| TCVN Tlé€u CHUAN quoc GIA TCVN 8516-2:2010 ISO 4829-2:1988 { Xudt ban Lin 1 THEP VA GANG - XAC DINH HAM LU'QNG SILIC TONG - PHUONG PHAP QUANG PHO PHUC B| KHU" MOLIPDOSILICAT - PHAN 2: HAM LUNG SILIC TRONG PHAM VI 0,01 % VA 0,05% ‘Stee! and iron — Determination of total silicon content - 3 Reduced molybdosilicate spectrophotometric method- Part 2: Silicon content between 0,01 % and 0,05 % HANOI-2010TeVvN 8516-2:2010 Loi nei au ‘TOVN 8516-2:2010 hoan toan trong v6r ISO 4829 2:1988, ‘TCVN 8516-2:2010 do Ban kj thudt eu chun quse gla TCVNITC 17 Thép bien soan, Téng cue Tieu chun Bo lvong Chit hrong dB nghi, 86 Khoa hoc v8 Cong nghé céngbé.TIEU CHUAN QUOC GIA TCVN 8516-2:2010 Thép va gang- Xac dinh ham lwong silic tng - Phuong php quang phé phirc bj khtr molipdosilicat - Phan 2: Ham wong silic trong pham vi 0,01 % va 0,05 % ‘Steel and ion - Determination of total silicon content - ‘Reduced molybdosilcate spectrophotometric method - Part 2: Silcon content between 0,01 96 and 0,05 %. 1 Pham vi ap dung ‘Tieu chun nay quy dinh phuong phap quang phb str dung phize molidosiicat bi Kn dB xde dinh ham twgng si ting rong thép va gang. Phuong phép nay ap dung cho ham lugng site trong pham vi 0,01 % (ki Keng) va 0,05 % (kt gg) trong thép va gan, 2 Talligu vign dn (Cée ti figu duo aay a rt cn tiét di voi vigc &p dung tibu chun nay. i v6 tA Hu © gh nim 8ng b6, dp dung phién bin duge nd, BSI vei tl bu kang o& nm cOng bb, &p dung phin én | mdi mht cd cc sta dBi, néu ob. TOWN 1811 (ISO 14284), Thép va gang — Ldy méu va chutin bj miu a8 xée din thanh phan nos | Ie. ‘TOWN 6910 (1S0 5725), D6 chinh xe (66 ding va ap chum) cio phuong phép do va két qué do. ‘TCVN 7149 (ISO 386), Dung eu th nghiém bang thy tinh - Burt ‘TOVN 7151 (ISO 648), Dyng cu thi nh bang thi th - Pipet mot mic TOWN 7183 (ISO 1042), Dung eu thi aghigm bing thy tinh - Binh anh mae.TCVN 8516-22010 3 Nguyan tae Hoa tan mB trong hi hop ait clohyeictant iti "Nang chy in king tan rong ant béng at peo “Tao ra molpdosiicat dang oxy ho (mu vang) rong dung dich ax yéu. ‘Sau kh lam tang nag 49 ax sunfuric v8 thé vo ait oxalic ab logi BO sy fn te ca photpho, ‘sen va vanadtién hn kh chon lc phic mofpdosiicat dn phie mau xanh bang axt ascorbic. ‘Bo quang phd ela phiteb kh: mau xanh & bu6e séng 810 rm. 4 Thube thir “rong qua tinh phan tic, néu khong 68 yéu clu ndo kn tl chi sir dung thus thir dupe: cong ‘gn c6 tinh kit phn ih, (Cae thuse thi age dng trong chal thuy tinh, kh ma co thé hp thy ot va tr nn tin an ‘mn thy tinh, Thuée thi kiém tah, ching hen nhu nati cacbonat va nat pooxt dc bet rt ray ‘cm, 08 lol tanh ei rob 6 nim gla tng tr ngubn nay, tt nt & chi sir yng cc chal hub ‘tnt mo ma pha ch dng dic. Ngodi a, ch alr dung ruse vita mei ft 48 pha ché cée dung dich thude thi va trong c@ qué trnh khong 87 dung aver duge Kh khong ig a0 Gi ion vl c6 th cén chika mot xg Hom Keo si. ‘D8 lop tar nhang 6 nhidm ngfu nhién, yéu cu nue pha due chun bj cho muc dich réng va ‘urge dung trong binh nha poipropylen 38 ding naa. Tak c& cde dung dich phai moi pha ché vA uge bio quan trong chal nhya Poliprpylen hode poftetratlootyten. 41 St tinh knit, ham krgng sie nhd hon 2 pla 4.2 Natr peoxit,kich thud hat $00 jm 43 Ait sunfurie, dung deh pha loang 1 +3, ‘Vira rot vir khully mat ech than trong 260 ml anit sunfuric p = 4,84giml vio 600 mi rib. Lam gud, pha lng bing muse dn 1.000 mi va lc Ky. 44 Alt sunfure, dung dich pha losing 1+ 19 Vira rt vira khuy mat ech thn trong 50 ml ait sunfuric p= 1,84g/ml vo 800 ml ube. Lam nau, ‘ha lading bang nue dn 1000 ma va eK.TeVN 8516-2:2010 4 Hon hop axit clohydric/axit nitric Rot 180 mi anit clohydric (p= 1,19 all) va 65 mi ant nic (p = 14 gl) vo 500 mi nue, lam ‘AGU, pha lang bing nude dén 1 000 mi va Mek, 4.6 Ait ascorbic, dung dich 20 gf Pha ché dung dich nay ngay tude Kh ding, 4.7 Axit oxalic, dung dich Hoa tan 6 g ait axa ng hal phan ty nude (C:H,0,.2H,0) trong nue, pha leang bing nude dén 100 mi va ey. 4.8 Hydropooxit Pha lng bang nut 200 ml hyeropaoxt 300 gf 1000 mv ek 4.9 Kall pomanganat, ung deh 225 gf {ge tr dg, 4.10 Nati moipdat, ung dich Hoa tan 2.5 nati molipdat (Na-MoO,.2H,0) trong 50 ml nuge va lac qua gidy loc dinh bong chy ‘rung bint. Ngay dc Khi dng, thé 15 ml at sunfric (4.5) pha long an 100 va Ke ky 4.11 Sil, dung dich tu chun 4.11.4 Dung djeh silie gbe,chire 19 Siren Dung cn 68 6 chinh xd 0,000 g, cin 2.1388 9 sic ont ob 45 tinh Khiét cao vira méi due nung (99,9% SiO.) va chuyn vao mot chén platin. (Trube kl ding phi nung sie oxt ob a6 tinh Kit 20 trong 1 h 8 110°C va lam nguol trong binh at dm). Trén dBu voi 16 g nati cacbonet khan va rung chay & 1050 °C trong 30 min.’Hod tach san phdm nung bang 100 mi nude trig obe polipropylen hog potetrafoetylen (xem cha thich). Chuyén dung ach hoa tach, khéng con vt can ‘do, sang binh dinh mite 1000 mi, pha long bang nue én vech va kc kj. Chuyn ngay sang binh Poltetrafloetyen duge nit kin a8 bao quan, ‘ml dung ajen gc nay chira 1 mg S. ‘CHU THICH: Hos tich sn phim nung en phi dn néng ti, 4.11.2 Dung djeh tiéu chuan sillc,chira 20 mg Si rn it ‘cho 10 mi dung de sic géc (4.11.1) vao binh ginh mite 500 ml, pha long bing nuse én vach va log. Chuyén ngay sang binh poltetraioetylen due nit kin dB ding ngay. 1 mi dung dich teu chudn nay chira 20 yg SiToVN 8516-22010 5 THIEL, dung cv fpyng 2 ng ng te phon nahi v8 154 cbe v8 ndp, bing polioropyen node potetasotye 15.2 chén, bing zcon ki ol (xem gi ch}, cng ti 50m qu THCH Chin icon th cb cng hay td cho chen con ken 15.3 00n9 cv thu tinh do thé tic “rir. dung cy thy tah o th ch pla loi A ph hap voi TOWN 7149 (SO 386), TOWN 7181, {1s0 648) hod TOVN 7158 080 1042) vyige st ung dung cy thuy nh pha han ch th gian ip xc tube to ngdn ahd, nu ing up tin boslicat thi ho gian tp xe 38 cho phép lau hon. ‘samy quang phd May quang phb ph uve trang bi 8 do 0 hp thy quang vo chibur6ng ng ph 10 nm hoBenh Jhon & bude séng 810 nm. Bude S6ng do pha cod chin xc + 2:nm nh ki do hp ty quang on lt cia kinh fe ddim 8 803 nm HoBc phuona php chudn phi hop Khe. Do hp thy quang ci ng dich voi hp thu quang lon nhStphai cé & lp et bibu thi bang sal lich tong dBi la + 0.3% sh hon. Lay mau hann dy mu phi hop vi TCVN 1811 (ISO 14284), ich tién anh 1 rong mu thir 1 06 di chinh xc 0,001 g, e&n 0,80 g + 0,01 g (m) mu phan tch & dang pho bao min, pho st yng si luong voit 8 od tube th, nhung ding 0.609 0019 st tin Kit (4.1), thay thd phan en, in tat qu nghigm tring doe KhBng ché tute sau nh mot & dt tp vc ti ham hét spin teh og tht hai ngiém tng cho ting 16 mBu phan ch va by 0 nn im ca tinh todn. Kt qua cz va phn tan cha th ng rng ph dro co King 8p nh va phdi 6 bién hap phat hién ra ngubn gay 6 nhiém bang cich kiém tra chdt lx@ngTeVN 8516-2:2010 ude va ela tig thube th sing r8trudec Kh thye hin tip theo, Oge big, nati peoxt va kal pemanganatcén cha ra chon do mot s6 lai thude thi nay cha Kt qua thi nghigm tng cao. Tét nt la 40 hp thy quang ca thi nghibm tng do vbi cet day 4 om Khéng wot qué 0,050, tues ‘avong v6 0,008 % (kh leg) stl 7.3 Céch xée ain 1 Phan hus méu phan tich CChuyén kh6i iugng mu phan tich (7.1) vao trong eb nha polieropylen hoe polteratoroetyien 250 mi (xem 6.1). Cho vio 85 mi hén hop cia axtclohyric va axtnivic (4.5), dy np (xem 6.1) vi {dun néng tt dn ki hoa tan miu, kg kam mt nib te ti, ‘khihén hop axt ngimg téc dung, loc dung dich qua gy lec din Kzong chy cham ob ham lzong tro {hp va thu nude lc vio ob $00 mi Riza ce bang 20 ml nude néng, ding dia thu inh du boo 20 6u tc bé nhing hat dinh bm va Ige nhimng phan nude rra nay qua cing gidy loc tr, Riza sy foe nhibu lin v6i 20 mi nebe néng. Git gidy lec 48 sir dung cho qua tinh thye hign néu trong 132. 7.3.2 Xtrly em khong tan ‘Chuyén gidy lo va en khong tan vao chén zicon kim lol (5.2) va nung & nhigt tp an ki fal 8 cacbon, sau 40 nung trong fo dign & 600 °C, Lam ngugl va tn cén ve 0,25 g na peo (4.2). Phi thém len trbn 0,25 g nat peoxt vi nung trong I 10 min & nhiét do 600 °C. Lam ngus, cho vao 415 ml nue, By nép chén va 68 cho phan Ung gidm bet. Cho vo 15 ml anit sunfric(4.4), Khudy ‘ho tan hét tia va g0p vo dung dich le thu drge trong phén 7.3.1. Rita chén vA nép bing nude va ‘960 vo dung dich Ipc 7.33 Chuan bj miu phan tien Pha long cing dich & 7.3.2 dén khodng 300 mi va tim ngugi. Cho v8o § ml dung dich kali PPemanganat (4.9), sau d6 tig gig mot én Khic6 duge mau héng tuoi bEn vong it nhét trong 4 min. (Thém hegng dung dch kali pomanganat (4.9) ve dung dich thi nghigm trng (xem 7.2) 48 cho +a mau héng trong dung dich thd). Bun dén si vad s6i nhe trong 2 min. Néu ob két ta mangan oxi, cho tim get dung dich hydropeonit (4.8) én kh Kt tba vr tan ht v8 dun 361 ne trong 5 'min. (XV ung alc ti nghigm tng cong giéng dung dich mBu phan tic, ngay cd Ki Khéng xy ra Et tia mangan dioxt). Lam nguti, chuyén vao binh ginh mite 1000 mi, pha long bang nurée dén vach va le kf. Chuyén ngay vlo mot binh potpropylen hose poktetraforoetyen. 7.3.4.Lén mau ‘Ding pipet hat ha thé ten 20 mi dung dich mu phan tch (xm 7.3.3) va hal th ich 20 nl dung dich {hi nghiém tring (7.2) vao trong cc binh dink mic thuy tinh bosiicat 50 ml iéng 8. Trong_ tema hop trén, mot binh ding cho mau phan tich va binh ka dng cho dung dich so sénhTOVN 8516-2:2010 ‘Dung dich mu phan th chia nib Node tantan sé cho két tia min ch ra Kh pha long. BE cho kat tia ling va ngay lp tc lc phan dung dich pia ten qua gi loc inh ung chay chim vo met binh kno tute kh hat dung gh fen mau. 86 mtv mit du ten “Tién Hanh xi tng dung dich phn ich va dung dich so sanh nhur ue nu dui dy Khi nit ‘rong knodng 15 °C dn cao nhdt 25 °C, si¥ dung pipet cho vie thém vao tt cd cc loa dung dich thube tha. 12) Dung leh phn cn ‘Cho vao dung ch phn tic hao th ty sau day, Kc du sau méi in cho: + 100 ml dung dich nat malipdat (8.10) v8.8 yn rong 20 min; = 80m cng eh at suri (4.3); = 80 mi dung ich a oxalic (4.7) = Noay ip to, 5,0 ml dun deh ait ascorbic (48), 1) Dung din so san ‘cho vae dung dch 20 sinh theo thi ty sau ay, the Abu sau ml ch = 80 i dng ich at suri (4.3; = 50m dung dich ax oxalic (4.7 10,0 eng ena olipdt (4.10) -Ngay lp te, 50 ml dung dich nt ascorbic (48) Pha long bing nude én vach va le kj. BB yen timg dung den thay (mau phén lich va thi nghigm ‘rng cing nur dung dich 60 sinh trong 30 min. 736 Bo quang phd “Tin hanh do quang ph ting dung ¢ich thu duge rong (7.3.4) & bude séng 810 nm (xem cha thich), trong cuvet 6 chibu dy 4 em, sr dung rue kim mol trong chun, Hu etinh a9 hdp thy quang cho tim dung dich th (mu phan tch va thi nghigm rng) bing cfc ‘nr ido dp thy quang oa dung dich so sah trong Ung CHO THICH: Ce bute s6ng Ke vi 810 mm (wong Khang HF 760 dén 860 nm) ob tb sir dyna, nu thu tn, c6 thd tao lap nhng 68 hép thy uang cho lat miu chun ten may quang ph sir dyna. HB 36 a6 No ‘thy quang ki ugg ig tl 810.8 dre dol 780 (‘em 714 Xay dg durdmg chun 17.44 Chuan bl dung dich teu chudn Cchuybn 0.50 g £0.01 g sét tinh Knit (8.1) vao ce oBe nha polipropylen va pottatoroetyen 250 ‘a ing (nem 5.1) v8 hoa tan theo nu trong 73.1 va 7.32 10TOWN 8516-2:2010 (Cho vao nang thé lich do ehiah xc dung dich teu chuain sie (4.11.2) 08 e9 day tou ehulin cho ‘ung pham vi ham kong sil nb rin bay trong bang 1. ‘Tidp tye x Wy day mu chudn nh 8 mig t& trong 7.3.3 nhung ba qua thi nghigm tng, sau 46 hye ign nu trong 7.34 nhung bé qua dung dich so sn, (CHO THICH : Dung le hi nghiém ing dung dc 90s 8 Khng cn tit cho pin eh mu cb vi ‘hal euge cnn sva ting qua mu chun “kong” ca dy Bingt Tlenangdehalcteu | Kliuergstctonging | Nineabstcbergedich outa ast) e eta ns si set 00 ° 0,000 25 50 0.020 50 100 0.040 18 150 0.060 100 200 0.080 125 250 0.100 7.42 Do quang phd Tién hanh do quang ph8 cia ting dung dich (74.1) tal bute séng 810 nm (xem cha thich 7.3.5) trong cuvet 6 chidu day quang hoc 4 cm ding nude lam mol tng higu chinh. Ly a9 hp thu quang cia tig dung dich méu chudn ta 66 dp thy quang méu chub "kg? 7.43 V6 ad thi chun va tinh hg $8 gée a DDyng ab th chun bing cach v8 46 np thy quang thyc so vei néng 49 sic tyeng ung tinh ra !mcrémiigam tn militia dung dich duoc do, 8 Tinh odin két qua 81 Phuong phi tinh tin CChuyén abd hnép thy quang d8 chinh sira cia tung dung dich tiy (mu phan tch va thi nghigm trang) (73.5) ra néng 40 sc tweng Ging tinh ra micrémiigam trén milit bang céch sir dung ab ti hud durge v8 trong 7.4.3, Tinh ham luong sic (S), bidu th bang phn trim theo khéi yang, bing bg thie sau‘TOVN 8516-2:2010 (0 -podx Tee un ta nbng 49 sil tong dung ch hi nghigm ting (88 chin sr ai voi dang dh so sen tinh bing microgram te mit; tad a ste rong dung ch mu phn tc (8 cin sta a wt dung ch 0 sh) tinh bing microgram tran iit Vp tata tich cba dung dlc pn tch (7.3.3), tinh ng iit ‘Vy ath tch oath tch dung eich phn ich hat ra (7.3.4) tinh bang ‘Vi lath teh eta dung ach pan tich da én mau (7.3.4) tin bg mii, sm 18 kn hagng mu phan teh (7.1, inh bang gem. 8.2.09 chym 2 ‘ge kid ra chy ea husong php nay 68 dura thys hin bal 15 pong ti nghim tus Mon dng 5 mic slic, mBl mt phdng th nghibm phn leh xc dnh ba Kt qua cho tang mac se equa dye xij bing purong pha tng Ké phi hep vol TCVN 6810 (180 5725) (xem Chi ch 4.2va3). cae dieu nhéndage cho thy knéng osu twong quan Ni thng no gle ham zona eile va 6B tap iro i Fv Kt bi 1 0,004 % ero) Sich dP er 9.088 2 en gna) Scho do tk RnB pg th gin v2 0.008% (8 xo) Sich 4 BP R ‘cic mu phan ich sir dung va kB qua phn eh ca ee mBu d® Ae tm it trong phy Me coHO THICH 1. a wong ba Bt gu xe ih rg Hy Hb Wong nha cu Win cS py ah GB oh one “Fevwo9t0 (50 6725 nah 8 mt hn vn th nh vr cong tnt Bu ib vin ha deg Bt Aha ‘cing dung chubn vi met Khong tN lan gn 2 Kb qui xe ahr ba Bug te ig a mc nc (2 mot ng He) ing do chin ann vin thigh a rong ch hich 1 wen, i ding cing tit | ang vt dng chun moh 2 | | | | | 7 |TOVN 8516-2:2010 3. Ter nang kit qua cba ngdy 1, th aro dol (vt tp (R) Su dyng phy enpquy Br rong ‘TOUN 6910 (ISO 5725). TW Bt qua du ten rong gay 4 va KB qu trong ny 2 tinh dge ti trong 2948 phng th him (Re. 9 Bao céo thir ‘Bio co thd phai ao gdm eae ehi bt sau {Tat cd mal théng tin cdn tht a8 phan biet dure méu, phOng thi nghiém va ng thang phan ih; ) Phuong php duge sir dung ign din teu chun nay, ©) Két qua v8 hinh the ching auge bibu thi 1) Nhong nét dc big kha thubng due ghi trong qua tin xc inh; 2) Moi céch thao tc khang argc quy dnh trong it chun nay hoe mei céch thao tac tu ¥ 06 nh hhutng din két qu phn ich, 3TOWN 8516-2:2010 Phy luc A. (Tham kno) ‘Thong tin b8 sung vb cae thir nghigm c6 sy hop téc qué 6 sing A118 Kd qua tr nhog I nghim phn cn qubs 6 dn han org nm 1985 én nm mau thép & bay quée gia do 1 phng thi nghiém thyc hi. Kt qua ai ching duoc tinh ay tong béo céo N 655 do ISO/TC7ISC 1 4n hanh thang 3 nfm 1986, Bang AA Mau wimirgna | a | F ‘0008 | 0020 | 0.028 | 00st "ERM 085-1 thep dB ct 0.8% 5) CRM 2854 (hép Co, HMO, coors | 0022 | o00sr | oor seuN. 0767) §88 023-8 (ihépkhéng hap Km) onze | 004s | 0.9053 | 0082 Bes 432/1 Chip knéng bop kin) ots | o0e0 | 00070 | 0.0088 es ase (hip 13% Ma) {0085 | oss | oonse | cose “4