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    Khoa Hoa Giao trnh thc hanh Phan tch cong nghiep 2

    2

    MUC LUC

    Noi dung Trang

    Muc luc ................................................................................................................................... 1Li m au .............................................................................................................................. 3Noi quy phong thc tap Hoa phan tch cong nghiep ................................................................ 4Mon hoc: Thc hanh Hoa phan tch cong nghiep 2 ................................................................. 5

    CHNG 1: PHAN TCH CAO SU .............................................................................................7

    Bai 1: Xac nh ham lng chat bay hi ................................................................................. 7Bai 2: Xac nh ham lng Nit .............................................................................................. 9Bai 3: Xac nh ham lng tro trong cao su thien nhien ....................................................... 11Bai 4: Xac nh tong ham lng chat ran trong cao su latex ................................................. 12Bai 5: Xac nh ham lng ong bang phng phap quang pho trong cao su latex .............. 13Bai 6: Xac nh ham lng Mangan phng phap hap thu quang pho cua Natri periodat trongcao su latex ........................................................................................................................... 16

    CHNG 2: PHAN TCH CHAT TAY RA............................................................................ 20Bai 1: Xac nh Na2O va SiO2 trong Natrisilicat nguyen lieu san xuat chat tay ra.............. 20Bai 2: Xac nh Las nguyen lieu san xuat chat tay ra ......................................................... 22Bai 3: Xac nh NaOH nguyen lieu san xuat chat tay ra ..................................................... 23

    Bai 4: Xac nh Na5P3O10 va Na2SO4 nguyen lieu san xuat chat tay ra............................... 24Bai 5: Xac nh ham lng Photphat trong bot giat............................................................... 26Bai 6: Xxac nh pH chat bay hi chat khong tan trong bot giat ..................................... 27Bai 7: Phan tch ham lng Glycerin va Cacbonat trong kem anh rang .............................. 29Bai 8: Xac nh ham lng Natri cacbonat............................................................................ 31Bai 9: Xac nh ham lng chat hoat ong be mat................................................................ 32

    CHNG 3: PHAN TCH GIAY................................................................................................35Bai 1: Xac nh pH nc chiet cua giay va bot giay ............................................................. 35Bai 2: Xac nh tinh bot trong giay ...................................................................................... 37Bai 3: Xac nh o tro trong giay va bot giay........................................................................ 41

    CHNG 4: PHAN TCH DAU KH .........................................................................................43

    Bai 1: o an mon tam ong ASTM D130 (copper strip corrosion) ...................................... 43Bai 2: Xac nh iem nho giot cua m nhn ASTM D566 (dropping point of grease)......... 47Bai 3: Xac nh nhiet o chp chay coc kn ASTM D56 (flash point closed cup) .............. 50Bai 4: Xac nh nhiet o chp chay coc h ASTM D92 (flash point open cup) .................... 53Bai 5: Xac nh o xuyen kim cua m ASTM D217 ............................................................ 56Bai 6: Xac nh ch so mau Saybolt (Saybolt corlor) ............................................................. 60

    CHNG 5: VAT LIEU DET NHUOM PHNG PHAP XAC NH O BEN MAU........63Bai 1: Xac nh o ben mau vi giat kho .............................................................................. 63Bai 2: Xac nh o ben mau vi ma sat................................................................................. 65Bai 3: Xac nh o ben mau vi moi hoi ............................................................................... 67Bai 4: Xac nh o ben mau vi nc ................................................................................... 70

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    Khoa Hoa Giao trnh thc hanh Phan tch cong nghiep 2

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    LI M AU

    e co tai lieu hoc tap cho sinh vien chuyen nganh Hoa phan tch va thong nhatchng trnh giang day cua bo mon hoa Phan tch cua trng Cao ang cong nghiep IV,chung toi a bien soan cuon giao trnh Thc hanh Phan tch cong nghiep II.

    Cuon giao trnh nay c bien soan theo cac tieu ch sau:

    1. Noi dung thc tap gom co 5 phan thuoc ve cac lanh vc cong nghiep nh:a. Cao sub. Chat tay ra

    c. Dau khd. Giaye. Det nhuom

    2. Nham trang b cho cac em sinh vien co c tay nghe va kien thc chuyen mon venghe phan tch, khi s dung cuon giao trnh nay sinh vien, hoc sinh se viec lamtrc tiep tren mau thc vi cac phng phap phan tch mi nhat hien nay ma thcte ang s dung cac doanh nghiep .

    3. Giao trnh c bien soan da tren cac tieu chuan ASTM, TCVN va tai lieu cuamot socong ty hien nay ang thc hien.

    Nhom bien soan gom co: Chng cao su, chat tay ra, giay, det nhuom: Nguyen Van Trong: Chng dau kh: Nguyen Hoang Minh, Nguyen Hu Sn, Tran Th Hong

    Cuon giao trnh nay mi bien soan lan au nen khong the tranh khoi nhng sai sot.Chung toi mong nhan c y kien ong gop e cuon giao trnh nay ngay cang hoanthien hn.

    Xin chan thanh cam nNhom tac gia bien soan

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    NOI QUY PHONG THC TAPHOA PHAN TCH CONG NGHIEP

    1. i hoc ung gi, sinh vien i tre qua 15 phut khong c vao phong thc tap.2. Sau khi kiem tra au buoi thc tap, neu sinh vien khong thuoc bai th giao vien

    yeu cau sinh vien ra khoi phong thc tap.

    3. Sinh vien chu trach nhiem ve cac dung cu thuy tinh nhan c khi vao phong thnghiem, neu co nt, be phai bao ngay vi giao vien hng dan.

    4. Khi thc tap, phai gi im lang, khong c hut thuoc trong phong th nghiem.

    5. Cac ong nho giot phai e lai ung chai cu, khong c bo qua chai khac lam hthuoc th hoac bo ba bai tren ban th nghiem.6. Nhng chai thuoc th phai e lai cho cu, khong c mang i ni khac.7. Khi dung may ly tam, phai luon luon dung hai ong nghiem co the tch tng ng

    e can bang.

    8. Khong c t tien lay hoa chat ve nha.9. Suy ngh ky ve quy trnh phan tch, tm hieu y ngha cua moi thao tac trc khi

    lam, khong c lam cau tha, vo y thc, nen co so tay ghi chep th nghiem.

    10. Khi ra ve, phai ra sach se cac dung cu, don dep ngan nap, giao tra u dung cucho giao vien hng dan.

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    MON HOC: THC HANH PHAN TCH HOACONG NGHIEP II

    1. Ma hoc phan: 036HO2312. So n v hoc trnh: 33. Trnh o thuoc khoi kien thc: Khoi ky thuat chuyen nganh4. Phan bo thi gian: Thc hanh 100%5. ieu kien tien quyet: a hoc xong l thuyet va thc hanh phan tch c s6. Mo ta van tat noi dung mon hoc: Hoc phan nay trang b cho sinh vien kien thc

    ve phng phap x ly mau hu c va quy trnh kiem tra mot vai ch tieu chu yeu

    trong mot so mau: cao su, my pham, chat tay ra7. Nhiem vu cua sinh vien: Tham d hoc va thao luan ay u. Thi va kiem tra gia

    hoc ky theo qui che 04/1999/Q-BGD&T8. Tai lieu hoc tap: giao trnh thc hanh phan tch cong nghiep, cac tai lieu tham

    khao9. Tai lieu tham khao:

    [1]. Nguyen Th To Nga Cac qua trnh chiet NXB ai hoc quoc gia Ho ChMinh.

    [2]. Vu Tam Hue va Nguyen Phng Tung Hng dan s dung nhien lieu daumo - NXB Khoa hoc va ky thuat.

    [3]. Cac TCVN oi vi my pham, dau kh va cao su[4]. Cac tieu chuan cua ASTM oi vi dau kh, chat tay ra

    10. Tieu chuan anh gia sinh vien:- Nam c c ban noi dung mon hoc- Co tnh chu ong va thai o nghiem tuc trong hoc tap- Kiem tra gia mon hoc e c d thi- Thi vi hnh thc trac nghiem, viet va bai tap.

    11. Thang iem: 10/1012. Muc tieu cua mon hoc: Giup cho sinh vien hieu va nam vng nguyen tac x ly

    mau va phan tch cac ch tieu hu c chu yeu.

    13. Noi dung chi tiet mon hoc:Chng 1: PHAN TCH CAO SU

    Bai 1: Xac nh ham lng chat bay hiBai 2: Xac nh ham lng NitBai 3: Xac nh ham lng troBai 4: Xac nh tong ham lng chat ranBai 5: Xac nh ham lng ong bang phng phap quang phoBai 6: Xac nh ham lng Magan bang phng phap quang pho

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    Chng 2: PHAN TCH CHAT TAY RA

    Bai 1: Xac nh Na2O va SiO2 trong Na2SiO3Bai 2: Xac nh LAS

    Bai 3: Xac nh NaOHBai 4: Xac nh Na5P3O10 va Na2SO4Bai 5: Xac nh ham lng phot phatBai 6: Xac nh pH chat bay hi chat khong tanBai 7: Xac nh ham lng Glycerin va Cacbonat trong kem anh rangBai 8: Xac nh ham lng Natri cacbonatBai 9: Xac nh ham lng chat hoat ong be mat

    Chng 3: PHAN TCH GIAY

    Bai 1: Xac nh pH nc chiet

    Bai 2: Xac nh ho tinh botChng 4: PHAN TCH DAU KH

    Bai 1: Xac nh o an mon tam ongBai 2: Xac nh iem nho giot cua m nhnBai 3: Xac nh nhiet o bat chay coc knBai 4: Xac nh nhiet o bat chay coc hBai 5: Xac nh o xuyen kim cua mBai 6: Xac nh ch somau saybolt

    Chng 5: PHAN TCH DET NHUOM

    Bai 1: Xac nh o ben mau vi giat khoBai 2: Xac nh o ben mau vi ma sat

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    CHNG 1: PHAN TCH CAO SU

    BAI 1: XAC NH HAM LNG CHAT BAY HI

    I. NGUYEN TAC:

    Say mau th 100 50C en khoi lng khong oi. Chat bay hi la lng mat itrong qua trnh say mau th.

    Chat bay hi la nc va nhng chat bay hi khac 1000C co trong cao su thiennhien hoac xam nhap t ben ngoai vao trong qua trnh bao quan va san xuat.

    Kiem tra ch tieu nay giup ngi san xuat co the kiem soat c qua trnh baoquan mu cao su.

    II. DUNG CU - MHOA CHAT:

    - May can phong th nghiem hai truc- Tu say co khong kh tuan hoan, nhiet o on nh 100 500C- Can phan tch chnh xac en 0,1mg- Bnh hut am- Khay nhom ay co uc lo kch thc lo khoang 1,5mm en 2mm- Bao polietylen, kch thc 200mm100mm0,06mm- Kep dung e kep mieng bao polyetylen

    III. CACH TIEN HANH:

    1. Chuan b mau:

    Chuan b mau th C theo TCVN 6086:1995. Can khoang 10g chnh xac en0,1mg. Can lai mau th a qua may can hai lan. T mau cao su sau khi can xong phaico o day khong qua 2mm. Neu co nhng phan ri ra t mau trong khi can th phai nhatlen cho vao mau.

    2. Say mau th:

    e cac t mau len khay va xep vao tu say. Say trong 4 gi 100 5

    0

    C. Say xongcho ngay mau th vao bao polyetylen. Gap mieng bao lam ba lan va kep kn lai tranhhi am trong khong kh xam nhap vao mau. Thao tac nay phai lam nhanh gon; trongvong 90 giay phai lam xong 5 mau.

    e nguoi mau trong bnh hut am trong 30 phut. Sau o lay mau th ra va can laingay.

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    IV. KET QUA:

    Ham lng chat bay hi (X) tnh bang phan tram theo cong thc:

    Trong o:m1: la khoi lng mau th trc khi say, tnh bang gam.m2: la khoi lng mau th sau khi say, tnh bang gam.

    001m

    mmX

    1

    21

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    BAI 2: XAC NH HAM LNG NIT

    I. NGUYEN TAC:

    Mu cao su c phan huy bang cach un nong vi acid Sulfuric va chat xuc tac,chuyen Nit thanh Amonisulfat. Dung hi nc nong loi cuon Amoniac va hap thu trongdung dch acid Boric bao hoa. Sau o chuan o bang acid Sulfuric chuan.

    II. HOA CHAT - DUNG CU:

    1. Hoa chat:Tat ca cac thuoc th la loai tinh khiet phan tch, nc cat theo TCVN 2117-77

    hoac nc co o tinh khiet tng ng.- Hon hp chat xuc tac dang bot mn, gom:

    30 phan theo khoi lng kali sulfat khan (K2SO4). 4 phan theo khoi lng ong sulfat ngam 5 nc (CuSO4.5H2O). 1 phan theo khoi lng bot salen, hay 2 phan theo khoi lng Natri Selenat

    ngam 10 nc (Na2SeO4.10H2O).- Axt H2SO4 am ac- Axt H2SO4 chuan 0,01N- NaOH 0,1N chuan; NaOH 40%- H3BO3 0,17N: hoa tan 40g H3BO3 vao 1 lt nc cat.

    - Ch th hon hp Tashiro: hoa tan 0,1g metyl o + 0,05g metylen xanh trong 100mlcon 96o

    2. Dung cu:- Bo chng cat Kelan- Can phan tch co o nhay 0,1mg- Cac pipet va buret thong thng

    III. CACH TIEN HANH:

    1. Vo c hoa mau:Can chnh xac khoang 0,1g mau cho vao bnh Keldan + 0,65g hon hp chat xuc

    tac va 3ml H2SO4 am ac. ay mieng bnh bang mot pheu nho, at len tren bep iennghieng mot goc 300 trong tu hut cho en khi phan ng xay ra hoan toan (khoang 1 gi).Luc o dung dch co mau xanh hoac khong mau. Lam nguoi va pha loang vi 10ml nccat.2. Chng cat:

    Chuyen toan bo dung dch trong bnh phan giai Keldal vao bnh chng cat cua bochng cat a chuan b san, trang sach bnh phan giai 2 en 3 lan bang nc cat. o luonnc trang vao bnh chng cat. Cho 10ml acid Boric vao bnh non, them 2-3 giot ch thhon hp, lap ong ngng vao bnh non sao cho au ong ngng nhung vao dung dch.

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    Them 15ml NaOH 40% vao bnh chng cat, trang mieng pheu 5ml nc cat, ongmieng lai, o nc cat ay pheu (at tren mieng bnh). Cho hi nc soi i qua trong 5phut. Sau o ha thap bnh non e au ong ngng pha tren mat dung dch va tiep tuc

    chng cat them vai phut na. Sau o ra sach au ong bang nc cat va hng nc ravao chung vi dung dch.Chuan o dung dch trong bnh non vi acid Sulfuric tieu chuan bang buret co chia

    o en 0,02ml.Chu y: Th vi mau trang: Tien hanh th mau trang cung theo trnh t nh tren

    thay mau th bang 1g Saccaroza.

    IV. KET QUA:

    Ham lng Nit (X3) trong mau tnh bang phan tram theo cong thc:

    X3 =m

    VV ).(028,0 21

    Trong o: V1: The tch acid H2SO4 tieu chuan dung xac nh mau th, ml.V2: The tch acid H2SO4 tieu chuan dung xac nh mau trang, ml.m: Khoi lng cua mau th, g.

    Ket qua th c tnh chnh xac en 0,01%.

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    BAI 3: XAC NH HAM LNG TRO TRONGCAO SU THIEN NHIEN

    I. NGUYEN TAC:

    Goi kn cao su trong giay loc khong tro. Cho vao chen va nung nhiet o 550 0Ccho en khi hoa tro hoan toan. Sau o lam nguoi roi can.

    II. DUNG CU THIET B:

    - Lo nung co bo phan t ong ieu chnh nhiet o, co the at c nhiet o 10000C- Chen nung bang thach anh hoac s, dung tch 50 cm3

    - Giay loc khong tro, ng knh 10 cm15 cm- Can phan tch chnh xac en 0,1mg- Bnh hut am

    III. CACH TIEN HANH:

    1. Chuan b th:Trc khi s dung, cac chen nung phai c ra sach, nung khoang 30 phut nhiet

    o 5500C 250C. Lam nguoi chen nung trong bnh hut am en nhiet o phong va canchnh xac en 0,1mg.

    Cat 1 mieng cao su khoang 5g t mau lay theo TCVN 6086:1995, can chnh xac

    en 0,1mg. Goi kn mau th trong giay loc khong tro va cho vao chen nung2. Tien hanh th:

    Xep cac chen vao lo nung va ieu chnh nhiet o 550 0C 250C. ong ngay calo va nung trong khoang 4 gi. Trong gi au tien, khong c m ca lo e tranh bocchay cac kh de chay. Sau 1 gi, m he ca lo e thong kh vao oxi hoa Cacbon trongcao su. Tiep tuc ot en khi Cacbon b oxi hoa hoan toan va tro co mau trang.

    Lay chen nung ra va cho ngay vao bnh hut am, e nguoi en nhiet o phong. Sauo, em can vi o chnh xac en 0,1mg.

    IV. KET QUA:

    Ham lng tro (X2) c tnh bang phan tram theo cong thc:X2 = 100.

    0

    12

    m

    mm

    Trong o:m0: khoi lng mau th, tnh bang gam.m1: khoi lng chen nung, tnh bang gam.m2: khoi lng chen nung va tro, tnh bang gam

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    BAI 4: XAC NH TONG HAM LNG CHAT RANTRONG CAO SU LATEX

    I. PHAM VI NG DUNG:

    Tieu chuan nay qui nh phng phap e xac nh tong ham lng chat ran cualatex cao su thien nhien co ac, cac loai latex cao su tong hp.

    Phng phap nay khong thch hp cho cac loai latex co nguon goc thien nhienkhac vi Hevea brasiliensis hoac latex a phoi lieu, latex a lu hoa hoac cao su khuyettan nhan tao.

    II. NGUYEN TAC:Mau th c say en khoi lng khong oi trong mot tu say di cac ieu kien

    c qui nh ap suat kh quyen, tong ham lng chat ran, c xac nh bang cachcan trc va sau khi say.

    III. DUNG CU THIET B:

    - a ay phang, thanh thap, ng knh khoang 60mm, co nap ay- Tu say, co the duy tr nhiet o 70 2oC hoac 105 50C

    IV. CACH TIEN HANH:

    Can a co nap ay chnh xac en 1mg. Rot vao a 2.0 0.5g latex, ay nap lai vacan chnh xac en 1mg, lang nhe a e latex bao phu ay a. Neu can thiet rot vao akhoang 1ml nc cat hoac nc co o tinh khiet tng ng va tron eu vi latex bangcach lac nhe.

    at a a m nap nam ngang vao tu say va say nhiet o 105 50C trong hai gicho ti khi mau mat mau het. Lam nguoi trong bnh hut am, ay nap va can. Lap lai quatrnh say tren khoang 30 phut hay 15 phut, cho en khi khoi lng mat i gia hai ketqua can lien tiep nho hn 1mg.

    Sau khi say 105 50C neu t cao su mau th tr nen qua dnh va qua trnh oxyhoa a say ra, lap lai cach th tren nhiet o 70 2oC.

    V. KET QUA:Tong ham lng chat ran (TSC) c tnh bang phan tram khoi lng theo cong

    thc:

    1000

    1 m

    mX

    Trong o: mo: la khoi lng cua mau th,tnh bang gam.m1: la khoi lng mau th sau khi say,tnh bang gam.

    Sai lech ket qua cua hai lan th lap lai khong ln hn 0.2%.

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    BAI 5: XAC NH HAM LNG ONG BANG PHNG PHAPQUANG PHO TRONG CAO SU LATEX

    I. PHAM VI NG DUNG:

    Tieu chuan nay qui nh phng phap quang pho e xac nh tong lng vet cuaong trong cao su tho, latex va cao su phoi lieu, cho ca cao su thien nhien va cao sutong hp.

    Phng phap nay co the ap dung cao su cha silic, vi ieu kien la co s ly bangaxit HF trong qua trnh th.

    Phng phap nay co o nhay nho hn 1mg Cu/kg.

    II. NGUYEN TAC:

    Mau cao su c tro hoa hay phan huy trong hon hp axit HNO 3 va H2SO4 amac. Sau o loai lng Canxi tha (neu co) va tao phc vi bat ky chat Sat nao vi s comat cua Amoni citrat. Sau o kiem hoa, dung dch tach ra c tron vi mot dung dchDietyldithiocarbamat + 1.1.1Tricloroetan e tao thanh va tach ra phan phc hp mauvang cua ong. Dung dch nay c o bang phng phap quang pho ke va so sanh viket qua o dung dch chuan thch hp tren, t o xac nh ham lng cua ong.

    III. HOA CHAT - DUNG CU:

    1. Hoa chat:

    - Natri Sunfat khan- HNO3, H2SO4, HF am ac- Hon hp axit HCl va HNO3 c ieu

    che theo t le: HCl:HNO3:H2O =2:1:3

    - Hydro peroxit 30%

    - NH3 am ac- HCl 5M- Axit Citric: hoa tan 50g axit citric

    trong 100g nc- Dung dch kem dietyldithiocarbamat

    Cach pha:

    - Dung dch Kem dietyldithiocarbamat: hoa tan 1g Kem dietyldithiocarbamat rantrong 1 lt 1.1.1Tricloroetan. Neu dung dch nay khong co san th ta co the ieuchebang cach hoa tan 1g Natri dietyldithiocarbamat trong nc + 2g Kem Sulfatheptahydrat, phan chiet ra co Kem dietyldithiocarbamat c tron lan vi 100ml1.1.1Tricloroetan trong mot bnh tach. Tach lp 1.1.1Tricloroetan va pha loang vi1000ml 1.1.1Tricloroetan. Dung dch nay ben khoang 6 thang khi c bao quantrong chai thuy tinh khong b phan quang.

    - Dung dch ong chuan cha 0,01g/l: can 0,393g CuSO4.5H2O cho vao 1 bechernho hoa tan trong nc. Them 3ml H2SO4 am ac chuyen dung dch qua bnh

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    nh mc mc 1000ml nh mc bang nc cat, dung dch nay dung lam dung dchd tr. Dung 10ml pha thanh 100ml th 1ml dung dch nay cha 0,01mg Cu.

    - Magie oxit, giay pH, gia y loc

    2. Dung cu:- May o quang pho ke co kha nang o dai song khoang 435nm ng vi ong so

    mau thch hp co o dai la 10mm.- Bnh Kendal co dung tch 100ml bang silic hay thuy tinh Boro Silicat- Chen s hoac chen Pt dung tch 50ml.- Pipet 25ml, bnh nh mc 100ml, 1000ml- Can phan tch- Be p ien hoac bep cat- ua khuay bang Pt

    IV. CACH TIEN HANH:1. Chuan b mau th:

    Cat mau thanh tng mieng nho khong ln hn 0,1g. Can chnh xac en 0,001g motmau th co khoi lng t 2g ti 10g, c mau th phu thuoc vao lng ong co mat trongmau co the c chon sao cho mat o quang o c nam trong khoang t 0,20,8 nv.

    2. Pha mau:

    Hoa tan mau th e o ong phai c tien hanh bang cach tro hoa hoac cong pha

    mau th bang axit. Neu mau th cha Clorin th nen dung phng phap cong pha maubang axt.Pha mau theo phng phap tro hoa:

    Sau khi tro hoa, them vao vai giot axit H2SO4 am ac va un cho boc hi. enguoi va them vao 3 giot axit H2SO4 am ac na va 5 ml axit HF am ac, untren bep ien hoac bep cach cat, khuay eu bang ua platin va lam bay hi enkho can. Lap lai qua trnh tren 2 lan hoac lam cho en khi nhan thay toan boSilicat bien mat, khi ay khong con khoi trang cua Silicon tetrafluorid.

    e nguoi, lam t chen tro vi mot lng t 0,5ml ti 1ml nc, them vao 10mlhon hp axit HCl : HNO3 : H2O = 2 : 1 : 3, ay kn bang mat knh ong ho va un

    1000

    C t 30 60 phut, chuyen lng dung dch vao trong bnh tam giacPha mau theo phng phap axit:

    Can 2g mau th, pha mau th vi 4ml H2SO4 am ac + 3ml HNO3 am actrong bnh kendan, un nong bnh tren bep ien. Neu phan ng xay ra qua manh,lam nguoi bnh trong mot ly nc lanh. Khi phan ng ban au giam, un nhe honhp cho en khi ngng phan ng manh va ke en un manh hn na cho en khihon hp sam mau. Them 1ml HNO3 am ac, un nong hon hp sau moi lan themaxit cho en khi hon hp sam mau. Tiep tuc thao tac nay cho en khi dung dch trnen khong mau hoac co mau vang nhat va khong u lam sam mau khi un themna. Neu viec phan huy mau b keo dai, can phai them 1ml H2SO4 am ac e

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    ngan chan hon hp b ong ran. Pha huy hoan toan cac vet hu c, e nguoi dungdch va them 0,5ml H2O2 30% va 2 giot HNO3 am ac. Sau o dung dch cho bochi, lap lai viec them vao va un cho en khi mau cua dung dch khong con giam

    na. Lam nguoi dung dch, pha loang 10ml nc va lam bay hi. Cuoi cung lamnguoi dung dch va them vao 5ml nc. Neu dung dch th giai oan nay khong co chat hoa tan, chuyen axit pha mau ti

    mot bnh tam giac va ra bnh kendan vi 3 lan moi lan 5ml nc, toan bo ccho vao bnh tam giac. Tuy nhien neu dung dch th cha chat khong hoa tan, locphan dung dch ben tren qua giay loc, dung dch qua loc c hng trong bnh tamgiac, loc sao cho gi lai chat khong tan trong bnh kenan cang nhieu cang tot.Them vao 5ml HCl am ac vao bnh kenan, un dung dch en soi va lac manhe ra thanh bnh. Loc qua giay loc vao bnh tam giac. Ra bnh kenan vi 3 lanmoi lan 5ml nc, chung cung c gom vao bnh.

    Them 5ml dung dch axit Citric 50% vao bnh tam giac va neu,khi lam nguoi dungdch van trong, trung hoa no bang cach them vao tng giot dung dch NH3 am acth bang giay pH. Neu Canxi Sunfat ket tinh ben trong dung dch khi lam nguoi,th lam lanh bnh va hon hp ti 100C, loc vao trong bnh tam giac th 2, ra va loc3 lan, moi lan 2ml nc lanh trc khi trung hoa bang NH3, lam nguoi dung dchdi voi nc, chuyen vao mot pheu tach, them 2ml dung dch NH 3 na va sau othem nc e pha loang khoang 40ml. Dung pipet hut 25ml dung dch Kemdietyldithocarbamat cho vao dung dch va lac 2 phut. Ngay sau khi tach lp, chietlp 1.1.1Tricloroetan vao trong bnh co nut ay cha 0,1g Na2SO4 khan. Neu dungdch con uc sau khi e yen 30 phut th them chut t Na2SO4 khan na cho en khi

    dung dch tr nen trong. Loc dung dch 1.1.1 tricloroetan qua lp bong thuy tinh hay giay loc bang xanh,dung dch qua loc em o quang bc song 435nm, dung dch so sanh la dungdch 1.1.1 tricloroetan.

    3. Chuan b ng chuan:

    Chuan b mot loat dung dch chuan, moi dung dch cha 5ml H2SO4 am ac +10ml nc.

    Them vao moi dung dch nay mot lng dung dch ong chuan thay oi t 0 10ml, sau o them 5ml axit Citric 50%. Them tng giot dung dch NH3 am acsao cho dung dch co tnh kiem nhe (th bang giay quy).

    Lam nguoi dung dch va chuyen vao 1 pheu rieng biet va them vao moi dung dch2ml dung dch NH3 na. Hut 25ml dung dch Kem dietyldithiocarbamat lac trong 2phut. Nay sau khi tach lp, chiet lp 1.1.1Tricloroetan vao 1 bnh co nap ay chakhoang 0,1g Na2SO4 khan. Tng dung dch 1.1.1Tricloroetan nay loc qua giay locva o bc song 435nm.

    V. KET QUA:1. Bang o th hieu chuan, xac nh nong o cua ong tng ng vi tr so hieu chnh

    va t o tnh toan ra ham lng cua ong co trong mau.2. Ket qua cua ong c tnh bang mgCu/kg?

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    BAI 6: XAC NH HAM LNG MANGAN BANG PHNG PHAPHAP THU QUANG PHO CUA NATRI PERIODAT

    TRONG CAO SU LATEX

    I. PHAM VI NG DUNG:

    Tieu chuan nay qui nh cac phng phap hap thu quang pho e xac nh Mangansau qua trnh oxi hoa vi Natri periodat trong cac loai cao su va latex cao su.

    Phan mot qui nh phng phap cho cao su phoi lieu hay cao su lu hoa ma khongcha Clo, phng phap khong b anh hng bi cac chat on tr co khoi lng nang

    chang han nh Silicat t nhien va tong hp, cac dang Canxi cacbonat khac nhau, hoacco mat cac chat phoi lieu tao thanh Photphat khong hoa tan trong cac ieu kien thnghiem.

    Phan hai qui nh cho phng phap dung cho cao su tho, latex va cao su phoi lieukhong cha cac chat on nang (ln hn khoang 10%) cua chat on tr Silicat hay bat kychat nao chang han nh Titan dioxit trong cac ieu kien th nghiem se tao thanhPhotphat khong tan. Phng phap co the c ap dung cho cao su thien nhien va tonghp khong cha Clo.

    II. NGUYEN TAC:

    Tro hoa cao su trong mot chen platin sau o nau chay tro vi Natri fluoroborat.Sau khi s ly bang cac axi Nitric va axit Sunfurit pha loang, chuyen cac chat long khongtan va oxi hoa cua Mangan thanh permanganat bang cach un soi bang dung dch Natriperiodat. o mat o quang pho vao khoang 525 nm cua dung dch nay cho biet s hapthu tng ng vi nong o cua Mangan.

    III. HOA CHAT - DUNG CU:

    1. Hoa chat:

    Natri fluoroborat: Neu loai tinh khiet phan tch khong co san, thuoc th nay sec chuan b nh sau: Hoa tan 110g Natri fluoroborat loai ky thuat trong 100 ml

    nc am 30

    o

    C. Sau khi loc qua mot t giay loc lam nguoi dung dch en nhiet ophong va them 100 ml etanol 96% trong khi khuay. Loc lay cac tinh the ket tuatren t giay loc trong mot cai pheu Buchener va loai nc hoan toan trong chankhong yeu, sau o chuyen qua mot cai chen s ay nong hay ua thuy tinh va say khoang 50oC trong chan khong.

    Natri periodat. Axit sunfuric, = 1.84 g/ml. Axit nitric, = 1.42g/ml. Nc on nh: Lay khoang 1 dm3 nc, them vao khoang 0.1 g Kali permanganat

    cung vi mot vai giot axit Sunfuric. Chng cat nc, loai bo 50 cm3 au va cuoi

    cua nc cat. Phan con lai cho vao bnh thuy tinh co nut ay.

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    Dung dch Kali permanganat, khoang 0.30 g/ l. Mangan, dung dch tieu chuan co 10 mg Mangan/dm3.

    Cac dung dch Mangan sau ay co the dung c:

    Can 0.720g Kali permanganat (KMnO4) trong mot cai coc nho va hoa tan trongnc co cha 2 ml axit sunfuric . Sau o them nc ro un soi dung dch trong15 phut, lam nguoi, chuyen qua bnh nh mc 500 ml va pha loang vi nc tivach nh mc

    Can 0.770 g Mangan sunfat (MnSO4.H2O) trong mot cai coc nho va hoa tan trongnc co cha 2 cm3 axit Sunfuric am ac. Chuyen dung dch vao vao mot bnhnh mc 500 ml va pha loang ti vach nh mc. Dung dch nay phai c onnh t nhat la mot thang. Hut 10 ml cua dung dch b cho vao mot bnh nh mc500 ml th hai va pha loang vi nc lai mot lan na ti vach nh mc, 1 ml cuacac dung dch tieu chuan nay cung cha 0.01 mg Mangan. Chuan b dung dch

    trc khi dung.2. Dung cu:

    May so mau Chen platin 30 ml Tam cach nhiet, day khoang 6 mm va vuong canh 100mm co mot lo chnh gia

    e gi chen sao cho hai phan ba cua chen hng ve pha di tam cach nhiet. Lo nung Loc thuy tinh, loai xop P40

    IV. CACH TIEN HANH:

    1. Chuan b mau th:

    Cao su thien nhien:Chuan mau th t mot mau hoac nhieu mau hoac bang cach cat cao su thanh tng

    manh nho, moi manh co trong lng khoang 0.1g. Can 10g mau th chnh xac en10mg. Cao su Latex:

    Lay mot phan mau latex nc a c tron ky co cha khoang 10g tong hamlng chat ran en khi khoi lng khong oi va cat thanh tng manh nho.

    Cao su a lu hoa:

    Tao t hay hat trong mot may can, hoac chia nho bang tay mot mau th 10 g.Chu y: tat ca cac giai oan chuan b mau, lam can than tranh s nhiem ban cao.

    2. Tro hoa mau th:

    Chon khoi lng mau th sao cho no cha khong qua 1g Titan dioxit. Chuyenphan mau th vao mot chen platin a can trc e chen len tam cach nhiet.

    Bat au chuan b mot dung dch trang cung mot luc bang cach dung mot coc tngt nhng khong co mau th va tiep tuc x ly phan mau th va mau trang trongcung mot phng phap giong nhau. ot chen mau bang mot ngon la ga nho cho

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    en khi con lai phan than kho va chuyen chen qua lo nung c duy tr nhiet o550oC 25oC va nung cho en khi tat ca cacbon b oxi hoa.

    Sau o lam nguoi chen trong bnh hut am, can chen e xac nh khoi lng tro va

    dung pipet sach them vao mot lng axit Sufuric am ac nho tng giot xungquanh thanh mieng chen e lam am eu tro. un en khi cho het khoi va nung lai 550oC trong vai phut. Lap lai cach lam am tro bang axit Sunfuric bang cachthem axit nh trc t mot pipet va un nhe cho en khi het khoi va nung lai 550oC trong vai phut. Sau khi lam nguoi nhiet o phong, them vao chen 8 phankhoi lng cua Natri fluoroborat mc toi a la 8g, t mot phan khoi lng tro.un nhe chen trong mot lo cong pha cho en khi hon hp c chay hoan toan, roigi yen cho en khi vat lieu b nau chay tr nen trong suot, hay cho en khi khongcon phan ng xay ra na va bat ky chat ran khong tan nao c phan tan trongchat long nau chay.

    3. S hoa tan:Lam nguoi chen nhiet phong, va them vao 12ml nc on nh va 4 ml axit

    Sunfuric am ac. Sau khi un nhe e hoa tan cac chat b ong ket, rot toan bo mautrong mot bnh non 100ml va x ly cac chat cha trong chen bang 10ml nc on nh vathem vao 2ml axit Sunfuric am ac cung se c cho vao bnh non.

    Cho them vao 5 ml axit Sunfuric am ac vao bnh va sau o rot dung dch quali loc bong thuy tinh sach, ra li loc mot lan bang 5ml nc on nh nong, chuyenchat long qua mot bnh hnh non khac, ra vi nc on nh, va them nc vao e co thetch tong cong la 40ml, them vao 0.3g Natri periodat va un soi dung dch. Tiep tuc un

    soi nhe trong 10 phut e am bao len ung mau. Sau khi lam nguoi, bat ky chat m ucnao nh Kali periodat b ket tua co the lam trong suot bang cach ly tam hay loc qua liloc P40.

    Chuyen dung dch vao mot bnh nh mc 50ml va pha loang ti vach nh mcbang nc on nh 20oC. Sau khi pha, mau sac phai on nh trong vai gi. Bat ky tnhhuong phai mau nao la do chat hu c va Clorit cha kh het. Neu ieu nay xay ra, laplai viec xac nh nhng dung them axit Sunfuric e x ly theo phan a.

    4. Chuan b ng chuan:

    Chuan b cac dung dch pha mau chuan:Chuan b mot loat dung dch pha mau chuan moi dung dch cha 25 ml nc on

    nh, 6 ml axit Sunfuric am ac va 5 ml axit Nitric am ac. T cac dung dch nay,them phan dung dch Mangan chuan thay oi t 0 en 10ml cung vi moi trng hp0.3g Natri periodat. un cac dung dch trong 10 phut e am bao len ung mau, cuoicung lam nguoi va pha loang vi nc on nh ti 50ml trong bnh nh mc. o quang pho:

    Ra ong so mau cua may o quang ien hay quang pho ke, trc tien bang dungdch Kali permanganat sau o vi nc on nh va sau cung la dung dch so mau chuanthch hp. Lay ay dung dch so mau chuan va o s hap thu bc song hap thu toi a(khoang 525 nm).

    Hieu chuan so oc bang cach tr i phan hap thu cua dung dch bu them vao

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    Cach xac nh:Ra ong so mau cua may o mau quang ien hoac quang pho ke trc tien bang

    dung dch kali permanganat sau o vi nc on nh va sau cung la dung dch th.

    Sau o o ay dung dch chuan va o o hap thu cua dung dch bc song cdung trong viec chuan b o th hieu chuan.Hieu chuan tr sobang cach tr i o hap thu cua dung dch trang c x ly tng

    t.Ve o th hieu chuan, xac nh nong o cua Mangan tng ng vi tr so hieu

    chnh va t o tnh ra ham lng Mangan cua mau th.

    V. KET QUA:

    1. Ket qua la gia tr trung bnh cua ket qua hai lan th nghiem.2. Tnh ket qua theo miligam cua Mangan tren kilogam cua mau.

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    CHNG 2: PHAN TCH CHAT TAY RA

    BAI 1: XAC NH Na2O VA SiO2 TRONG NATRISILICATNGUYEN LIEU SAN XUAT CHAT TAY RA

    I. NGUYEN TAC:

    Trong Natrisilicat co ham lng Na20, ta thc hien phan ng chuan o bang HClvi ch th bromothymol xanh tai iem tng ng dung dch se chuyen t mau xanhsang mau vang, sau o ta them KF va HCl vao dung dch co mau vang va ta tiep tucchuan dung dch bang Na0H, tai iem tng ng dung dch chuyen t mau vang sangmau xanh.

    Na2O + 2HCl = 2NaCl + H2OSiO2 + 6KF + 2H2O = K2SiF6 + 4KOHKOH + HCl = KCl + H2OHCl + NaOH = NaCl + H2O

    II. HOA CHAT DUNG CU:

    - Coc nha

    - Pipet 25ml- Bnh nh mc 100ml- NaOH 0.5N- HCl 0.5N- KF tinh the

    - Bnh nh mc 100ml

    - NaOH 0.5N- HCl 0.5N- Ch th bromothymol xanh- Ch th phenolpthalein- KCl tinh the

    III. CACH TIEN HANH:

    1. Xac nh Na2O co trong Natrisilicat:

    Can khoang 2 gam mau (o chnh xac 0.0001g), sau o cho them mot t nc catnong va khuay cho ti tan roi nh mc 100ml.

    Hut 25ml cho vao bnh nha + 3 giot Bromothymol xanh, chuan lai bang HCl0.5N cho ti khi dung dch chuyen xanh sang vang, dung dch gi lai e xac nh SiO2.

    % Na20 =m

    NVHCL

    4,12)(

    Trong o:N,V : la nong o va the tch cua HClm : khoi lng mau

    2. Xac nh SiO2:

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    Them vao bnh nha 2.5 g KF lac nhe cho tan het, dung dch co mau xanh, cho25ml HCl 0.5N vao dung dch co mau vang + 10g KCl lac eu, e yen trong 10 phut,dung NaOH 0.5N chuan lng acid d cho ti khi dung dch chuyen t mau vang sang

    xanh% SiO2 =

    m

    ].6(NV)[(NV)OHH

    Trong o:N,V : the tch va nong o cua acid va baz a dung chuan o.Modul silicat :

    M =O%Na

    .1,0323%SiO

    2

    2

    62

    69

    M

    M

    ONa

    SiO

    2

    i2 1,0323

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    BAI 2: XAC NH HAM LNG LAS - NGUYEN LIEUSAN XUAT CHAT TAY RA

    I. NGUYEN TAC:

    Xac nh chat hoat ong anion trong moi trng cha pha nc va Clorofom bangcach chuan o vi mot lng the tch dung dch chuan chat hoat ong dang Cation(benzetoni clorua) co mat thuoc th la hon hp thuoc nhuom Cation (dimitibromua) vathuoc nhuom Anion (disunfin xanh)

    II. HOA CHAT - DUNG CU:

    - Dung moi Clorofom- Hyamine (C27H42ClNO2) :0.004N- Ch th acid- Ch th phenolpthalein 0.1%

    - NaOH 0.5N- Bo may chuan o hai pha- Bnh nh mc 500 ml- Pipet 2ml

    III. CACH TIEN HANH:

    Can khoang 2g Las vao coc thuy tinh 100ml, hoa tan bang nc nong sau o nhmc thanh 500ml bang nc cat va cho ca t len khuay that eu trong 10 phut.

    Dung pipet hut 2ml dung dch Las tren cho vao may chuan o hai pha, them 2-3giot ch th PP sau o dung NaOH 0.5N chnh cho ti khi dung dch co mau hong

    Dung ong ong lay khoang 20ml nc cat +10ml hon hp ch th acid+ 5ml CHCl3bat may khuay, khuay eu. Chuan o bang Hyamine 0.004N cho ti khi mau hong cualp CHCl3 va mat i va xuat hien mau tm khoai mon th dng chuan o.

    % AD =mV.1000

    100.VM.)NV(

    x

    mLasminhya

    Trong o: m: khoi lng mauV: the tch hyamine chuanM: phan t lng cua las (322)

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    BAI 3: XAC NH NaOH NGUYEN LIEUSAN XUAT CHAT TAY RA

    I. NGUYEN TAC:

    V NaOH luon hap thu mot lng ln CO2 nen trong dung dch NaOH luon coNa2CO3. Khi chuan o NaOH bang dd HCl, NaOH c trung hoa ong thi Na 2CO3cung c trung hoa en nac th nhat ng vi s oi mau cua ch th PP (chuyen t mauhong sang khong mau) sau o nac th hai cua Na2CO3 tiep tuc trung hoa ng vi s oimau cua ch th MO (chuyen t mau vang sang cam).

    NaOH + HCl = NaCl + H2ONa2CO3 + HCl = NaHCO3 + NaClNaHCO3 + HCl = NaCl + CO2 + H2O

    II. HOA CHAT:

    - Dung dch chuan HCl 0.5N- Ch th phenolpthalein- Ch th MO

    III. CACH TIEN HANH:

    Can khoang 0.4g mau cho vao erlen 250ml (phai thao tac nhanh e tranh anh

    hng cua CO2) them mot t nc cat sau o cho them 3 giot ch th PP, va dung HCl0.5N e chuan, iem tng ng nhan c khi dung dch chuyen t mau hong sangkhong mau, ghi the tch V1. Them tiep vao o hai giot MO, tiep tuc chnh bang HCl0.5N en khi dung dch chuyen t vang sang cam, ghi the tch V2.

    Cong thc: % NaOH =m

    4).VV(N 21

    Trong o: V1: the tch HCl dung e chuan o vi PPV2: the tch HCl dung e chuan o vi MON: nong o HCl

    m: khoi lng mau can

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    BAI 4: XAC NH Na5P3O10 VA Na2SO4 - NGUYEN LIEUSAN XUAT CHAT TAY RA

    I. NGUYEN TAC:

    e xac nh Na5P3O10 ngi ta chuyen hoa hoan toan tat ca cac dang photphatve dang orthophosphat bang acid HCl va no c chuan o pH t 4.3 en 8.8 bang dungdch NaOH chuan.

    Na5P3O10 + 2HCl + 2H2O = 3NaH2PO4 + 2NaClNaH2PO4 + NaOH = Na2HPO4 + H2O

    e xac nh Na2SO4 ngi ta ket tua goc sunfat bang bari clorua tao thanh kettua BaSO4, can khoi lng ket tua t o tnh ra ham lng natri sunfat co trong bot giat.

    Ba2+ + SO42- = BaSO4

    II. HOA CHAT - DUNG CU:

    - Dung dch HCl 1:1- Dung dch NaOH 0.5N- HCl 1:5- BaCl 10%- AgNO3 1%- Dung dch MO 0.1%

    - Burett 25ml- May o pH- Lo nung- Chen nung- Can phan tch

    III. CACH TIEN HANH:

    1. Xac nh Na5P3O10:

    Can khoang 5g mau, sau o ta tro hoa mau tren bep ien trong vong 20 phut, vacho vao becher 250ml hoa tan mau bang 100ml nc cat ta cho them 20ml HCl 1:1 vaun soi trong vong 30 phut. Luc o tat ca cac dang Photphate c chuyen thanhorthophotphat.

    e nguoi ti nhiet o phong, them khoang 10ml NaOH 30% e trung hoa btlng HCl d, sau o dung may o pH va ieu chnh pH cua dung dch ve khoang 4.3

    bang NaOH 0.5N, sau o tien hanh chuan o bang NaOH 0.5N en khi pH = 8.8, ghi thetch NaOH a dung.

    2. Xac nh Na2SO4:

    Can khoang 2g mau (chnh xac 0.0001g) vao becher 250ml. Hoa tan mau bangnc cat, un tren bep cach thuy cho soi, nho vao becher vai giot MO va dung acid HCle trung hoa cho en khi xuat hien mau hong o roi tiep tuc them 3-5 ml acid na, rot tt dung dch BaCl210% vao va khuay eu un nhe them vai phut na roi cho 5mlBaCl210% vao xem con ket tua hay khong, neu con th tiep tuc them Bari clorua, neuthay het th dng.

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    ay becher bang mat knh ong ho sau o un nhe them 10 phut. Loc tu a quagiay loc bang xanh. Dung bnh tia nc nong ra trang coc va don tat ca mau xuongpheu loc, ra mau bang nc nong cho ti khi het ion Cl- (th bang AgNO3).

    Can than cho vao chen s a nung en khoi lng khong oi. em tro hoa trenbep ien cho giay chay t t sau o cho vao trong lo nung va nung 800 oC trong vong30 phut e trong tu hut am, sau khoang 15 phut th em can ta c khoi lng m2.

    IV. KET QUA:

    1. Xac nh Na5P3O10:

    Lng Na5P3O10 c tnh theo cong thc sau:

    % P2O5 =m

    (NV)OH

    7,098

    % Na5P3O10 = % P2O5 .1,7277

    Trong o:N, V: nong o va the tch NaOH 0.5N dung chuan

    2. Xac nh Na2SO4:

    Lng Na2SO4 c tnh theo cong thc sau

    %Na2SO4 =m

    mm 100.60857,0).( 12

    Trong o:m1: khoi lng chen canm2: khoi lng chen + mau

    m : khoi lng mau can ban au0,60857: he sochuyen oi t Natri sunfat sang Barisunfat

    233

    142

    4

    42 BaSO

    SONa

    M

    M= 0,60857

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    BAI 5: XAC NH HAM LNG PHOTPHATTRONG BOT GIAT

    I. NGUYEN TAC:

    Cac muoi Photphat trong bot giat c chuyen sang dang Octophotphat va chuanbang Natrihidroxit theo ch th Phenolphtalein .

    II. HOA CHAT - DUNG CU:

    - HCl (d = 1.19)

    - NaOH 0.1N- NaOH 30% khong co cacbonat- Metyl da cam dung dch 0.1% trong

    nc

    - Chen s hoac da s 50ml

    - Lo nung co ieu chnh nhiet o- Coc un 250ml- Bnh nh mc 250ml- Phenoltalein, dung dch 0.1% trong

    ru etylic

    III. CACH TIEN HANH:

    Can 5g bot giat vi o chnh xac 0.001g cho vao chen s, ot tren bep ien cho enkhi phan ln chat chay c chay het, chuyen che n s sang lo nung, nung 550oC trongkhoang 10-15phut, chat con lai co tro xam. e nguoi them can than 10ml HCl, chuyen

    sang coc 250ml, trang chen s bang nc cat, gop vao coc, them nc en khoang100ml. ay mat knh ong ho, un soi nhe trong 30 phut. e nguoi chuyen vao bnhnh mc 250ml, nh mc en vach, lac ky, loc qua phieu kho, giay loc kho vao cockho. Trang bo phan nc loc au. Lay 50ml dung dch loc cho vao coc 250ml, them0.5ml Metyl da cam, trung hoa luc au bang Natrihidroxit 30% gan en iem chuyenmau, them tng giot Natrihidroxit 0.1N en khi mau dung dch chuyen t o sang vangsang. Them 0.5ml Phenolphtalein, chuan o vi Natrihidroxit 0.1N en khi mau dungdch chuyen sang hong.

    IV. KET QUA:

    Ham lng Photphat quy ra P2O5 tnh bang % theo cong thc:

    X = V*0.003549*100 /mTrong o:

    V: The tch dung dch natrihidroxit 0.1N a chuan o, ml0.003549: Lng P2O5 tng ng 1ml dung dch natrihidroxit 0.1Nm: Khoi lng mau th e chuan o, g

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    BAI 6: XAC NH pH CHAT BAY HI CHAT KHONG TANTRONG BOT GIAT

    I. HOA CHAT - DUNG CU:

    - Mat knh ong ho- Bnh hut am- Tu say ieu chnh nhiet o 100-105oC- Can phan tch, o chnh xac 0.001g- Thuoc th phenolphtalein

    - Coc dung tch 250ml- Chen loc xop G4- Can phan tch- May o pH

    II. CACH TIEN HANH:1. Xac nh o pH:

    Can 5g mau th chnh xac en 0.001g cho vao bng nh mc 500ml, hoa tan maubang 100ml nc cat, them nc en vach nh mc. o pH bang giay ch th van nanghoac bang may o pH dung ien cc ch th la ien cc thuy tinh va so sanh la Calomen.

    2. Xac nh ham lng nc va chat bay hi:

    a. Tie n hanh xac nh:

    Can 2g mau th vi o chnh xac en 0.001g vao mat knh ong ho (a c say

    kho en khoi lng khong oi va can chnh xac ti 0.001g), cho vao tu say va say nhiet o 100- 105oC sau ba gi lay ra e nguoi trong bnh hut am en nhiet o phong ,roi can, sau o cho vao tu say tiep. C sau 1 gi lai em ra e nguoi va can lai nh tren.Khoi lng khong oi at c khi chenh lech khoi lng gia hai lan can ke tiep khongvt qua 0.0056g.

    b. Tnh ket qua:

    Ham lng nc va chat bay hi (X) tnh bang % theo cong thc :

    X = (m m1)*100 /m

    c. Trong o:

    m Khoi lng mau trc khi say, gm1 Khoi lng mau sau khi say, g

    3. Xac nh ham lng chat khong tan trong nc:

    a. Tien hanh xac nh:

    Can 2g mau bot giat (kem giat) vi o chnh xac 0.001g vao coc 250ml, them100ml nc cat nong 80-90oC. Hoa tan mau e lang, loc qua chen loc xop G4 (a sayen khoi lng khong oi va can chnh xac en 0.001g) hoac giay loc thng (a csay kho va can trc). Ra can bang nc cat nong nhieu lan cho en khi nc ra

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    khong con tnh kiem vi thuoc th phenolphtalein. Say kho chen loc (giay loc) 100-105oC cho en khi khoi lng khong oi. e nguoi va can.b. Tnh ket qua

    Ham lng chat khong tan trong nc (X), tnh bang % theo cong thc sau:X = (m2 m1)*100 /m

    Trong o:m2 Khoi lng chen loc (giay loc) cha can sau khi say, gm1 Khoi lng chen loc (giay loc), gm Khoi lng mau th, g

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    BAI 7: PHAN TCH HAM LNG GLYCERIN VA CACBONATTRONG KEM ANH RANG

    I. NGUYEN TAC:

    e nh lng ham lng Glycerin ngi ta da vao phan ng oxy hoa kh cuaGlycerin vi Kali periodat trong moi trng axit Clorhydric, Kali periodat d tac dungvi Kali Iodua giai phong lng Iod tng ng. nh lng Iod sinh ra bang dung dchNatrithiosulfat t o tnh ra ham lng Glycerin co trong mau.

    e nh lng ham lng Cacbonat ngi ta da tren c s tao thanh phc bencua Canxi va Magie vi EDTA pH = 10 vi ch th ETOO.

    II. HOA CHAT - DUNG CU:

    - Be p cach thuy- Dung dch Na2S2O3 0,1N- Dung dch KIO4 0,1N- Dung dch KI 10%- Ch th ETOO

    - Dung dch NaOH 10%- Dung dch em pH = 10.- Dung dch EDTA 0.01M- Ho tinh bot- Dung dch HCl 1:1

    III. CACH TIEN HANH:

    1. Chuan b mau:Can chnh xac khoang 1g mau kem anh rang vao beacher 250ml. Them 5ml HCl

    1:1 dung ua thuy tinh dam mau va nhe tren bep cach thuy cho en tan hoan toan. enguoi chuyen mau vao bnh nh mc mc 250ml. Dung nc cat trang ra coc nhieulan, don tat ca nc trang vao bnh nh mc mc, nh mc ti vach, lac eu ta thuc dung dch A.

    2. Xac nh Glycerin:

    Dung pipet hut chnh xac 10ml dung dch mau A cho vao bnh non nut nham250ml. Them chnh xac 25ml dung dch KIO4 0,1N, lac eu mau va e yen 15 phut. Laymau ra cho 20ml dung dch HCl 1:1 + 20ml dung dch KI 10%. Lac tron, ay nut va eyen trong bong toi 5 phut. Sau o dung nc cat trang t co bnh xuong. Chuan bangdung dch Na2S2O3 0,1N cho ti mau vang rm them 5 giot ch th ho tinh bot, tiep tucchuan cho ti khi dung dch chuyen t mau xanh sang khong mau. Ghi the tch Na 2S2O3tieu ton.

    Tien hanh mot mau trang song song.

    3. Xac nh Cacbonat:

    Dung pipet hut chnh xac 10ml dung dch A cho vao erlen 250ml. Them vao10ml dung dch em pH = 10 + mot t ch th ETOO. Chuan bang dung dch EDTA

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    0.01M cho en khi dung dch chuyen t mau o nho qua xanh lam. Ghi the tch EDTAtieu ton.

    Tien hanh mot mau trang song song.

    IV. KET QUA:1. Tnh ham lng Glycerin:

    Ham lng glycerin (X) tnh bang % theo cong thc sau:

    m10

    5,755)V(VX 21

    Trong o: V1 : the tch cua dung dch Na2S2O3 0,1N tieu ton khi chuan mau trang (ml) V2 : the tch cua dung dch Na2S2O3 0,1N tieu ton khi chuan mau that (ml) m : khoi lng mau

    2. Tnh ham lng Cacbonat:

    Ham lng cacbonat c tnh theo cong thc sau:

    m

    VVX

    5,2)( 21

    Trong o: V1 : la the tch cua dung dch EDTA tieu ton khi chuan mau trang (ml) V2 : la the tch cua dung dch EDTA tieu ton khi chuan mau that (ml) m: la khoi lng mau

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    BAI 8: XAC NH HAM LNG NATRI CACBONAT

    I. NGUYEN TAC:

    Ham lng natri cacbonat trong nc ra chen c xac nh bang dung dch axitSufuric vi ch th Metyl da cam.

    II. HOA CHAT - DUNG CU:

    - Dung dch H2SO4 0,1N- Ch th metyl da cam 0,1%- Buret 25ml

    - Pipet cac loai- Erlen 250ml

    III. CACH TIEN HANH:

    Can chnh xac khoang 2g mau, hoa tan bang 50ml nc cat + 4 giot ch th MO.Chuan bang dung dch H2SO4 0,1N cho en khi dung dch chuyen t mau vang cam sangmau hong nhat. Ghi the tch H2SO4 tieu ton.

    IV. KET QUA:

    Ham lng Cacbonat Canxi c tnh theo cong thc sau:

    1000053,0

    m

    VX

    Trong o:V: the tch dung dch H2SO4 0,1N tieu tonm: khoi lng can cua mau th

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    BAI 9: XAC NH HAM LNGCHAT HOAT ONG BE MAT

    I. NGUYEN TAC:

    Chat hoat ong be mat c tach ra khoi bot giat (kem giat) bang ru etylic 96o

    (bot giat) hoac tuyet oi (kem giat) va c tnh sau khi tr nhng thanh phan khac cungtan trong ru etylic.

    II. HOA CHAT VA DUNG CU:

    1. Hoa chat:

    - Ru etylic tuyet oi hoac 96o

    - Dung dch H2SO4 0.1N- Ch th Metyl dacam 1%

    - Dung dch AgNO3 0.1N- Dung dch MgSO4 20%

    - Kalicromat dung dch 5%: hoa tan 5g kalicromat trong nc cat, them dung dch bacnitrat 0.1N cho en khi xuat hien mau o nhat. Loc pha loang en 100ml.

    2. Dung cu:

    - Hai bnh non co nham, dung tch 100ml- Mot coc dung tch 250ml

    - Mot ong ngng hi thang- Mot ong ngng hi ngang- Bep cach thuy- Tu say

    - Bnh hut am- Can phan tch o chnh xac 0.001g

    - Pheu loc, giay loc thng.- Bnh non 250ml- Bnh nh mc 250ml- Buret 25ml

    III. CACH TIEN HANH:

    1. Xac nh chat tan trong ru:

    a. Cach lam:Can khoang 2g mau th chnh xac en 0.001g vao coc 250ml, them 50ml ru

    etylic 95o (neu la bot giat) hoac ru tuyet oi (neu la kem giat). ay coc bang mat knh

    ong ho, un nong tren bep cach thuy, khuay cho mau phan tan hoan toan.e lang va loc vao trong bnh non 100ml a say kho 100 -105oC en khoi

    lng khong oi va can chnh xac en 0.001g. Khi loc gan co gi can trong coc cangnhieu cang tot.

    Tiep tuc lap lai qua trnh tren hai lan, moi lan vi 200ml ru etylic. Sau o catthu hoi ru cua dung dch loc trong bnh non tren bep cach thuy cho en khi ch con laican. Say bnh cha can 100-105oC en khoi lng khong oi.

    e nguoi trong bnh hut am, can chnh xac en 0.001g.b. Tnh ket qua:

    Ham lng chat tan trong ru (X1) tnh bang % theo cong thc:

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    X1 = (m2 m1) *100 /m

    Trong o :m2 Khoi lng bnh non va can, g

    m1 Khoi lng bnh non, g2. Xac nh ham lng Na2CO3 tan trong ru:

    a. Nguyen tac:Ham lng Natricacbonat tan trong ru xac nh bang cach chuan o vi acid

    theo ch th Metyl da cam.b. Tien hanh xac nh :

    Hoa tan chat tan trong ru trong nc cat, them vai giot ch th Metyl da cam vachuan o bang acid sunphuric en khi dung dch chuyen t vang da cam, sang o, dungdch sau khi chuan o gi lai e xac nh Clo.

    c. Tnh ket qua:Ham lng Natri cacbonat (X2) tnh bang % theo cong thc:

    X2 = V*0.0053*100 /m

    Trong o: V :The tch dung dch acid suphuric 0.1N a dung, ml 0.0053 : Lng Natricacbonat tng ng vi 1ml aicd sunphoric 0.1N m : Kho i lng mau th ,g

    3. Xac nh ham lng muoi Clorua tan trong ru:

    a. Nguyen tac:Ham lng muoi clorua qui ra NaCl c chuan o vi AgNO 3 theo ch thKalicromat.b. Tie n hanh xac nh:

    Dung dch sau khi xac nh Natricacbonat, ieu chnh en khoang pH = 6-8 them10ml Magie nitrat, un nong tren bep cach thuy en khi xuat hien ket tua.

    e nguoi, chuyen vao bnh nh mc 250ml, them nc en vach, lac ky, loc quagiay loc kho, pheu kho va hng dung dch loc vao bnh non kho, trang bo phan nc locau.

    Lay 100ml vao trong bnh non them 1ml dung dch Kalicromat, chuan o bang

    dung dch AgNO3 en khi mau cua dung dch co mau o gach ben. ong thi tien hanhmot mau trang.c. Tnh toan ket qua:

    Ham lng muoi clorua quy ra NaCl tan trong ru (X 3) tnh bang % theo congthc.

    X3 = (V1 V2)*0.00585*100/m

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    Trong o : V1 : The tch dung dch AgNO3 0.1N a chuan o mau th, ml. V2 : The tch dung dch AgNO3 0.1N chuan o mau trang

    0.00585 : Lng NaCl tng ng vi 1ml dung dch AgNO3 0.1N. m : Kho i lng mau e chuan o, gHam lng chat hoat o be mat (X) tnh bang % theo cong thc

    X = X1 (X2 + X3)

    Trong o :X1 Ham lng chat tan trong ru,%X2 Ham lng Natricacbonat tan trong ru,%X3 Ham lng Natriclorua tan trong ru

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    CHNG 3: PHAN TCH GIAY

    BAI 1: XAC NH pH NC CHIET CUAGIAY VA BOT GIAY

    I. PHAM VI NG DUNG:

    Tieu chuan nay quy nh phng phap xac nh pH nc chiet cua giay va botgiay. Gia tr pH khong phai la so o tong lng acid hoac kiem co trong vat lieu c

    chiet.Phng phap nay c ap dung cho tat ca cac loai giay va bot giay vi nc chietco o dan ln hn 0.2 ms/m khi xac nh theo ISO 6587, tr cac loai giay s dung lamgiay cach ien.

    II. NGUYEN TAC:

    Chiet 2g mau th trong mot t bang 100ml nc cat lanh hoac nong. o pH cuanc chiet nhiet o t 20oC en 25oC.

    III. HOA CHAT - DUNG CU:

    1. Hoa cha t:

    Nc cat hoac nc loai Ion: Trong phep cat ch s dung nc cat hoac nc loaiIon. o dan cua nc khong c ln hn 0.1ms/m sau khi c un soi hoac lam lanh.

    Chu thch: Thong thng nc s dung ca hai qua trnh cat va loai ion. Neu khongcan than khi cat nc, vi vat lieu lam phan ngng tu va cac be mat ma sau o hi ncngng tu tiep xuc, nc cat co the khong at en mc o dan oi hoi. Neu ch loai ionma khong cat. Co the co tac ong em do s co mat cua cacacid hu c, tr khi qua trnh loai ion co s dung chat co s trao oi ion manh. Khikhong co nc co o sach nh quy nh, co the s dung nc co o dan cao, nhng odan cua nc s dung phai c ghi vao bao cao th nghiem.

    Dung dch em tieu chuan : Dung dch em tieu chuan co gia tr pH la 4,0; 6,9 va9,2. Dung dch em co san dang thng pham hoac c ieu che nh sau:- Dung dch pH = 4,0: Kali hydrophtalat (dungdch 0.05mol/l): Hoa tan 10.21g

    Kalihydrophtalat (KHC8H4O4) trong nc cat trong bnh nh mc 1 lt va phaloang ti vach, pH cua dung dch tai nhiet o 20oC la 4,00 va tai 25oC la 4,01.

    - Dung dch pH = 6,9: Kalidihydroorthophosphate va Dinatrihydro orthophosphate:Hoa tan 3,39g Kalidihydro orthophosphate (KH2PO4) va 3.54g Dinatrihydroorthophosphate (Na2HPO4) trong nc cat trong bnh nh mc 1 lit va pha loangti vach, pH cua dung dch tai nhiet o 20oC la 6.87 va tai nhiet o 25oC la 6.86.

    - Dung dch pH = 9,2: Dinatri tetraborat (dung dch nong o 0.01 mol/l): Hoa tan

    3.80g Dinatri tetraborat decahydrat (Na2B4O7.10H2O) bang nc cat trong bnh

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    nh mc 1 lit va bo xung nc ti vach, pH cua dung dch tai 20 oC la 9.23 va tai25oC la 9.18.

    2. Dung cu:

    - Bnh thuy tinh co noi, nut mai, coc va ong sinh han, tat ca cac dung cu thuy tinhphai c ra can than bang nc cat nong va phai say kho trc khi s dung.

    - Bep ien- May o pH- Nhiet ke

    IV. CACH TIEN HANH:

    1. Chuan b mau:

    S dung gang tay cao su khi chuan b mau. Cat hoac xe mau thanh cac manh nho

    co kch thc sap x 5mm x 5mm. Tron eu cac manh mau, e mau trong bnh sach conap.

    2. Cach tien hanh:a. Chuan b nc chiet:- Can mau:

    Can 2g mau chnh xac ti 0.1g (khoi lng kho tuyet oi), vao bnh co kch c phuhp va tien hanh theo quy nh trong phan chuan b mau.- Chie t nong:

    Dung pipet lay 100ml nc cho vao bnh tng t kch c bnh co cha mau. Lapong sinh han vao bnh va un ti soi. Bo ong sinh han ra va o tat ca nc nong trong

    bnh vao bnh co cha mau, lap ong sinh han va un trong 1 gi.Lam nguoi nhanh en nhiet o 20oC 25oC (van e ong sinh han). e x si lang

    va chat nc chiet vao coc nho tien hanh chiet hai mau.- Chie t lanh:

    Dung pipet lay 100ml nc cho vao trong bnh cha mau. ong bnh bang nut thuytinh va e 1 gi tai nhiet o 20oC en 25oC. Trong thi gian o lac mau t nhat 1 lan.Chat nc chiet vao coc nhob. Xac nh pH:

    Hieu chuan may o pH bang hai dung dch em tieu chuan co gia tr pH sao chopH cua nc chiet nam trong khoang pH cua hai dung dch em. Sau khi hieu chuan ra

    sach ien cc mot vai lan bang nc cat va lan cuoi bang mot lng nho nc chiet.Kiem tra e nhiet o cua nc chiet trong khoang 20oC en 25oC. Nhung ien cc vaonc chiet va o gia tr pH.

    Lap lai phep o vi mau nc chiet th hai.

    V. KET QUA:

    Tnh gia tr trung bnh cua hai lan o gia tr pH lay chnh xac ti 0.1 n v. Cacket qua o khong c sai khac nhau qua 0.2. Neu khong at, lap lai phep o tren haimau nc chiet. Bao cao gia tr trung bnh va dai o cua tat ca cac lan o?

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    BAI 2: XAC NH TINH BOT TRONG GIAY

    I. PHAM VI NG DUNG:

    Tieu chuan nay quy nh phng phap xac nh tnh va nh lng tinh bot khongbien tnh, tinh bot bien tnh bang ky thuat oxi hoa thong thng hoac s dung enzym,c cho vao trong qua trnh nghien bot giay hoac e gia keo be mat.

    Phng phap nay xac nh tong ham lng tinh bot co trong giay, khong phan biettinh bot trong hoac tren be mat giay.

    Mot so loai tinh bot: cationic, c the, c ghep hoac lien ket vi keo khong

    tien hanh theo phng phap nay, bi v cac loai tinh bot o co cac yeu cau ky thuat acbiet. Phng phap nay ch ap dung cho tinh bot co the chiet c va tao phc chat viIod.

    II. HOA CHAT - DUNG CU:

    1. Hoa chat:

    - HCl am ac- Cac dung dch co t le HCl va nc la 1:1, 1:9 va 1:19- Thuoc th KI - I2 : Hoa tan 7.5g KI va 5g I2 trong 10ml nc cat khuay cho tan het

    I2

    sau o nh mc thanh 1 lit.- X bong vun- Dung dch natri thiosunphat: hoa tan 2g en 3g natri thiosunphat (Na2S2O3. 5H2O )

    trong 100ml nc cat- Dung dch Iot: Nong o khoang 0.01 N I2 pha dung dch goc nong o 0.01N bang

    cach hoa tan 0.13g I2 va 2.6 g KI trong 5ml nc sau o pha loang ti 100ml. Phaloang mot phan dung dch goc o trong chn phan nc ti mau vang nhat e cdung dch th nghiem, pha loang dung dch goc trc moi lan th nghiem.

    2. Dung cu:

    - May anh ti: e anh ti cac manh mau trong nc. May co toc o khuay troncao la thch hp nhat, nhng co the s dung cac dung cu khac nh cac hat thuy tinhlac trong bnh cung vi mau.

    - May ly tam thch hp nhat la co dung lng ln hn 50ml.- May o mau quang pho: o o hap thu tai bc song 580nm.- Co c loc thuy tinh hoac pheu loc: co o loc tho, dung tch khoang 50ml hoac ln

    hn. Hoac pheu loc Buchner va giay loc whatman so 40, giay loc acid tngng, giay loc si huy tinh whatman 934 AH.

    - Dung cu thuy tinh va cac dung cu khac: coc 50ml, 150ml; ong ong 100ml; pheuloc nho, giay loc.

    - Bnh loc: dung tch 500ml hoac ln hn.

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    - Cac dung cu khac: bnh nh mc 50ml, 100ml va 500ml; pipet 25ml va 2.5ml; coc250ml; noi cach thuy; ong ho bao giay.

    III. CACH TIEN HANH:

    1. Phng phap nh tnh:

    a. Chuan b mau:Can khoang 0.5g mau th va xe thanh cac manh nho co kch thc t 5mm en

    10mm.b. Cach tien hanh:

    un cac manh mau mot vai phut trong 10ml nc cat, loc, e nguoi nc loc vanho 1 giot dung dch I2 loang. Neu nc co mau xanh la co tinh bot. Mau tm nhatkhong c coi la co tinh bot, v trong mot so trng hp giay khong co tinh bot van chophan ng nay.

    2. Phng phap nh lng:

    a. Chuan b mau th:Can 1g chnh xac ti 5mg mau th a c xe thanh cac manh nho co kch thc

    t 5mm en 10mm.Chu thch: khong c nghien giay trang thai kho v co the lam mat mot phan

    tinh bot, ac biet la vi mau co cha chat on.b. Cach tien hanh:

    anh ti mau th trong 60ml 20ml nc cat nong (nhiet o t 40oC en 80oC) ,sau o chuyen mau vao coc 250ml va dung nc cat nong e trang ra sao cho lng

    nc cat trong coc la 100ml. un trong noi cach thuy vi nhiet o trong coc la 92o

    Ctrong 15 phut.Chu thch: neu mau th khong u e tao thanh mieng. Th bo xung mot lng bong

    vun vi khoi lng nho hn 1g.Loc mau tren coc loc (co s dung hut) ra phan con lai bang 10-12ml nc cat

    nong. Lam nguoi ti nhiet o phong trong be nc a. Bo xung 25ml HCl (1:1) vao cocloc va e trong 3 phut (nen dung ua thuy tinh e phan tan phan con lai tren coc loc) vas dung hut. Lap lai bc chiet xuat bang 25ml HCl trong 3 phut. Loc hut dung dch. Boxung 25ml HCl am ac, khuay tron phan con lai tren coc loc trong 40 giay. Lam ngngngay phan ng bang cach bo xung khoang 50ml nc cat ( nhiet o phong vao coc loc.

    Hut dung dch va lac bnh loc e tron eu HCl am ac trong dch lo c, ra phan con laitren coc loc t 3 en 4 lan vi mot lng nho nc cat (khoang 25ml) sao cho tonglng dch loc khong qua 450ml kiem tra xem tinh bot a c loai het ra khoi maubang cach nho 1 hoac hai giot dung dch iot loang vao phan con lai tren coc loc, neu convet tinh bot th se co mau xanh. Neu tinh bot van con lai trong mau th chuyen phan conlai tren coc loc vao coc 250ml. Bo sung100ml 150ml nc va lap lai nh tren tai bcung nong. Neu tinh bot van con sau hai lan chiet xuat th bo mau o va tien hanh lamlai hoan toan.

    Chu thch: thi gian chiet xuat HCl phai c kiem tra chat che e tranh tinh botb thuy phan.

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    Chuyen dung dch tinh bot vao bnh nh mc 500ml, lam nguoi en nhiet ophong va bo xung nc cat ti vach. Lac eu dung dch, neu dung dnh b uc do chaton hoac do chat chiet xuat th dung may li tam trong 10 phut. oi khi e dung dch

    lang qua em co the cho ket qua tng ng tuy nhien, s thuy phan co the xay ra khie thi gian dai.Chu thch: neu can thiet phai chiet xuat lan hai. Hon hp tat ca cac dch loc va

    bnh nh mc 1000ml, lam nguoi ti nhiet o phong va bo xung nc ti vach.Dung pipet lay 25ml dung dch trong cho vao bnh nh mc 50ml. Dung pipet cho

    2.5ml dung dch KI - I2 vao trong bnh, sau o bo sung nc ti vach va lac eu.Chuan b mau th nghiem trang bang cach hon hp 25ml HCl (1:9) vi 2.5ml dung dchKI- I2 trong bnh nh mc 50ml va bo sung nc ti vach, lac tron eu, o he so hap thucua mau th nghiem trang va mau th nghiem trong te bao quang ien 1cm tai 580nm.Neu chum tia quy chieu c s dung trong thiet b, th dung nc trong chum tia quy

    chieu, mau trang chay tren moi mau th nghiem c chuan b bang cach cho mot giotNatri thiosunphat vao te bao quang ien cha mau th nghiem. Lac va o lai he so hapthu.c. Lap o th chuan:

    Neu co the, s dung cung mot loai tinh bot c cho vao trong giay e lap o thchuan. Neu khong the th s dung hon hp cua ba en bon dang tinh bot thong thngcan 0.1g tinh bot (a c tr o am va o tro) cho vao trong coc 250ml, bo sung 100mlnc cat va un 15 phut sau khi nhiet o trong coc at 92 0C. Bo sung 1.0g bong vun vaun 15 phut hoac lau hn. Loc co hut qua coc loc thuy tinh tho, dung nc nong e racoc va loc lai nc loc qua tam em e nguoi ti nhiet o thng trong be nc a.

    S dung HCl va chiet xuat theo ung nh tien hanh vi mau th nghiem. Pha loangdung dch loc ti 500ml trong bnh nh mc. Lay mot phan dung dch cho va o may lytam trong 10 phut va lay dung dch e chuan b lap ng o th. o he so hap thu nhoi vi mau th nghiem tai tat ca cac nong o cac nong o pha loang c ch ra trongbang sau:

    Nong o tinh bot(g/l)

    Tong the tch(ml)

    Dd tinh bot(0.2g/l, ml)

    Nc cat(ml)

    Dung dch KI(ml)

    0.010 100 5 0 5

    0.020 100 10 5 50.030 100 15 10 5

    0.040 100 20 15 5

    0.050 100 25 20 5

    Dung HCl 1:19 e pha loang ti vach trong bnh nh mc, dung ong ong e laync, dung pipet hoac buret e lay dung dch.

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    Tnh nong o thc cua tinh bot t moi dung dch chuan. Lap o th cua he so hapthu thc theo nong o tinh bot thc, ng o th o la ng tuyen tnh i qua goc toao. Xac nh kha nang hap thu a t o doc cua ng thang.

    A = a.b.cTrong o :

    A: la he so hap thu thc nh phan trena: la kha nang hap thu cua tinh botb: la o dai cua te bao quang ienc: la nong o tinh bot thc tnh bang g/la, b: la o doc cua ng thang

    Tnh a va gia tr trung bnh cua ket qua, hoac lap o th va lay gia tr a t o th.Tnh gia tr trung bnh cua hai lan xac nh chnh xac ti 0.1%.

    IV. KET QUA:Ham lng tinh bot c tnh bang phan tram theo cong thc sau :

    SV

    VV

    ab

    Ax

    A

    f

    10

    10

    Trong o :- A : la he so hap thu thc = Amau th nghiem A mau th nhiem trang Amau trang- a : la kha nang hap thu tinh bot xac nh c t ng o th, tnh bang

    (lit/g-cm)- b : la o dai cua te bao quang ien tnh bang (cm)- V

    o: la the tch cua dung dch tinh bot sau khi chiet xuat tnh bang (ml)

    - Vf: la the tch cua dung dch tinh bot c lay e o mau, tnh bang (ml)- VA : la the tch cua dung dch lay t Vo thng la 25ml, tnh bang (ml)- S : la khoi lng mau th kho tuyet oi, tnh bang (g).

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    BAI 3: XAC NH O TRO TRONGGIAY VA BOT GIAY

    I. PHAM VI NG DUNG:

    Tieu chuan nay quy nh phng phap xac nh o tro cua tat ca cac loai giay vabot giay. Gii han di cua phep xac nh la khoang 0.2%.

    II. NGUYEN TAC:

    Mau th c cho vao coc nung va nung tai nhiet o 900 oC 25oC trong lo nung.Khoi lng tro c xac nh bang cach can coc can va mau th sau khi nung.

    III. DUNG CU - THIET B:

    - Coc nung: c lam bang platin, s hoac thach anh, co the tch u e cha c10g mau th (thng coc nung co the tch 50ml la phu hp) coc nung khong cgiam hoac tang khoi lng khi nung va khong co phan ng hoa hoc vi mau thhoac phan con lai cua mau th sau khi nung.

    - Lo nung: Co kha nang duy tr c nhiet o 900oC 25oC lo nung nen at vao nico thiet b hut khoi.

    - Can phan tch: Co o chnh xac ti 0.1mg.

    IV. CACH TIEN HANH:

    1. Chuan b mau:

    Mau th c xe thanh cac manh nho co kch thc khong ln hn 1cm2 va ce can bang o am trong tui nilon hoac bnh co nap.

    Neu mau th t phai e kho gio ni khong c co bui trong phong th nghiem.

    2. Cach tien hanh:

    Tien hanh xac nh hai mau song song, tat ca cac lan can chnh xac ti 0.1mg.Can mau th e xac nh o kho, o am va o tro cung mot thi iem.Can khoi lng mau th nho nhat la 1g hoac u e sau khi nung khoi lng con lai

    la 10mg.Vi mau th co o tro thap (th du nh giay khong tro), can mau th u e cac

    phan con lai sau khi nung la 2mg.Coc nung c ra sach, anh so va nung trong lo nhiet o 900oC 25oC va thi

    gian t 30 phut en 60 phut. La nguoi ti nhiet o phong trong bnh hut am (thng thigian e trong bnh hut am oi vi coc nung lam bang platin la15 phut va oi vi cocnung lam bang s hoac thach anh la 45 phut) va tien hanh can coc nung.

    Chuyen mau th vao coc nung ot t t e mau th khong chay thanh ngon la.Khong c e mat mau do b bay.

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    Vi mau th co o tro thap, v khoi lng mau th ln nen co the ot lien tiep tngphan mau th cho ti het.

    Chu thch 1: Bc ot mau th phu thuoc vao dang lo nung s dung. Mot so lo

    nung co dang ca khi m se tao thanh mot buc nam ngang trc ca lo . Buc o hoacmot bo phan tng t co the s dung khi ot chat hu c trong mau th. Khi mau th achay het hoac gan het co ngha la cac cham en con lai nhn thay rat t, th at coc nungvao nhiet o 900oC 25oC trong lo nung vi thi gian la 1 gi.

    Chu thch 2: Khong keo dai thi gian nung va nung ti khoi lng khong oi. Motso thanh phan co the b mat khi thi gian nung qua dai. Lay coc nung ra khoi lo nung,cho vao bnh hut am e lam nguoi ti nhiet phong va tien hanh can.

    V. KET QUA:

    o tro (X) c tnh bang phan tram theo cong thc sau:

    100maX

    Trong o:- X: la o tro, tnh bang phan tram- a: la phan tro con lai sau khi nung en kho kiet, tnh bang gam- m: la khoi lng mau th sau khi nung en kho kiet, tnh bang gam

    Chu thch: gia tr o tro cua hai mau xac nh song song khong c khac gia trtrung bnh qua 5%. Tnh gia tr o tro cua hai mau xac nh song song vatnh gia trtrung bnh, lay chnh xac ti 0.1%.

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    CHNG 4: PHAN TCH DAU KH

    BAI 1: O AN MON TAM ONG ASTM D 130(COPPER STRIP CORROSION)

    I. PHAM VI NG DUNG:

    Ap dung cho xang oto, xang may bay, nhien lieu phan lc, diezel, dau hoa, daunhn, cac phan oan chng cat va cac san pham dau mo khac co ap suat hi bao hoa

    khong qua 18 psi.Lu y: Xang t nhien co the co ap suat hi cao hn, do o bom th cha xang tnhien khong c at 1000C. Cac mau co ap suat hi Reid cao hn 18 psi (124 kPa) cothe co ap suat u e gay be bom khi 1000C. Vi cac mau co ap suat hi tren 18psi, sdung phng phap th D1838.

    II. MUC CH VA Y NGHA:

    Xac nh tnh chat an mon cua mieng ong ieu kien th cho trc e anh giamc o an mon kim loai cua san pham dau.

    III. TOM TAT PHNG PHAP:

    Tam ong a c anh bong va lam sach theo tieu chuan, ngam trong mau canth nhiet o va thi gian ac trng cho mau th. Sau o lay ra lau sach va so sanh vibang mau chuan theo ASTM.

    IV. THIET B HOA CHAT:

    - Be on nh nhiet- Ong th- Nhiet ke- Ong quan sat

    - Glyxerin- Giay nham- Tam ong

    Be on nhiet: co kha nang on nhiet va duy tr khoang thi gian th nghiem, sailech 4010C, 5010C va 10010C. Co gia phu hp e gi lay ong th hay bom th vtr thang ng va dm o sau 100mm. Be nc, dau hay khoi nhom eu phu hp.

    Ong th 25150mm.Bom ng ong th lam bang thep khong g co kha nang chu c 100 psi.Nhiet ke, loai nhung chm hoan toan, co thang chia nho nhat la 0,10C.Gia e anh bong tam ong.Ong quan sat, ong th thuy tinh phang, e bao ve mieng ong b an mon khi kiem

    tra va bao quan.

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    Dung dch ra: s dung mot loai Hydrocacbon khong co Lu huynh de bay hi,khong an mon ong khi th 50 C0 . Iso octan loai th ch so octan la phu hp va phais dung trong trng hp tranh chap.

    Giay hoac vai nham anh bong co kch thc hat 65 micromet (240-grit). Con sdung hat nham silicon carbide 105 m(150-mesh).Tam ong: S dung tam ong rong 12,5 mm, day 1,5 3.0 mm, dai 75mm, co o

    tinh khiet 99,9%. Tam ong co be mat b bien dang can loai bo.Chuan b be mat tam ong: Dung giay nham co c hat thch hp e loai bo cac vet

    ban khoi 6 mat tam ong. Ket thuc bang giay nham 65 m e loai bo cac vet xc cuagiay nham loai s dung trc o. Dm tam ong vao dung moi ra t o co the lay rangay e anh bong lan cuoi hay bao quan cho s dung lan sau.

    Chuan b lan cuoi (anh bong): Lay tam ong ra khoi dung moi ra. Gi tam ongtren ngon tay vi giay loc khong tro. au tien anh bong g sau o cac canh vi hat

    nham silicon carbide 105 m lay t mot tam thuy tinh sach bang bong co tham dungmoi. Lau bang mot mieng bong hut nc mi va sau o ch kep tam ong bang kep thepkhong g, khong dung tay. Kep tam ong vao gia va anh bong cac mat chnh bang hatnham silicon carbide tren bong hut nc, khong anh bong theo vong tron, ma cha theotruc dai cua tam ong t au en cuoi. Lau sach cac bui kim loai bang bong. Khi tamong a sach, dm ngay vao mau a chuan b.(S dung anh bong cuoi cung vi kch c hat ln hn e tao o gho ghe kiem tra trenbe mat cua tam ong la v tr bat au phan ng an mon).

    V. BANG AN MON CHUAN:

    Bang an mon chuan la s tai hien lai mau cua cac tam th ac trng ai dien chomc o an mon tang dan va c boc plastic. Bang chuan nay phai c bao ve khoianh sang e tranh phai mau. Kiem tra o phai mau bang cach so sanh vi bang chuanc bao ve ky (mi). Quan sat di anh sang ban ngay, ban au chieu thang va sau ochieu nghieng 450. Neu nhan thay co phai mau nhat la pha ben trai cua bang, can phailoai bo.

    Neu be mat cua lp vo plastic b xc, can thay the bang chuan.

    VI. LAY MAU:

    Mau can c ng trong chai thuy tinh sach, toi mau, chai plastic, hay cac bnhng phu hp khac ma khong anh hng en tnh chat an mon cua mau. Tranh s dung

    cac bnh co phu thiec.Nap bnh cang ay cang tot va ay nap lai ngay sau khi lay mau. Khi lay mau

    tranh anh sang mat tri trc tiep hay ngay ca anh sang khuyech tan ban ngay. Sau khinhan mau tien hanh th cang nhanh cang tot va ngay sau khi m bnh.

    Neu mau co nc hoac nhu tng phai loc mau qua fliter loc nhanh trc khi chovao ong th. Thc hien thao tac nay trong phong toi.

    VII. CACH TIEN HANH:

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    Thi gian va nhiet o th quy nh nh sau la thng s dung nhat va c a ratrong cac ac tnh k thuat ASTM cua cac san pham nay (ieu kien khac co the s dungkhi co yeu cau cua ac tnh ky thuat hay co s thoa thuan cua cac ben tham gia).

    oi vi xang may bay - Jet A1 - Lay 30ml mau sang, khong co nc vao ong thkho, sach, trong 1 phut sau khi hoan tat anh bong, tha tam ong vao ong mau. at ongmau vao bom va ong nap. Ngam trong be on nhiet 10010C trong 2h 5. Sau o laybom ra ngam vai phut trong nc may. M bom, lay ong th ra kiem tra tam ong nhhng dan.

    oi vi dau hoa: 1000C trong 3h 5.oi vi dau nhn: Th nghiem co the thc hien cac thi gian khac nhau va

    nhiet o nang cao hn 1000C.Kiem tra tam ong:

    Cuoi qua trnh th lay bom ra va lam lanh nhanh en nhiet o phong. Dung kep

    lay tam ong ra, nhung vao dung dch ra. Lay tam ong ra ngay, lam kho bang giay locva so sanh vi bang mau chuan.Chu y: Gi tam ong va bang mau chuan sao cho co the quan sat anh sang phan

    chieu t chung di goc 450 e de so sanh va anh gia.Khi kiem tra so sanh, co the tranh c vet xc neu at tam ong vao tam thuy

    tinh phang c nut bang bong hut nc.

    VIII. GIAI THCH:

    Mau tam ong gia hai mau cua bang chuan th anh gia theo so mau am hn.Mau tam ong da cam am hn 1b th coi tam ong van thuoc loai 1 tuy nhien, neu thayco mau o khi quan sat th coi tam ong thuoc loai 2.

    Tam ong co mau o Boco (loai 2) co the nham vi tam ong o ta tren nenong thau (loai 3). e phan biet nhung tam ong vao dung moi ra:

    - Neu ta m ong co mau da cam sam, th anh so 2- Neu ta m ong khong oi mau th anh so 3

    Phan biet tam ong co nhieu mau (loai 2 va 3): at tam dong vao ong th gia nhiet ennhiet o 315 -3700C tren bep ien phang trong 4-6 phut. ieu chnh nhiet o bang cachat nhiet ke vao ong th 2:

    - Neu ta m ong oi mau sang anh bac, roi sang vang: anh gia so 2- Neu ta m ong oi thanh mau en th anh gia so 3

    Lap lai th nghiem neu co dau tay, vet xc hay vet giot nc tren tam ong hoac mau canh am hn tren be mat.

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    IX. KET QUA:

    Bao cao theo o mau c anh gia ghi nhiet o, thi gian th.X. O CHNH XAC: Khong qui nh.

    Bang 1: Phan loai tam ong

    Loai Ten Mo ta

    1 Xn nhea. Da cam sang, gan vi tam ong mi anh

    bongb. Da cam am

    2 Xn trung bnh

    a. o Bocob. Mau o tic. Nhieu mau: xanh dng, o ti hay bac

    hay ca hai tren nen o Bocod. Mau bace. Mau ong thau hay vang

    3 Xn sama. Mau o ta tren nen ong thaub. Nhieu mau: o va xanh la cay (long

    cong). nhng khong sang

    4 An mon

    a. en o, sam am hay nau vi mau xanh lalong cong.

    b. Mau ch hay en xn.c. en bong hay en hat huyen.

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    BAI 2: XAC NH IEM NHO GIOT CUA M NHNASTM D 566

    I. PHAM VI AP DUNG:

    Phng phap nay dung e xac nh o nho giot cua m nhn. Phng phap khongdung cho nhiet o > 288 C0 . Vi nhiet o cao hn s dung phng phap D2265.

    II. MUC CH VA Y NGHA:

    Thong thng, nhiet o nho giot la nhiet o ma tai o m chuyen t trang thai banran sang long di ieu kien th. S thay oi trang thai nay la ien hnh cho m co chaxa phong lam ac loai thng. M cha cac chat lam ac khac xa phong thong thngse tach dau ma khong lam thay oi trang thai. Phng phap nay co ch giup cho viecnh danh m ve chung loai va e thiet lap duy tr dau hieu kiem tra chat lng. Ket quach c coi nh co y ngha gii han ve kha canh tnh nang v ay la th nghiem tnh.

    III. TOM TAT PHNG PHAP:

    Mau m cha trong coc nho treo trong ong th c gia nhiet trong be dau vi toco nh trc. Nhiet o ma tai o ma mau ri t lo ay coc c lay trung bnh vinhiet o cua be dau va c ghi nhan la iem nho giot cua m.

    IV. THIET B HOA CHAT:

    - Nhiet ke -5 3000C chia 10/ vach- Ong ong- Chen ng mau bang ong ma Crom- Chat tai nhiet- Que khuay- Ong nghiem chu nhiet dai 180 200 mm- Coc thuy tinh 500 ml- Manh giay loc

    - Bep ien

    - M

    Coc m - Coc bang ong thau ma Crom.Ong th - Bang thuy tinh chu nhiet, co mieng, chieu dai 100 103mm, ng

    knh trong 11,1 - 12,7 mm, co 3 cho lom vao trong eu theo chu vi cach ay 19mm egi coc.

    Nhiet ke - Khoang nhiet o -5 C0 en 300 C0 (20C).Dung cu phu tr - Be dau co khuay gom co coc 400 ml, gia vong va vong cua

    be dau, kep nhiet ke, 2 nut lie, day kim loai ng knh 1,2 1,6mm, dai 152mm, cainh c nut coc va cai nh c o sau nhiet ke.

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    1. Nhiet ke -5 3000

    C chia 10

    / vach2. Ong ong3. Chen ng mau bang ong ma Crom4. Chat tai nhiet5. Que khuay6. Ong nghiem chu nhiet dai 180 200 mm7. Coc thuy tinh 500 ml8. Manh giay loc9. Bep

    V. CHUAN B THIET B:

    Lam sach coc va ong th bang dung moi spirit.Ch s dung coc sach. Khi mat trong cua coc co dau hieu b mon, bo i.Khi dung coc mi, kiem tra kch thc bang cai nh c nap coc. Kiem tra ay

    bang que 2,72 mm de dang xuyen qua, con que 2,82 mm th khong. Neu lo nho thkhoan rong ra, con ln qua th bo i.

    Kiem tra ong th, bau nhiet ke va o sach. Kiem tra dan hng vong lie, nut tren.Dung sai tong gia dan hng vong lie va thanh trong cua ong th la 1,5mm.

    VI. CACH TIEN HANH:Nhoi ay m vao coc bang cach an mieng rong vao m. Bo m d bang dao. An

    nhe coc, gi thang ng vi mieng nho xuong di. Xuyen que kim loai t di len trenen khi no nho len 25mm. An que vao coc sao cho que kim loai tiep xuc vi ng chuvi thap va cao cua coc. Gi tiep xuc nay, xoay coc tren que theo ngon tro e tao chuyenong xoan xuong pha di que e loai phan m hnh chp dnh doc theo que. Khi cocat en iem cuoi que, rut can than que ra khoi coc sao cho mang phang khong co botkh, co o day mong muon con gi lai trong coc.

    at nut lie vao nhiet ke. Nh cai nh c o sau nhiet ke at trong ong th, chnhlai v tr nut lie tren cua nhiet ke sao cho ay bau nhiet keva kht vao cai nh c o

    sau.Thay cai nh c bang coc m sao cho nhiet ke a vao nam o sau a nh. Khi

    o bau nhiet kekhong cham vao mau m cung nh coc.Treo ong th vao be dau en o sau sao cho mieng ong nam tren mc dau t nhat

    la 6mm.Treo nhiet ke th 2 vao be dau sao cho bau nhiet ke nam v tr xap x cung v tr

    bau nhiet ke ong th.Khuay be dau, gia nhiet vi toc o 4 7 C0 /phut en khi at nhiet o khoang

    17 C0 di iem nho giot d kien. Khi o giam toc o gia nhiet xuong 1 1,50C/phut. Skhac nhau gia be dau va ong th la 1 2 C0 . Khi nhiiet o tang, m se eu an nho ra

    Hnh 1. Dung cu xac nh nhiet o

    nho giot cua m boi trn

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    khoi lo coc. Khi giot m rt xuong, ghi nhiet o cua 2 nhiet ke va lay gia tr trung bnhchnh xac en 1 C0 lam iem nho giot.

    Hai xac nh co the thc hien ong thi trong cung mot be, mien la hai mau co

    xap x cung nhiet o nho giot.VII. KET QUA:

    Bao cao nhiet o nho giot chnh xac en 1 C0

    VIII. O CHNH XAC:

    - o lap lai 7 C0

    - o tai lap 13 C0

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    BAI 3: XAC NH NHIET O CHP CHAY COC KNASTM D 56

    I. PHAM VI AP DUNG:

    Phng phap xac nh iem bat chay coc kn cua san pham dau mo bang thiet bcoc kn Pensky-Martens, ap dung cho khoang nhiet o 40 3600C.

    Quy trnh A ap dung cho nhien lieu chng cat (diesel, dau hoa, dau gia nhiet,nhien lieu turbin), dau nhn mi va cac chat long dau mo ong nhat.

    Quy trnh B ap dung cho nhien lieu ot lo can, can, dau nhn a s dung, hon hpdau long va ran, cac chat long co khuynh hng tao mang be mat hoac khong ong nhat ieu kien th nh quy trnh A.

    Phng phap nay dung e phat hien cac chat de bay hi va de chay nhiem trongcac chat tng oi khong bay hi va khong chay.

    II. MUC CH VA Y NGHA:

    Tieu chuan nay quy nh phng phap xac nh iem chp chay coc kn cua sanpham dau mo e ap dung vao van e bao quan, van chuyen bao am an toan.

    III. TOM TAT PHNG PHAP:

    Mau trong coc th c gia nhiet va khuay eu toc o quy nh. Khi a ngonla tieu chuan trc tiep vao be mat cac mau cac khoang thi gian eu an va ongthi ngng khuay. Nhiet o bat chay la nhiet o thap nhat tai nhiet o o hi cua mautren be mat coc th bat chay khi co moi la tieu chuan c a vao.

    IV. THIET B HOA CHAT:

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    - Bep gia nhiet- Coc mau- Bo phan khuay- Nguon la

    - Dau D.O- Kerosel- aceton

    V. CACH TIEN HANH:

    1. Chuan b mau:Can t nhat 75 ml mau cho moi lan th. Khi lay mau dau can, bnh cha pha i cha

    t 85-95% mau. oi vi cac loai mau khac 50-85% mau.Mau th tiep theo phai lay t cung mot bnh cha mau, mau th 2 phai lay t bnh

    cha khong t hn 50% mau. Khong m bnh cha mau khi khong can thiet e tranh matphan nhe hay hap thu hi nc. Bao quan mau nhiet o khong qua 35 0C. Bnh cha

    mau phai co nap trong. Vi mau long lam lanh mau va rot mau nhiet o thap hnnhiet o chp chay d kien 180C.Khong cha mau trong bnh tham thau kh.Mau qua nht c gia nhiet trong bnh cha u e chay long, trong 30 phut

    nhiet o thap nhat khong vt qua 280C di iem chp chay d kien. Neu mau vancha chay long co the gia nhiet them 30 phut na. Sau o lac nhe e tron eu, quay bnhtheo phng nam ngang, trc khi chuyen vao coc th.

    Mau cha nc hoa tan hay t do can c tach nc bang CaCl2 hay bang cachloc qua giay loc.2. Chuan b thiet b:

    at thiet b tren ban vng chac tranh ni gio lua, khong s dung trong tu hut ang lamviec.Lam sach va kho coc th va cac bo phan phu tr trc khi th.3. Cach tien hanh:

    Can than lam sach coc loai bo het cac vet ban cua lan th trc,say kho coc, rotmau can th en vach mc,ay nap va at coc vao may.

    Khuay tron nhe nhang nh day khuay. Khuay eu mau vi toc o 90-120 vong/phut.

    Tang nhiet o cua coc t t.Vi loai san pham dau mo co iem chp chay d kien t 50 1500C th toc o gia

    nhiet tang khoang 5-80

    C/phut.Vi loai san pham dau mo co iem chp chay d kien ln hn 1500C th toc o gianhiet tang khoang 10-120C/phut.

    Khi cach iem chp chay d kien khoang 30 0C th giam toc o tang nhiet o con20C/phut. Khi cach iem chp chay khoang 100C th bat au th iem chp chay. Chamla moi va ieu chnh ngon la moi thch hp (co ng knh 3.2 - 4.8 mm). Ngngkhuay va cho ngon la moi vao be mat mau th bang c cau tren nap, kiem tra tam chansao cho nguon la ha xuong vung hi cua coc th trong vong 0.5s, lu lai v tr thaptrong 1s va nhanh chong tr ve v tr cu. Neu nhiet o bat chay cua mau th thap hn150 0C th c tang 10C th mot lan.

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    Neu nhiet o bat chay cua mau th cao hn 1500C th c tang 20C th mot lan.Th cho en khi hi cua mau bat chay thc s trong coc, khi xuat hien ngon la

    mau xanh th tat ngay, nhiet o o la iem chp chay co kn va ghi lai nhiet o nay.(Moi la co the gay ra quang xanh va ngon la rong trc iem chp chay thc,can bo qua).

    Tiep tuc nang nhiet o len 1 20C na va lai th tiep tuc, neu khong thay xuathien ngon la th th nghiem xem nh sai, phai lam lai t au.

    oi vi mau cha biet iem chp chay th phai lam th nghiem tham do bang cachnang nhiet o 40C/phut va sau 40C lai th mot lan. Sau khi xac nh tham do c iemchp chay th tien hanh th nghiem nh tren

    VI. KET QUA:

    Neu iem chp chay ln hn 1040C, sai lech khong qua 5,50C. Neu iem chpchay nho hn 1040C, sai lech khong qua 20C.

    Lam tron so en 0,50C, theo cong thc hieu chnh sau :

    T= C + 0,25 (101,3-K)

    - T: La nhiet o bat chay sau khi a hieu chnh- C: la nhiet o bat chay cua mau quan sat c- K: la ap suat cua moi trng th kPa

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    V. CACH TIEN HANH:

    1. Chuan b mau:

    Bao quan mau trong chai kn, lam bang vat lieu khong tham thau kh (khong ngtrong chai nha), e nhiet o thap tranh lam bay hi cac phan nhe, tien hanh rot mau nhiet o thap hn nhiet o bat chay 56oC, khong m nap khi khong can thiet e tranhmat phan nhe va a hi nc vao. Khi co the phai xac nh iem chp chay trc tienva bao quan mau nhiet o thap.

    Mau ran hoac nht th ham nong mau en nhiet o u e chay long, nhngkhong bao gi gia nhiet en tren nhiet o ma nhiet o nay thap hn nhiet o bat chay doan la 56oC trc khi cho vao coc. Neu mau c gia nhiet tren nhiet o nay, can lamnguoi en 56oC di iem chp chay d oan trc khi th.

    Neu mau cha nhieu nc co the lam kho bang Canxiclorua hoac loc qua giay

    loc nh tnh, neu mau qua nht, co the un nong mau (thap hn nhiet o bat chay doan 56oC).Chu y: Neu mau cha nhieu phan nhe khong un cung khong loc.

    2. Chuan b thiet b:

    Th nghiem c tien hanh ni kn gio. Khong tien hanh th trong tu hut anglam viec.

    Can than lam sach coc loai bo het cac vet dau ban cua lan th trc, neu co canCacbon loai bo bang bui nhui thep loai manh. Say kho coc, e nguoi coc en t nhatdi nhiet o chp chay d kien la 56oC.

    3. Tien hanh th :Rot mau can th en luc mat khum cua mau trung vi vach mc, neu cho mau qua

    nhieu th dung xylanh hut bt ra, khong e mau co bot hoac bot kh trong suot qua trnhth. Nhiet o cua coc va mau khong vt qua nhiet o ma nhiet o o di nhiet ochp chay d kien 56oC, at coc len bep.

    Nhiet ke gi v tr thang ng sao cho ay cua bau thuy ngan cach ay coc 6,40,1ml va iem nam gia ban knh vuong goc vi ng cong quet cua ngon la th.

    Cham ngon la va ieu chnh e no co ng knh t 4,2 - 4,8mm.Chu y: Can than khi s dung gas, khi lam mau co cha thanh phan co iem bat chaythap co the bung chay manh, hoac nhng mau co iem bat chay en 400 oC

    Cap nhiet vi toc o tang nhiet o cua mau khoang 14 17oC/phut.Khi nhiet o cua mau th thap hn iem chp chay d oan 500C th giam toc o

    tang nhiet o xuong con 5 6oC/phut cho en khi cach nhiet o d oan 28 0C. Khinhiet o at 28oC di iem chp chay d kien, cung cap moi la th, c tang 2oC th 1lan, cho moi la chay ngang qua iem gia be mat coc th, tiep tuc th ngon la en khixuat hien bat la. Thi gian ngon la i qua coc mau moi lan khoang 0,1s.

    Ghi lai nhiet o tren nhiet ke la nhiet o quan sat c khi xuat hien ngon la mauxanh au tien tren mot phan hay toan bo be mat mau.

    Khi mau th ma nhiet o chp la khong biet trc th mau th c rot vao cocth nhiet o nho hn 50oC, cung cap moi la th bat au nhiet o cao hn nhiet o

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    rot mau la 5oC, tiep tuc un nong mau th 5-6oC/phut va c tang 2oC th 1 lan cho enkhi thu c iem chp la a2Chu y:

    Cac chi tiet nh: Kch c moi la, toc o gia nhiet, toc o a moi la qua mau theu anh hng en ket qua. Moi la co the gay ra quang xanh va ngon la rong trciem chp chay thc, can bo qua.

    Khi thu c iem chp chay lan th au tien, ngng th, lap lai vi mau mi vath lan au tien nhiet o di nhiet o chp chay lan trc (co c lan th au tien)28oC.

    e xac nh iem bat chay tiep tuc un nong mau th sau khi ghi lai iem chpla, tang nhiet o mau th vi toc o 5-6oC/phut c 2oC th 1 lan cho en khi bat chaymau trong 5s, ghi lai nhiet o nay.

    Khi thiet b nguoi en di 60oC, lay ra va lam sach coc mau.

    VI. KET QUA:T = Tquan sat + 0,25(101,3 K)

    T = Tquan sat + 0,033(760 P)

    Trong o:T- la nhiet o bat chay cua mau sau khi hieu chnh)Tquan sat - la nhiet o bat chay cua mau quan sat cP- la ap suat kh quyen tai thi iem th,mmHgK- la ap suat kh quyen tai thi iem th,KPa

    VII. O CHNH XAC:S khac nhau gia cac ket qua cua 1 ngi th tren cung 1 thiet b va cung ieu

    kien th, cho phep 1/20 lan g