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Analytick chemie a/b

Pavel Matjka Pavel.Matejka@vscht.cz K08, N01 skripta - Analytick chemie I a II (Volka a kol.) star uebnice - Analytick chemie (Holzbecher a kol.) - Analytick pruka (Zka a kol.) anglick uebnice - Analytical Chemistry Analytick tabulky Sbrky pklad Internetov zdroje

Analytick chemie - a
1) Zkladn pojmy a definice - terminologie 2) Rovnovhy v roztocch a jejich vznam v analytick chemii - acidobazick, komplexotvorn, redoxn - srec 3) Chemick kvalitativn analza - prvkov a molekulov - anorganick a organick analyty

Analytick chemie - a
4) Chemick analza kvantitativn gravimetrie a odmrn analza

5) Elektrochemick metody zkladn pojmy, statick metody, dynamick metody


6) Spektrln analza zkladn pojmy, kvalitativn a kvantitativn informace (optick metody)

Analytick chemie - b
7) Metody spektrln analzy (vetn specilnch) 8) Separan metody 9) Elektromigran metody

10) Spaen techniky a dal pokroil metody


11) Zpracovn a vyhodnocovn analytickch dat 12) Odbr vzork, pprava vzork a postup analzy

Zkladn pojmy
Definice IUPAC
Analytical chemistry is a scientific discipline that develops and applies methods, instruments and strategies to obtain information on the composition and nature of matter in space and time, as well as on the value of these measurements, i.e., their uncertainty, validation, and/or traceability to fundamental standards.

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Definice - American Chemical
Society Division of Analytical Chemistry
What is Analytical Chemistry? Analytical Chemistry seeks ever improved means of measuring the chemical composition of natural and artificial materials. The techniques of this science are used to identify the substances which may be present in a material and to determine the exact amounts of the identified substances. Analytical chemists work to improve the reliability of existing techniques to meet the demands for better chemical measurements which arise constantly in our society. They adapt proven methodologies to new kinds of materials or to answer new questions about their composition. They carry out research to discover completely new principles of measurement and are at the forefront of the utilization of major discoveries such as lasers and microchip devices for practical purposes. They make important contributions to many other fields as diverse as forensic chemistry, archaeology, and space science. As the emblem above points out, analytical chemistry serves the needs of many fields.

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Definice Wikipedia
Analytical chemistry is the science that seeks ever improved means of measuring the chemical composition of natural and artificial materials.

Chemical composition is the entire picture (composition) of the material at the chemical scale and includes geometric features such as molecular morphologies and distributions of species within a sample as well as single dimensional features such as percent composition and species identity.
The analytical results enabled by analytical chemistry have played critical roles in science from the understanding of basic science to a variety of practical applications, such as biomedical applications, environmental monitoring, quality control of industrial manufacturing and forensic science.

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Definice - Karl Heinz Koch
Fresenius J Anal Chem (1992) 343 : 821 - 822

Analytical Chemistry is a multidiscipline, comprising various

fields of chemistry with special understanding of physics,


mathematics, computer science, and engineering; it uses chemical, physicochemical, and physical or even biological methods for analytical signal production, followed by problem and matter-related signal processing and signal interpretation

in order to provide reliable (quality assured) qualitative,


quantitative and/or structural information about a sample.

Zkladn pojmy
Definice citace z lnku Karl Heinz Koch
Fresenius J Anal Chem (1992) 343 : 821 - 822

"Analytical Chemistry is a science of chemical characterisation and measurement" (H. A. Laitinen;1982) Analytical Chemistry is the application of principles of analytical measurement to generate information about chemical systems or to solve chemical problems as well. Analytical Chemistry, as defined above as a multidiscipline, is from a philosophical point of view an information science, and from an applied pragmatic point of view a problem solving science. (R. Kellner, H. Malissa; 1984)

Zkladn pojmy
VZOREK pracovn analyzovan materil, o nco pesnji reprezentant analyzovanho materilu

celkov, laboratorn, testovac, analytick - vzorkovn, odbr prava skladovn vzorku ANALYT pedmt analzy prvek, slouenina to co se snam identifikovat, stanovit MATRICE zbytek vzorku krom analytu (vliv na identifikaci, stanoven analytu?)

Zkladn pojmy
Analytick experiment princip - fyzikln a/nebo chemick a/nebo biologick zklad absorpce foton, chemick reakce metoda - pstrojov technika - FTIR spektrometrie postup - pouit metody pro konkrtn materil stanoven ropnch ltek v pitn vod nvod - sled pokyn pro konkrtn realizaci postupu podnikov norma, nvod ve skriptech SOP - standardn operan postupy

Analytick metody
KVALITATIVN ANALZA - CO ?

KVANTITATIVN ANALZA - KOLIK ? (pesn)


SEMIKVANTITATIVN ANALZA - KOLIK ? (zhruba)

doplujc otzky - KDE ? - lokalizace, distribuce


V JAK FORM ? - strukturn aspekty

Analytick metody
DESTRUKTIVN NEDESTRUKTIVN mal i velk spoteba vzorku on-line, in-situ, in-vivo CHEMICK ANALZA - reakce

BIOCHEMICK ANALZA - enzymatick reakce


FYZIKLN ANALZA - fyzikln princip

Analytick metody
ANALZA ANORGANICKCH MATERIL ANALZA ORGANICKCH MATERIL ANALZA BIOLOGICKCH MATERIL

ANALZA PEVN FZE pm i rozpoutn/rozklad


ANALZA KAPALN FZE

ANALZA PLYN
ANALZA FZOVHO ROZHRAN - povrchy, transport

Analytick metody
ELEMENTRN (prvkov, atomov) ANALZA

JAK PRVKY ?
KOLIK PRVKU ?

V JAK FORM ? MOLEKULOV ANALZA


JAK MOLEKULY ?

KOLIK DANCH MOLEKUL ?


STRUKTURA MOLEKUL (funkn skupiny) ?

Analytick metody - dle navky


MAKROANALZA - minimln desetiny gramu

SEMIMIKROANALZA - dov destky miligram


MIKROANALZA - dov desetiny miligramu a miligramy ULTRAMIKROANALZA - pod desetinou miligramu a k nanogramm

Analytick metody
PROCESN METODY on-line nasazen, rychlost, nzk cena PROVOZN METODY jednoduchost, rychlost, nzk cena KONTROLN METODY hodnocen surovin a produkt - urovn cen spolehlivost, rychlost, pimen cena ROZHOD METODY arbitrn zen i mezinrodn vysok spolehlivost, mezilaboratorn reprodukovatelnost

Typy sloek vzorku


HLAVN MAKROSLOKY - majoritn - nad 1 %

VEDLEJ MAKROSLOKY - minoritn - nad 0,01 %


MIKROSLOKY - stopov - pod 0,01 %

Rozloen sloek vzorku


HOMOGENN NEROVNOMRN s ostrmi hranicemi NEROVNOMRN s difznmi hranicemi

Sled krok pi analze


VOLBA ANALYTICK METODY ODBR VZORKU, TRANSPORT, SKLADOVN PRAVA VZORKU SEPARACE SLOEK

MASKOVN RUIVCH SLOEK


VLASTN POZOROVN I MEN VLASTNOST ANALYTU - v pvodn i upraven form ZPRACOVN a VYHODNOCEN VSLEDK

Dleit pojmy kvalitativn analzy


DKAZ - prvky, skupiny
IDENTIFIKACE - molekuly, formy analytu

MEZ DETEKCE - mez postehu, mezn zedn, mezn pomr SKUPINOV reakce (metody)
SELEKTIVN reakce (metody)

SPECIFICK reakce (metody)


SROVNVAC (slep) pokusy

Dleit pojmy kvantitativn analzy


STANOVEN MEZ STANOVITELNOSTI - um - slep pokus - vpoty nejistot PRACOVN ROZSAH CITLIVOST smrnice zvislosti signlu na obsahu analytu OPAKOVATELNOST REPRODUKOVATELNOST
KALIBRACE VALIDACE REGRESN METODY ZPRACOVN DAT

Zkladn pojmy
signl - namen data
zpracovn a vyhodnocovn dat
-prava dat - potlaen ruivch signl, jejich pvod lze popsat -potlaen umu (nhodn charakter) - statistick vyhodnocen

- hledn struktury dat

analytick vsledky - informace

ANALYTICK VSLEDEK
POADAVKY NA VSLEDEK
sprvn pesn opakovateln reprodukovateln

POADAVKY - NA EXPERIMENT
(vetn odbru a ppravy vzorku)

- NA ZPRACOVN DAT

ANALYTICK VSLEDEK
SPOLEHLIV VSLEDEK
validace celho postupu, tj. vech krok test ROBUSTNOSTI odolnost vi zmnm experimentlnch podmnek (nap. vnj teplota, tlak, zmna pstrojovch parametr) VKONNOSTN charakteristiky deteknho systmu
Rozsah pouitelnosti Prbh odezvy nap. linearita Citlivost Stabilita Opakovatelnost

Zkouky ve vce laboratoch reprodukovatelnost

METODY/TECHNIKY
Metoda Gravimetrie Men vlastnost Hmotnost istho analytu i sloueniny s definovanou stechiometri Objem odmrnho roztoku Ziv tok emitovan i absorbovan pi dan vlnov dlce Hmotnost vztaen na jednotkov nboj pro ion analytu a fragmentov ionty Rzn fyzikln chemick vlastnosti analyt Elektrick vlastnosti analyt v roztocch Charakteristick ionizujc zen emitovan analytem Pouit Kvantita hlavn a vedlej makrosloky Kvantita hlavn a vedlej makrosloky Kvalitativn, kvantitativn a strukturn analza od hlavnch makrosloek a po mikrosloky Kvalitativn, kvantitativn a strukturn analza od hlavnch makrosloek a po mikrosloky Separace sms - od hlavnch makrosloek a po mikrosloky Kvalitativn a kvantitativn analza od hlavnch makrosloek a po mikrosloky Kvalitativn a kvantitativn analza od hlavnch makrosloek a po mikrosloky

Odmrn analza Atomov a molekulov spektrometrie Hmotnostn spektrometrie Chromatografie

Elektrochemick metody Radiochemick analza

Namen data a jejich dimenze


jedna hodnota 5,00 mg (skalrn veliina - bod jednorozmrn prostor) ada dat uspodan N-tice 15,8; 27,2; 38,3 (vektor, N-rozmrn prostor) funkn zvislosti - dvojice hodnot - x, y - trojice hodnot - x, y, z - vce dimenzionln (matice) , tabulky, grafy

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