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    TCVN 8124 2009 5936

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    Léi ndi dau TCVN 8124 : 2009 hoan toan tuong dueng voi ISO 2171 : 2007; TCVN 8124 : 2009 do Ban ky thuat tiéu chudn quéc gia TCVN/TC/F13 Phuong phép phan fich va l4y mau bién soan, Téng cuc Tiéu chudn Do lvéng Chat lveng dé nghi, BO Khoa hoc va Cong nghé cing bd. Ngii céc, dau d6 va phy pham — XAc dinh ham lvong tro bang phuo'ng phap nung Cereals, pulses and by-products — Determination of ash yield by incineration 1 Pham vi 4p dung Tiéu chudn nay quy dinh phwoeng phap xac dinh ham lveng tro cla ngii céc, dau dé va san pham nghién cia ching dure ding dé lam thye pham. Cac nguén nguyén li@u bao gm a) hat ngii céc; b) bét va Idi; ¢) cdc s4n pham nghién (cam va cac sén pham co ham Iuong cam cao, tam); d) bét ngii cde 4a tron (hén hep); e) cac phy phdm tir nga cdc ngoai cac san phém nghién; va f) dau a8 va cac phy phdm ola chung. Tiéu chudn nay khéng ap dung cho cdc s4n pham tinh bét va cdc dan xuat tir tinh bét (xem ISO 3593), cae san phdm ding lam thire dn chan nudi [xem TCVN 4327 (iSO 5984)] hoac hat gidng. 2 Tai ligu vién dan Cac tai ligu vién dan sau rat cdn thiét cho viée 4p dung tiéu chudn nay. Béi vei cdc tai figu vién d&n ghi nam céng bé thi ap dung phién ban duoc néu, Bi voi cac tai liéu vidn d4n khdng ghi nam céng bé thi 4p dung phién ban mdi nhat, bao gdm ca cae sia d6i, bd sung (néu cd) TCVN 4846 (ISO 6540), Ngé — Phuong phép x4c dinh ham lueng am (Ngé bot va ngé fal). ISO 712, Cereals and cereal products — Determination of moisture content — Routine reference method [(Ngtt cbc va san pham nga céc — Xde dinh dé dm (Phuong phép chudn thang dung)]. ISO 24557, Pulses — Determination of moisture content — Air-over method (Bau dé — Xac dinh dé am — Phuong phap dung lo khéng khi néng). 3 Thuat ngif va dinh nghia Trong tiéu chuan nay stv dung thuat ngt va dinh nghia sau day Tro (ash) Phan khéng chay due con lai sau khi nung thee phurong phap qui dinh trong tiéu chudn nay. 4 Nguyén tac Phan mu tht duge nung cho dén khi chat hiru co’ chay hoan toan, sau a6 can phan can cén lai. Phan can thu durgc nay cé dang tro xép sau khi nung 6 550°C va thuy tinh hea sau khi nung 900 °C. Nhin chung, cac san phdm cé chira mudi (vi du, natri clorua, pyrophosphat) cAn dugc nung & nhiét da (550 = 10) °C. Bang 1 néu nhiét 46 nung tong tng voi tirng loai san pham. Bang 1 — Nhiét dé nung va loai san phdm Nhiét d6 nung Loai san phim Bat ihn | (550 4 0) °c (900 + 25) °C ; Léi { ire (550 £10) °C al (90025)°c | | Hat ngis céc (550 si 10) °C (900 + 25) °C | | san pham nghién kha (vi du: da ean pham cé (550 + 10) °G i - nhiéu cam, tam) $An phdm ngii cdc da tron (hdn hep) (550 + 10) °C - Phu phdm cia ngdi cdc ngoai san phdm nghién (550 + 10) °C - Bau dé va phy phdm cla ching (850 + 10) °C “ | 5 Thuéc thir Chi st dung cae thudc thir loai tinh khiét phan tich, nud cdt hodc nude da loai khodng hode nue co 46 tinh khiét tong duong, triy khi cé qui dinh khae, 5.1 Axit elohydric, dung dich Jang gdm mét phan thé tich HCI (35 % thé tich) va mét phan thé tich nue, §.2 Diphospho pentoxit tinh khidt (P,O,9). 5.3 Etanol. 6 Thiét bi, dung cu 6.1 May nghién, dé lam sach va ¢6 khoang lam viéc nhé, dam bao nghién nhanh va dau, 6.2 Bia dé tro hoa, dung tich khéng nhé hon 20 mi, hinh chi nhat hodc hinh tron, day bang va cé dién tich bé mat khéng nhd hon 12 cm”. Cac vat liéu thich hep lam dia tro hod didi day khéng bi hw héng duréi cac diéu kién nhiét dé thir nghiém: a) nung & 900 "C — thi ding dia bang platin hodc rodi: b) nung & 550 °C — thi dling dia bang thach anh hoac sili¢ dioxit Trong ca hai truréng hep, vat ligu st dung phai phu hep voi cas gia tri dé chum. Cac dia tro hoa phai duc lam sach bang cach nhung ngap trong axit clohydric (5.1) it nhdt 1h, sau dé trang bang déng nud chay va bang nude ct. Sau khi rira, cdc dia dwg lam khé trong td sdy (6.7) voi nhiét d6 va khodng théi gian dui d& loai nue. 6.3 Lé nung bang dién, co hé thong théng gid thich hop dugc cung cap bang hé théng kiém soat nhiét 4, cd lop vd chju nhiét dé khdng bi héng & nhiét dé tro hod, va co thé duy tri & nhiét dé (900 + 25) °C hodc (560 + 10) °c. 6.4 Binh hat 4m chan khéng, duoc trang bj dia nhém hode dia str due duc [6 va cd chat lam khd nhu diphospho pentoxit (5.2). 6.5 Can phan tich, co thé can chinh xac dén 0,01 mg 6.6 B6 chia mau cé nhiéu ngan hoac b6 chia mau hinh nén. 6.7 Ti say, dé say cac dia tro hoa. 7 Lay mau Mau gtri dén phang thtr nghiém phai la mu dai dién. Mau khéng bi hu hdng hodc thay adi trong sudt qua trinh van chuyén hodc bao quan. Phuong phaép lay mau khéng qui dinh trong tiéu chudn nay. Nén ldy m4u theo ISO 6644 va TCVN 5451 (ISO 13690}. 8 Chuan bj mau ther B6i voi cdc loai hat hoc cdc san phdm cé chiva hat nguyén, thi tron va chia mau sao cho thu duc mét luong dai dién phi: hop vei may nghién (6.1) duec st dung. Nghién mau thu dures. 816i vei cac san phAm khac thi khéng can nghién. 9 Cach tién hanh 9.4 Xa djinh 46 dm Xac dinh truée 46 4m ctia mau thir theo ISO 712 d4i voi ng cdc trv ngd hoac theo TCVN 4846 (ISO 6540) 464i voi ngd hodc theo ISO 24557 déi voi dau 46. Bau dé va cdc san phdm cua ching duc tién hanh theo ISO 712 voi thi gian sAy la 90 min va duoc bao 6n trvorc néu d6 4m dudi 7 % hoac trén 13 %. 9.2 Chuan bi cac dia tro hoa Dé cdc dia tro hod thich hep khi si dung & 900 °C (6.2), dua cac dia da duoc lam sach truée aén nhiét d@ nung bang cach dat chung trong lé nung (6.3) trong 5 min, lay dia ra dé ngudi trong binh hut 4m chan khéng (6.4), sau dé dung can (6.5) dé can, chinh xAc dén 0,1 mg 64 cae dia tre hoa thich hep khi sl dung & nhiét d6 550 °C, dat cac dia 44 dugc lam sach trong tl say (6.7) trong théi gian can thiét dé lam khé (vi du 90 min & 130 °C), Trude khi st dung, lay ngay dia ra khdi tl s4y va dé nguéi trong binh hut 4m chan khdng (6.4), sau d6 dung can (6.5) 48 can, chinh xac dén 0,1 mg. 9.3. Chuan bi phan mau the Tu mu thi 4 chudn bi theo Bidu 8, trén ky, dling can (6.5) can nhanh phan mau thi khodng tir 3,9 g dén 4,1, chinh xac dén 0,1 mg, khi duoc nung & 900 °C va khoang tir 4,9 g dén 5,1 g khi dug'c nung & 550°C. B4Gi voi céc san phdm c6 ty trong th4p, thi phan mau ther co thé tir (2 + 0,1) g dén (34+ 0,1) 9 Dan san pham trén dia tro hod 4A duoc chudn bj va duos can nhu trong 9.2, dé tao thanh lop ding nhat ma khéng bao géi 9.4 Tro hoa so bé Dat dia tro hod cling vei mau thir vao 1d da nang dén nhiét dé tro hoa. O nhiét 46 900 °C sadn phém sé@ chay thanh ngon ita, O' 550 °C, can thiét phai dét san phdm vei etanol (5.3). Dé tro hod so b6 & 550 °C, cho phép dat cdc dia vao Id nguéi va dé nhiét dé cua ld tang dén nhiét 46 yéu cau, 9.5 Tro hoa Doi cho dén khi san pham chay hét, sau d6 dat dia vao trong Io nung. Dong clra 6 nung. Tiép tuc tro hod cho dén khi toan b6 mau da duc chay hét, ké ca cdc hat cacbon co trong can, cy thé it nhat la 1h& 900 °C va it Nhat 4h 6 550 °C Khi qua trinh tro hoa két thc, ly dia ra khdi l6 nung va lam ngudi trong binh hut Am chan khéng (6.4) é duy tri higu qua cla binh hit 4m chan khéng, khéng xép chdng cac dia Do tinh hit 4m ty nhién cia tro, cén dua dia vé nhiét dé méi treéng cang nhanh cang tét (cy thé Ia 415 min dén 20 min déi vi dia kim loai, téi thiéu 60 min dén 90 min déi vdi dia thach anh hoac dia silic dioxit), c€n nhanh, chinh xac dén 0,1 mg. Béi voi phan mau thir duoc nung & 550 °C, aac biét cha ¥ khi me binh hut 4m chan khong dé tranh tro bi cuén di cling khéng khi. Tinh hiéu lve cla cac két qua thu duec trén mau nay cén du¢c kiém tra vé tiéu chi cla chinh phong ther nghiém (vi du: biéu dé kiém seat). 9.6 $é lan xae djnh Tién hanh it nhat hai phép xac dinh trén cing mot mau ther. 10 Biéu thi két qua Ham lu'eng tro tinh thea chat khé, duoc biéu thi bang phan tram khdi lurgng, Waa, thee céng thtre (1) Was = (17ty ~ 1,) x 100 x 100 mm” 100-w, ) trong dé: m a khdi lvgng cda phan mau thir (9.3), tinh bang gam (g); m, 1a khdi long cla dia tro hoa (9.2), tinh bang gam (g); m la khdi long cla dia tro hoa (9.2) cting véi phan cén lai sau khi nung (9.5), tinh bang gam (g); Wm 18 46 4m cda mau, tinh bang phan tram khdi luong (xem 9.1). Lay két qua la trung binh céng cla hai phép x4c dinh néu thod man cac didu kién vé a6 lp lai (xem 11.1) Biéu thi két qua chinh xac dén 0,01 % khdi long Néu can, ham lugng tro tinh theo phan khéi lveng wet, duoc bidu thi bang phan tram khéi lveng, Wav: theo céng thirc (2): z Way = (Mz — 4) x pe (2) 11 Déchum 41.4 Phép thir lién phong thir nghiém Cac gid tri vé gidi han lap lai, tai lap va sai s4 tei han thu due tly cdc két qua cla cac phép the lién phéng thir nghiém tién hanh theo TCVN 6910-1 (ISO 5725-1), TCVN 6910-2 (ISO 5725-2) va TCVN 6910-6 (ISO 5725-6), Chi tiét dug néu trong Phu luc A. Cac gia tri thu duoc tir phép tht? lién phdng thir nghiém nay c6 thé khéng ap dung cho cdc dai ndng 46 va cac chat nén ngoai cac dai néng d6 va cdc chat nén da néu, 11.2 86 lp tai Chénh léch tuyét d6i gitra cac két qua cla hai phép thtr doc lap, don ié thu dugec khi sir dung cting phurong phap trén vat ligu thr giéng hét nhau trong cling mét phong the nghiém, do mét ngudi thyrc hign, str dung cling thiét bi, thurs hién trong mét khoang thdi gian ngan, khéng qua 5 % cac trvéng hep vugt qua: f= 28x5 3) r=2,8x 0,009 = 0,025 déivdi 0,49 % =< Wag = 1,00 % (4) r=2,8% 0,012 =0,034 déivei 1,00 % < Wea = 2,53 % (5) trong 46 s, 18 46 l&ch chudn lap lai Chénh léch tuyét déi gitra cac két qua cia hai phép thir déc lp, don |é, thu duoc khi stv dung cing phwong phap trén vat liéu thir ging hét nhau trang cdc phong thir nghiém khac nhau, do nhiing nguéi khac nhau thy hién, str dyng cac thiét bj khac nhau, khéng qua 5 % cac truéng hep vet qua R=2.8% sp (6) R= 2,8 x 0,023 = 0,064 déi véi 0.49% < Way 5 1,00% (7) R=2,8x 0,027 = 0,076 déi vai 1,00 % < Wags 2,53 % (8) trong 46 Sp la dé léch chudn tai lap. 11.4 Sai sé téi han Sai 36 toi han la chénh léch gifra hai gia tri trung binh, thu dure tir hai két qua thir vé dé lap lai. 11.4.1. So sanh phép do cia hai nhom trong mot phong thir nghiém. Chénh léch gitra hai gid tri trung binh thu dug tlr hai két qua ther trong cling mét phong thdy nghiém dui cac didu kién vé dé lap lai la sai sé tei han trong phong tht? nghiém, CD,,1.3: CDinua = 2,8 5; = 2ast- 1,98 s, (9) CDjra = 0,018 di voi 0,49 % < Wag < 1,00 % (10) CDipra = 0,024 ddi voi 1,00 % < Wag < 2,53 % (11) trong d6 7, va mp la sé két qua the tueng tkng voi mdi gid tri trung binh: & day n.= nz = 2. 11.4.2 So sanh phép do cua hai nhom trong hai phong ther nghig@m. Chénh léch gilra hai gia tr trung binh thu due tu hai két qua thir trong hai phéng thir nghiém khac nhau dui cdc diéu kién vé 46 lap lai |4 sai 4 téi han lién phong thir nghiém, CDinier (ries a = CDinter = 2.8 \ See = 2,8 's*n 0,58? (12) 1 as CDimor = 0,062 Adi voi 0.49 % < Wea < 1,00 % (13) CDinte, = 0,071 ddi voi 1,00 % < Wag < 2,53 % (14) %em bang dua ra trong Phu luc B 11.6 6 khéng dam bao do 56 khéng dam bao do la mét thang sé dac trung vé 46 phan tan clia cac gid tri cé thé quy vé két qua Dé khéng dam bao do nay duoc thiét lap qua sy phan bé thong ké cdc két qua dug ra tir phép thir lién phdng thir nghiém va dac trung béi 46 Iech chudn thc nghiém. Trong tiéu chuan nay, 46 khéng dam bdo do, u, bang d6 léch chudn téi lap céng hodc trv hai ln, vidu: u=+2 Sa. 12 Bao cao thir nghiém Bao cao ther nghiém pha ghi ra: a) mi théng tin cn thiét dé nhan biét day dui vé mau ther: b) phuong phap |Ay mau 44 sir dung, néu bidt; ¢) phuong phap th nghiém 44 dung, vién d4n tiéu chudn nay: d) moi chi tiét thao tac khéng dugc quy dinh trang tiéu chuan nay hoc nhirng diéu dvr coi lA tuy y cling nhu' cac sy’ 06 bat ky ma cé thé nh hung dén két qua the; e) ket qua thi nghiém thu dugc, hoc néu théa man yéu cau v4 dé lap lai thi néu két qua cudi cling thu duge. f)_ tinh kf thuat ma dua theo dé dé tinh két qua (uot va/hoac khé) Phu luc A (Tham khao) Két qua phép the lién phong thir nghiém Két qua cla mét sé phép thir lién phéng thir nghiém thyc hién & Hungari (H), Vuong quéc Anh (GB) va ICC 48 két hop dé thu due at liu duoc liét ké trong Bang A.1 Bang A.1 — Két qua théng ké cia phép thir lién phong thir nghiém Nguén — San pham sé | ciaty | pelech | Gioi | Beigch | DOléch | Gidihan | BO lech phéng | trung | chudn | han lap chuan chuan | tailap R chuan | thir binh lap lai lai tuong déi tai lap tueng déi | nghiam lap lai | R=2,8s9 tai lap w & r=2 85 Se | CVnest i CViRiesn'w | % Khdi | | | lveng | er | See Ehailt Botmyp | GB a | 0,490 | 0007 | 0,020 1,48 0.013 | 0.038 265 Botmy2 | H 29 «| 0.494 | 0,008 | 0,022 1.62 0.026 | 0.073 5,26 Bét my | thuong 2 icc 7 0,516 00,0017 0,0049 0,33 | 0.0118 0.0330 2.29 BotmyB | GB 12 «©| 0536 | 001 | 0,028 1.87 0.027 | 0,076 5,04 BetmyA | GB 12 | 0868 | 0005 | oo14 0.88 0,032 | 0,090 5,63 BotmyC | GB 11 | 0606 | 0.014 | o039 231 | 003 | 0,084 4,95 BotmyF | GB 12 | 0609 | 0,014 | 0,039 2,30 ao21 | 0,059 245 | Batmye | GB 12 | 0641 | 0,011 | 0,031 1.72 0.022 | 0,082 3,43 Botmy \ mong | © | 13 | 0.728 | o.o104 | oazez | 143 | Q.or42 | 0.0307 1,86 aes aoe ie) Bot my 1 H a0 | 0771 | 0,006 | 0,017 | 0,78 0.022 | 0,062 2,85 . Al - i | 7 E | meets icc | 12 «| o9a6 | ooo71 | oo1ss | 0,75 0.0185 | 0.0517 1.96 ee icc 14 | 4,187 | 0.0134 | 0.0376 | 113 | 0.0283 | 0,0790 2,38 Luamy2 | H a1 | 4615 | 0011 | 0.031 0,68 0,033 | 0,092 204 | Loamy1 | H 2a =| 4714) 0,01 | 0,028 0,58 0.034 | 0,095 1,98 cam icc | 12 | 2530] 0,015 | 00420) 0,59 0,021 | 09,0590 0.83 i L - xe = 1 Méi quan hé gira 46 léch chudn Kip lai va d6 léch chudn tai lap dug vé theo ham Iwang tro trung binh tinh theo phan tram khdi lung chat khé theo Hinh A.1 va Hinh A.2 tuong wing. Phvong trinh duéng tuyén tinh di vei 46 lap tai: s,= 0,008 W,,, + 0,0068 (H@ s6 higu chinh: c? = 0.2189) CHU DAN 8, a6 léch chudn lap lai; Wy ham lvong tro trung binh tinh theo phan tram khdi lueng chat khé. Hinh A.1 — Méi quan hé gitra 46 léch chudn lap lai va ham Iverng tro trung binh tinh theo phan tram khéi lwgng chat khd 0,035 0,03 0,025 0,02 0,015 0,01 ad Phuong trinh duéng tuyén tinh adi vai dé tai lap Sa = 0,0035W, , + 0.0204 (Hé sé hiéu chinh: c? = 0,0812). CHU DAN Sa 6 léch chudin tai lap; W, ham lveng tro trung binh tinh theo phan tram khdi long chat khd Hinh A.2 — Méi quan hé gitra 46 !@ch chudn tai lap va ham lweng tro trung binh tinh theo phan tram khéi lugng chat khd Phy luc B (Tham kha) Thy té 4p dung cac giéi han lap lai va tai lap Sai sb tei han cia phép thir lién phong thir nghiém CDe 0,062 Bang B.1 et 4 = ™ Pham vi Dai danh gia | Do ch | Gigihan | Saisétéi | DOlgch | Gidihan ap dung | chudn | lip lai hantrong | chudin tai lap 9% khdi lureng | ip ta | phong ther | tai ip | 1 | 1228s, nghigm R=2.8 5, | & | | Sr : | | ©, | | | | | | | | fas 0.49 < Was < 1,00 o.00e | 0.026 0.018 0,023 0.064 { Be 4,00

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