhit ca cht lng trong bnh
phn ng sao cho cht lng s si sau khong 15 pht. Tip tc un si trong 30 pht na, iu chnh
mc si sao cho khng b tro vo ng sinh hn. Tt ngun nhit, ngng lu thng khng kh, tho
ng hp th lau sch ri cn nh trc (xem 7.2.2).
8. Biu th kt qu
Cc kt qu c th biu th di dng hm lng cacbon cacbonat hoc hm lng cacbon dioxit
tng ng, nh sau:
Hm lng cacbon ca mu phn tch, WC, biu th bng phn trm khi lng tnh theo cng thc
sau:
27,29 m2
WC
m1
Hm lng cacbon dioxit ca mu phn tch, WCO2, biu th bng phn trm khi lng tnh theo cng
thc sau:
100 m2
WCO 2
m1
trong
m1 l khi lng ca phn mu th, tnh bng gam;
m2 l phn tng khi lng ca ng hp th, tnh bng gam.
Bo co kt qu l trung bnh ca php xc nh kp, tnh chnh xc n 0,01 %.
Cc kt qu ca php th m t trong tiu chun ny c bo co trng thi kh khng kh. Tnh
kt qu trn c s khc theo TCVN 318 (ISO 1170).
9. chm
9.1. Gii hn ca lp li
Kt qu ca cc php xc nh kp thc hin ti cc thi im khc nhau trong khong thi gian ngn
trong cng mt phng th nghim, do cng mt ngi thao tc, trn cng mt thit b, trn cc phn
mu th i din ly t cng mt mu phn tch, khng c chnh lch vt qu cc gi tr cho
trong Bng 1 hoc Bng 2.
9.2. S chnh lch ti hn ca ti lp
Gi tr trung bnh ca cc kt qu ca cc php xc nh kp thc hin trong tng phng ca hai
phng th nghim khc nhau trn cc phn mu i din ly t cng mt mu, sau ln chia mu cui
cng khng c chnh lch vt qu cc gi tr cho trong Bng 1 hoc Bng 2.
Bng 1 - chnh xc khi phn tch hm lng cacbon cacbonat
Chnh lch ln nht cho php gia cc kt qu
(c tnh theo cng hm lng m)
Cacbon cacbonat
Cng phng th nghim Cc phng th nghim khc nhau
( lp li) ( ti lp)
n 0,4 % 0,02 % gi tr tuyt i 0,04 % gi tr tuyt i
0,4 % v ln hn 5 % gi tr tng i 10 % gi tr tng i

Bng 2 - chnh xc khi phn tch hm lng cacbon ioxit

 Chnh lch ln nht cho php gia cc kt qu
(c tnh theo cng hm lng m)
Cacbon dioxit
Cng phng th nghim Cc phng th nghim khc nhau
( lp li) ( ti lp)
n 1 % 0,05 % gi tr tuyt i 0,1 % gi tr tuyt i
1 % v ln hn 5 % gi tr tng i 10 % gi tr tng i
10. Bo co th nghim
Bo co th nghim gm cc ni dung sau:
a) vin dn tiu chun ny;
b) nhn dng mu th;
c) kt qu v phng php biu th kt qu;
d) nhng iu kin khng bnh thng c ghi li trong qu trnh xc nh;
e) cc thao tc khng quy nh trong tiu chun ny hoc coi l ty chn;
f) ngy, thng tin hnh php th.

Ph lc A
(tham kho)
Dn sut cc h s s dng tnh ton kt qu
A.1. Khi qut
Trong ph lc ny cc khi lng phn t v khi lng nguyn t c trnh by bng cng thc
ha hc t trong ngoc vung. Khi lng nguyn t nu trong Bng A.1 c s dng trong tnh
ton.
Bng A.1
Nguyn t K hiu Khi lng nguyn t
Hyro H 1,008
Cacbon C 12,011
Oxy O 15,999
Natri Na 22,990
Canxi Ca 40,078
A.2. Php th kim tra
Khi lng l thuyt ca cacbon ioxit, mCO2, gii phng t khi lng ca thuc th kim tra natri
cacbonat, mNa, c tnh theo cng thc:
[CO2 ] 44,009
mCO 2 m Na m Na 0,4152 m Na
[ Na 2 CO3 ] 105,998
Khi lng l thuyt ca cacbon ioxit, mCO2, gii phng t khi lng ca thuc th kim tra canxi
cacbonat, mCa, c tnh theo cng thc:
[CO2 ] 44,009
mCO 2 mCa mCa 0,4397 mCa
[ NaCO3 ] 100,086
A.3. Php xc nh
Hm lng cacbon cacbonat ca mu, WC, tnh bng phn trm khi lng, theo cng thc:
[C ] m 2 100 27,29 m 2
WC
[CO2 ] m1 m1
trong
m1 l khi lng ca phn mu th, tnh bng gam;
m2 l phn tng khi lng ca ng hp th, tnh bng gam.