Atomic fluorescence tov configuration
Kev npaj ntawm atomic fluorescence standard tov yog ib tug dilution txheej txheem, thiab high-concentration standard tov yuav tsum tau diluted mus rau qhov yuav tsum tau concentration raws li qhov yuav tsum tau, thiab ua ib tug concentration sequence, thiab ntsuas atomic fluorescence tus nqi yog linearly txiav txim.
Yog li ntawd, kev npaj cov kev daws teeb meem yuav cuam tshuam ncaj qha rau qhov tseeb ntawm cov ntaub ntawv pov thawj. Txij li thaum ntsuas cov xwm txheej ntawm arsenic thiab antimony yog qhov zoo ib yam, ob lub ntsiab lus tuaj yeem txiav txim siab ib txhij. Yog li ntawd, JJG939-2009 "Atomic Fluorescence Spectrometer" txheej txheem pov thawj yuav tsum tau npaj cov txheej txheem sib xyaw ntawm ob lub ntsiab lus. Kev npaj cov tshuaj reagents thiab cov txheej txheem kev npaj tshuaj muaj nyob rau hauv JJG939-2009 yog qhov yooj yim. Cov hauv qab no yog cov ntsiab lus sib tham txog kev npaj, khaws cia thiab ceev faj txog cov txheej txheem kev daws teeb meem rau atomic fluorescence photometer verification.
1. Reagents thiab lawv cov khoom rau atomic fluorescence spectrophotometric
1. Hydrochloric acid: qib ntshiab ntshiab (GR)
Concentrated hydrochloric acid yog cov kua tsis muaj xim lossis daj me ntsis nrog cov ntxhiab tsw. Nws yog miscible nrog dej thiab soluble hauv lye. Kev ua haujlwm yuav tsum tau ua nyob rau hauv lub fume hood.
2. Potassium borohydride (borohydride)
Lub purity tsis tsawg tshaj li 95%. Dawb mus rau dawb dawb crystalline hmoov los yog pob, uas yog heev hygroscopic thiab yog li ntawd yuav tsum tau muab khaws cia ua ke nrog ib tug desiccant. Soluble nyob rau hauv dej, kua ammonia, insoluble nyob rau hauv ether, benzene, hydrocarbons, ruaj nyob rau hauv cov xwm, muaj zog nyob rau hauv reducibility, thiab nws cov tshuaj yog tsuas yog siv raws li ib tug txo tus neeg sawv cev. Vim tias cov tshuaj potassium borohydride yog yooj yim decomposed los ntawm lub teeb, cov tshuaj yuav tsum tau muab cia rau hauv ib lub raj mis xim av nyob rau hauv qhov tsaus ntuj nti.
3. Potassium hydroxide (sodium hydroxide)
Analytically ntshiab (AR) yog siv los tiv thaiv poov tshuaj borohydride. Nws yog dawb siv lead ua nyob rau hauv chav tsev kub, nws yog dej-absorbing thiab corrosive heev; nws yog yooj yim soluble nyob rau hauv dej thiab emits ntau cua sov.
4. Thiourea: Analytically ntshiab (AR)
Dawb ci iab siv lead ua, soluble hauv dej txias, ethanol, me ntsis soluble hauv ether, solubility hauv dej ntawm 20 ° C yog 137g / L. Nws yog tshuaj lom thiab tuaj yeem nqus tau los ntawm kev sib cuag ntawm daim tawv nqaij. Yog li ntawd, tsis txhob sib cuag nrog daim tawv nqaij thaum tsim cov tshuaj.
5. Secondary deionized dej
Hais txog cov dej tau txais los ntawm sub-boiling distillation ntawm cov dej deionized, uas feem ntau yog siv rau hauv physicochemical los yog analytical tests. Ntawm lawv, cov dej npaj los ntawm txoj kev sib pauv ion hu ua dej deionized, thiab cov dej deionized tsis yog dej tsis muaj ions, tab sis cov dej tau los ntawm kev sib pauv ion tsis cuam tshuam ions thiab muaj qhov nruab nrab pH (kev cuam tshuam ions feem ntau xa mus rau calcium, Magnesium, carbonate, sulfate, thiab lwm yam, tab sis cov organic teeb meem ib txwm muaj nyob rau hauv dej deionized tsis tuaj yeem raug tshem tawm). Cov dej deionized txawv ntawm cov dej distilled. Txoj kev distillation tsuas tuaj yeem tshem tawm cov khoom tsis-volatile hauv dej, thiab tsis tuaj yeem tshem tawm cov roj yaj hauv dej. Qhov purity ntawm cov dej distilled feem ntau tsis zoo li cov dej deionized. Cov dej deionized muaj qis dua cov dej distilled. Nyob rau hauv ib txwm muaj xwm txheej, kev soj ntsuam ntau npaum li cas ntawm cov dej distilled yuav siv tau, ntsuas dej feem ntau yog xaiv raws li cov txiaj ntsig ntawm qhov loj ntawm cov dej, tus qauv yam tsawg kawg nkaus yog dej deionized, ntawm no vim tias qhov tshwm sim yog qhov loj heev, yog li kev siv Secondary deionized dej.
6. Txuj kev daws teeb meem
Standard Tshuag tov ntawm arsenic (GBW08611, 1000μg / mL, U = 1μg / mL, k = 2, Tuam Tshoj Measurement Science Research Institute), 锑 (GBW (E) 080545, 100μg / mL, U = 1%, k = 2) .
2. Cov khoom siv uas xav tau rau kev npaj reagent rau atomic fluorescence photometer pov thawj
1. Qhov sib npaug: Qhov hnyav tshaj plaws yog 200g lossis 500g, thiab tus nqi faib tsis ntau tshaj 0.1g.
2. Cov cuab yeej ntsuas iav (Qib A): 100mL, 200mL, 1000mL muaj peev xwm fwj; 100 mL, 500 mL beakers; 1ml, 5mL, 10mL, 20mL pipettes los yog pipettes; iav rods.
3. Lwm yam kev sim ntsuas.
Thib peb, atomic fluorescence photometer pov thawj reagent npaj, khaws cia thiab ceev faj
1. Lub hauv paus ntsiab lus ntawm kev ua ntawm reagents rau atomic fluorescence photometer xyuas
JJG939-2009 qhia tias yuav tsum tau npaj ib qho kev daws teeb meem ntawm arsenic thiab antimony. Tus yuam sij rau kev txiav txim siab ntawm arsenic thiab antimony yog txo qis As(V) thiab Sb(V) rau hydrides. Raws li (V) thiab Sb(V) hnov mob nrog cov poov tshuaj borohydride rau lub sijhawm ntev, thiab As (III) thiab Sb(III) muaj feem ntau tsim cov hydride. Pretreatment yuav tsum txo cov pentavalent arsenic thiab antimony rau trivalent, yog li nws yog tsim nyog los ntxiv thiourea thiab ascorbic acid rau prereduction. JJG939-2009 qhia tias 100g / L thiourea aqueous tov yuav tsum tau ntxiv thaum tsim cov qauv kev daws teeb meem. Ascorbic acid tsis tau hais txog vim tias txoj haujlwm ntawm ascorbic acid yog ua kom cov tshuaj ruaj khov thiab txhawb kev txo qis. Lub luag haujlwm ntawm thiourea yog txo qis thiab Cu2 + Co3 +, Ni2 + plasma ua cov nyhuv npog, thiab txo cov nyhuv ntawm thiourea thiab ascorbic acid ua ke zoo dua. Raws li cov kev cai ntawm JJG939-2009, cov txheej txheem kev npaj yuav tsum tau siv tam sim no, thiab ntxiv ntawm ascorbic acid tsis muaj txiaj ntsig.
Thaum lub sij hawm soj ntsuam, cov tshuaj poov tshuaj borohydride tau ntxiv ib txhij nyob rau hauv acidic tej yam kev mob, thiab cov nram qab no cov tshuaj tiv thaiv tshwm sim:
E yog ib yam hydride (arsenic, antimony), thiab m tej zaum yuav los yog tsis sib npaug rau n.
Tom qab tsim hydride yog atomized, nws zoo siab los ntawm lub teeb lub zog ntawm qhov chaw hloov mus rau qib siab zog, thiab radiates atomic fluorescence thaum rov qab mus rau qis zog.
Nws yuav tsum tau muab sau tseg tias poov tshuaj borohydride yog ib tug muaj zog txo tus neeg sawv cev, uas yog yooj yim decomposed nyob rau hauv nruab nrab thiab acidic tej yam kev mob, reacts nrog oxygen thiab carbon dioxide nyob rau hauv dej los yog huab cua, thiab yog yooj yim decomposed los ntawm lub teeb. Qhov sib ntxiv ntawm cov poov tshuaj hydroxide rau cov tshuaj tso cai rau nws nyob ruaj khov dua, thiab tswj nws ntawm qhov kub thiab txias slows nws decomposition. Nyob rau tib lub sijhawm, potassium hydroxide yooj yim reacts nrog silicon nyob rau hauv lub khob los tsim sodium silicate, yog li cov tshuaj npaj tau muab khaws cia rau hauv lub raj mis yas kom tswj tau qhov zoo ntawm cov tshuaj. Yog tias nws tau siv tam sim no, nws yuav muaj kev cuam tshuam me ntsis ntawm iav.
2. Kev npaj cov reagents rau atomic fluorescence photometer pov thawj
(1) Kev npaj ntawm 100g / L thiourea tov
Siv qhov kev npaj ntawm 100 mL tov ua piv txwv. Nyhav 10g thiourea (dawb crystalline khoom, muab tso rau hauv ib tug me me beaker thiab hnyav nws los ntawm txawv txoj kev) nyob rau hauv lub analytical tshuav nyiaj li cas, dissolve nws nrog ib tug me me npaum li cas ntawm lwm yam deionized dej, maj mam do lub khob pas nrig, yog hais tias lub dissolution tsis tiav, thov siv da dej kom haum. Thaum tshav kub kub, tab sis tsis siab dhau. Cov tshuaj yaj thiourea tau pauv mus rau 100 mL volumetric flask siv lub iav pas nrig rau ntim. Hauv kev npaj ntawm thiourea tov, ascorbic acid yuav ntxiv los yog tsis.
(2) Kev npaj ntawm 100 ng / mL txheem cia tshuaj ntawm arsenic thiab antimony
Txoj kev dilution step-by-step tuaj yeem txo qhov yuam kev thiab txhim kho qhov tseeb. Yog li ntawd, thaum diluting cov arsenic thiab antimony txheem daws, nws yog diluted nyob rau hauv ob kauj ruam kom tau ib tug txheej txheem Tshuag tov. Pipette 1 mL ntawm arsenic txheem tov thiab 10 mL ntawm hydrazine txheem tov rau hauv 100 mL volumetric flask nrog ib tug pipette los yog pipette, thiab dilute mus rau ntim nrog lwm deionized dej los npaj 10 μg / mL arsenic thiab bismuth standard intermediate tov. Tom qab ntawd, 1 mL ntawm cov npaj 10 μg / mL arsenic thiab bismuth standard intermediate tov tau muab coj mus rau hauv 100 mL volumetric hwj, thiab lub ntim tau kho nrog cov dej deionized thib ob.
(3) Kev npaj cov txheej txheem sib xyaw ntawm arsenic thiab antimony
Pipette 100 ng / mL arsenic thiab bismuth standard stock solutions 0 mL, 1.0 mL, 5.0 mL, 10.0 mL, 20.0 mL nyob rau hauv 100 mL volumetric hwj, thiab ntxiv 100 mL / L thiourea tov 20 mL, feem. 10 mL ntawm hydrochloric acid yog diluted mus rau lub cim nrog lwm deionized dej.
(4) Kev npaj ntawm 5% hydrochloric acid tov
Siv 50 mL ntawm cov concentrated hydrochloric acid nyob rau hauv ib lub tog raj kheej ntsuas, dilute nrog li 200 mL ntawm cov dej theem nrab deionized, ces hloov mus rau 1000 mL volumetric hwj thiab dilute nrog lwm yam deionized dej.
(5) Kev npaj cov tshuaj potassium borohydride
Qhov concentration ntawm poov tshuaj borohydride yog txiav txim siab los ntawm cov concentration ntawm cov khoom yuav tsum tau ntsuas. Qhov concentration ntawm cov kua qaub kua qaub yog txiav txim siab los ntawm qhov concentration ntawm poov tshuaj borohydride, thiab cov kua khib nyiab zaum kawg yog acidic. Hauv kev sim txhua hnub, kev npaj ntawm 1.5% potassium borohydride tov yeej ua tau raws li qhov yuav tsum tau ua. Txoj kev npaj tshwj xeeb yog raws li hauv qab no: 15 g ntawm poov tshuaj borohydride yog hnyav thiab yaj nyob rau hauv 200 mL ntawm ob deionized dej yav tas los ntxiv nrog 5 g ntawm poov tshuaj hydroxide nyob rau hauv ib tug hluav taws xob tshuav nyiaj li cas, stirred kom txog thaum yaj, thiab xa mus rau ib tug 1000 mL volumetric hwj. iav pas nrig rau cov kua dej, thiab tom qab ntawd siv ob zaug. Dilute cov dej deionized rau lub cim.
3. Kev ceev faj hauv kev npaj tshuaj
(1) Lub iav ntsuas cov cuab yeej siv hauv kev npaj cov kev daws teeb meem yog raws li kev soj ntsuam sab.
Txoj kev sib txawv rau kev ntxuav. Cov iav rau kev txiav txim siab ntawm cov kab lus, thawj zaug txhuam nrog txhuam, yaug tawm cov teeb meem soluble nrog dej thiab txhuam tawm cov plua plav adhering rau saum npoo, ces muab tso rau hauv lub dropper, pipette, me me xeem raj hauv 10% nitric acid tov rau ntau. ntau tshaj 8 teev. Tom qab ntawd yaug nrog dej ntshiab. Thaum cov iav ntxuav tau muab tso rau hauv, cov dej yuav tsum ntws tawm ntawm lub nkoj phab ntsa yam tsis muaj dej ntws. Nyob rau lub sijhawm no, lub khob iav tau ntxuav 3 zaug nrog me me ntawm cov dej ntshiab, thiab cov impurities coj los ntawm cov kais dej raug ntxuav tawm thiab ntws tawm.
(2) Chav tsev ntawm cov tshuaj yuav tsum tau ua tib zoo tsim yog qhov loj concentration lossis qhov ntim concentration.
(3) Tom qab cov khoom reagent yaj nyob rau hauv lub beaker, nws yog drained mus rau hauv lub volumetric hwj nrog ib tug iav pas nrig, thiab lub beaker thiab lub iav pas nrig yog ntxuav ob peb zaug nrog rau lwm yam deionized dej, thiab cov dej ntxuav kuj poured rau hauv. lub raj mis volumetric. Lub beaker thiab lub khob ntim ntim tsawg kawg yog ntxuav. 3 rau 4x.
(4) Thaum lub ntim tau teem, ua ntej dilute nrog dej deionized kom dilute mus txog 3/4 ntim, ces co lub volumetric hwj ob peb zaug (tsis txhob co nws) ua ntej sib tov. Tom qab ntawd ntxiv cov dej thib ob deionized mus rau lub cim ze thiab ntxiv me ntsis kom ua rau lub ntsej muag concave ntawm cov tshuaj tangent mus rau txoj kab ntim ntawm lub ntim ntim. Tom qab ntawd siv lub iav stopper kom rov qab ntim lub khob ntim rov qab thiab tawm ob peb zaug kom sib tov cov tshuaj zoo.
(5) Thaum siv lub pipette los yog pipette los ntsuas cov reagent, nws yuav tsum tau muab yaug 2 mus rau 3 zaug nrog cov kev daws teeb meem.
(6) Thaum cov tshuaj aspirated, lub qhov ncauj hauv qab ntawm pipette los yog pipette yuav tsum tsis txhob yuav ntiav heev los yog tob heev kom muab tso rau hauv cov tshuaj yuav tsum tau noj. Yog tias nws ntiav heev, nws yuav ua rau nqus, thiab cov tshuaj yuav nqus mus rau hauv lub pob ntseg kom stain cov tshuaj. Sib sib zog nqus, nws yuav lo kua ntau dhau sab nraum lub raj.
(7) Txhawm rau txo qhov kev ntsuas qhov yuam kev, lub pipette yuav tsum siv cov nplai saum toj kawg nkaus raws li qhov pib taw tes txhua zaus, thiab tso cov ntim uas xav tau qis qis dua qhov ntim ntau npaum li cas. Tsuas yog lub tshuab nqus tsev twj tso kua mis, ib qho me me ntawm cov tshuaj tseem tshuav ntawm qhov kawg ntawm cov pipette tsis tuaj yeem raug yuam kom ntws tawm los ntawm kev quab yuam sab nraud.
(8) Ua ntej siv lub ntim ntim, sim cov dej xau, uas yog, muab cov kais dej tso rau hauv lub raj mis ze ntawm cov kab kos, npog lub ntsaws, tuav lub stopper los ntawm tes, thiab sawv ntsug lub khob ntim dej los saib seb puas muaj dej nkag hauv. lub raj mis. Yog tias nws tsis xau, Tom qab txhim kho lub raj mis, tig lub stopper txog 180 ° thiab tom qab ntawd sawv ntsug dua.
(9) Tsis txhob siv lub ntim ntim ntim ntim cov tshuaj npaj tau ntev. Yog hais tias cov tshuaj npaj yuav tsum tau khaws cia rau lub sij hawm ntev, nws yuav tsum tau hloov mus rau ib tug huv si sib tsoo reagent fwj.
(10) Thaum lub raj mis ntim tsis siv lub sijhawm ntev, nws yuav tsum tau ntxuav. Muab lub stopper rau ntawm daim ntawv ncoo kom tsis txhob qhib lub stopper tom qab lub sijhawm ntev.
(11) Cov concentration ntawm tus neeg sawv cev txo qis yog txiav txim siab los ntawm cov qauv, thiab cov concentration ntawm cov cab kuj yog txiav txim siab los ntawm cov concentration ntawm tus neeg sawv cev txo qis, thiab thaum kawg cov kua khib nyiab yog acidic. Yog hais tias nws tsis yog acidic, poov tshuaj borohydride yuav precipitate ntawm qhov qis tshaj ntawm cov kav dej thiab ces txhaws.
(12) Cov zaub mov yuav tsum tsis txhob muab tso rau hauv chav kuaj kom tsis txhob kis kab mob.
(13) Yog tias koj tsis txaus siab txog cov ntsiab lus ntawm cov tshuaj potassium borohydride thiab cov kua hauv lub cev, koj tuaj yeem siv cov ntawv ntsuas pH los kuaj nws. Yog tias cov kua khib nyiab yog acidic, nws yuav ua tau raws li qhov kev sim; Yog tias cov kua khib nyiab yog alkaline, cov tshuaj potassium borohydride Cov concentration siab dhau lawm.
(14) Cov txheej txheem kev daws teeb meem kuj tuaj yeem npaj nrog 5% hydrochloric acid, cov khoom siv tshuaj yuav ruaj khov dua thiab tuaj yeem khaws cia rau lub sijhawm ntev.
4. Kev txuag cov tshuaj rau atomic fluorescence
Ntxiv nrog rau cov txheej txheem kev daws teeb meem tuaj yeem khaws cia rau 6 lub hlis ntawm 0 ~ 5 ° C, lwm cov kev daws teeb meem yog siv tam sim no.
Txawm li cas los xij, WUBOLAB tau txais cov iav iav zoo tshaj plaws rau koj. Txawm li cas los xij iav iav hom lossis loj npaum li cas koj xav tau, peb nyob ntawm no los muab koj qhov zoo tshaj plaws. Peb cov iav saum toj kawg nkaus tuaj hauv ntau qhov ntau thiab tsawg; iav beakers, iav fwj lag luam wholesale, boiling lauj kaub, Laboratory funnels, thiab lwm yam. Koj tuaj yeem nrhiav cov khoom kuaj iav zoo meej rau koj cov kev xav tau. Dhau li ntawd, yog tias koj xav tau kev xaiv iav tshwj xeeb ntau dua, peb muaj cov iav tshwj xeeb. Cov khoom siv iav no muaj ntau yam kev xaiv rau koj qhov kev sim kuaj. Sib nrug los ntawm tag nrho cov no, mus rau peb cov iav tshwj xeeb yog tias koj xav tau cov kev daws teeb meem tshwj xeeb. Thaum kawg, peb kuj muaj customizable khob iav cov kev xaiv uas yuav dhau koj qhov kev cia siab! Yog li, tsis muaj kev ncua ntxiv, tso koj daim ntawv xaj tam sim no!
