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교재 : Quantitative Chemical Analysis (5th Edition, 1999) (D. C. Harris): 원서사용 권장 : 2 학기 교재임. 강의실 변경 : 과 424  과 B101. 연락처 : 이동수 : 2123-2641, [email protected] ( 메일사용 권장함 ): 과 442. 조교정보. 성적평가 : 1. 수업참여도 : 10% 2. 시험 (3 회 ): 65% 3. 문제풀이 및 기타 : 25%.

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Quantitative chemical analysis 5th edition 1999 d c harris

교재 :QuantitativeChemicalAnalysis

(5thEdition,1999) (D.C.Harris):

원서사용권장 : 2학기 교재임

강의실 변경:

과 424  과 B101


Quantitative chemical analysis 5th edition 1999 d c harris

연락처:이동수:2123-2641,[email protected](메일사용권장함):과442

조교정보

성적평가:

1. 수업참여도:10%

2.시험(3회): 65%

3.문제풀이및기타:25%

조교: 하재윤추후공고과443A,443B


Quantitative chemical analysis 5th edition 1999 d c harris

화학: the science that deals with the properties, composition, and structure of substances (defined as elements and compounds), the transformations that they undergo, and the energy that is released or absorbed during these processes.

무기화학: 무기물을 관찰하여 얻은 정보(구조, 성질, 반응 등)를 분류.

정리하여 체계화 한 학문

유기화학: 유기물을 관찰하여 얻은 정보(구조, 성질, 반응 등)를 분류

정리하여 체계화 한 학문

분석화학: 화학에서 다루는 모든 대상물질의 관찰방법을 다룸

물리화학 : 무, 유기물에 대한 모든 지식과 정보들의 공통적인 배경을

귀납하고 가설을 세워 이론적인 배경을 도출하여 체계화

시킨 것


Quantitative chemical analysis 5th edition 1999 d c harris

분석화학 영역

  • environmental

The ore-carrier Treasure sunk off the coast of South Africa June 23, 2000, spilling 1300 tons of oil. The massive oil spill oiled thousands of birds who live on Robben and Dassen Islands.

  • manufacturing

  • forensic

traces of car paint found on the bicycle

Chemical analysis plays an essential role in all aspects of chemistry:


Quantitative chemical analysis 5th edition 1999 d c harris

  • sleuthing

2-dimensional diffraction pattern of small amount of soil sample

traces of soil on the boot

  • Medicine

  • Archeology


Quantitative chemical analysis 5th edition 1999 d c harris

분석화학의 분류

정성분석과 정량분석:

정성분석: 시료에 들어 있는 원소나 화합물의 종류

정량분석: 시료에 들어 있는 원소나 화합물의 량

--> 분석화학에서는 주로 정량분석을 다룸

고전분석과 기기분석

고전분석(습식분석): 시료 중 분석물질을 분리하여

무게나 부피측정을 통해 정량

기기분석 : 분석물질의 물리적 성질(전기, 빛, 질량등)

측정을 통해 정량

두 방법 모두 유용함: 분석화학I은 주로 고전분석내용


Quantitative chemical analysis 5th edition 1999 d c harris

용어 (Terminologies)

Heterogeneous material composition of the material varies from one part to another

Homogeneous material composition of the material is uniform throughout

Lot the total material from which samples are taken from

Bulk sample a portion of material obtained from the lot for analysis

Laboratory sample

a portion of the bulk sample


Quantitative chemical analysis 5th edition 1999 d c harris

Aliquot a small test portion of the laboratory sample which are used for individual analyses.

Analytethe chemical substance being measured during a chemical analysis

Interference occurs when species other than the analyte increases or decreases the response of the analytical method thus making it appear that there is more or less analyte than is actually present

분취량

분석물질

방해물질


Quantitative chemical analysis 5th edition 1999 d c harris

Masking transforming interfering species into a form that is not detected by the analytical method;

eg

Analysis: Ca2+ in natural waters

Analytical method: measurement with EDTA 적정

Interference: dissolved Al in the water also reacts wit EDTA thus causing interference to the analysis

Masking: Treatment of water sample with excess F- which reacts with Al3+ to form AlF3- which does not react with EDTA

6


Quantitative chemical analysis 5th edition 1999 d c harris

화학분석의 일반절차

1. Define problem

2. Select analytical procedures

문헌 조사 ㅡ> 방법선택/ 개발

3. Bulk sampling

4. Sample preparations :분쇄, 혼합, 용액화, 농축,

분리, mask

5. Measuring analyte concentration

6. Reporting and interpretation: 신뢰도(유효 숫자),

정확도

7. Drawing conclusions: 올바른 정책결정, 반영 유도


Quantitative chemical analysis 5th edition 1999 d c harris

0장 화학분석과정 (절차)

Task : 쵸코렛 함유 카페인과 티오브롬 정량

티오브롬 : 카페인의 전구물질

분석방법 선택 : 고성능 액체크로마토그래피법 (HPLC:High Performance Liquid Chromatography)

Chemical Abstracts search를 통해 방법 선정

HPLC : Text p 713 참조


Quantitative chemical analysis 5th edition 1999 d c harris

시료제조 (Sample Preparation)

  • 마쇄하기

  • 무게재기

  • 용해-원심분리-여과로 방해물질제거 (지방, 비 용해성 물질)

Fig 0-2 Fat extract, Fig 0-3 residue removal

쵸코렛의 조성

1. 분석물질 (카페인, 티오브롬) : 수용성

2. 지방(fat) : 주요방해물질 : 지용성

3. 비 용해성 물질(polysacharide?)

: HPLC 분석방해 : 여과제거


Quantitative chemical analysis 5th edition 1999 d c harris

Chemical Analysis

액체 크로마토그래피의 원리: Fig 0-4

Using High Performance Liquid Chromatograph(HPLC)

Stationary Phase : C-18 column

Mobile Phase (eluant) : 79% H2O+ 20% MeOH

+ 1% HOAc

UV detection

Fig 0-5 HPLC chromatogram for the sample


Quantitative chemical analysis 5th edition 1999 d c harris

From Chromatogram, Peak Identification  Fig 0-6

머무름시간(retention time) 정성분석

Peak Area or Height 정량분석

Calibration Curves (검량선)

See Fig. 0 -7 : Standard Preparation

Interpreting the Results

See Table 0-1 Analysis results

Standard deviation (표준편차)


Quantitative chemical analysis 5th edition 1999 d c harris

5cm radius patches chosen at random

Random heterogeneous material

Sampling and Sample Preparation

1. Sampling : process of selecting representative material

. 비균질 시료의 채취

예1) Al정량을 위한 해수채취 (Fig. 0-8)

Na나 Cl의 경우 문제가 덜 심각함

예2) glass panel (Box 0-1), or Rock


Quantitative chemical analysis 5th edition 1999 d c harris

2. Sample preparation: process which converts the bulk sample into homogeneous laboratory sample; also refers to steps that eliminate interfering species.

. 분쇄-혼합

Bulk sample --> Laboratory sample : Fig. 0-9

Take an aliquot for analysis

. 방해물질 제거, 분석물질 농축

예1 ) 분리를 통한 Fat의 제거

예2 ) Masking법 : Ca+2 정량시 Al +3 masking by F-


Quantitative chemical analysis 5th edition 1999 d c harris

Lot the total material from which samples are taken from

Bulk sample a portion of material obtained from the lot for analysis

Laboratory sample

a portion of the bulk sample

Sample type Fig. 0- 9


Quantitative chemical analysis 5th edition 1999 d c harris

화학분석의 일반절차

1. Define problem

2. Select analytical procedures

문헌 조사 ㅡ> 방법선택/ 개발

3. Bulk sampling

4. Sample preparations :분쇄, 혼합, 용액화, 농축,

분리, mask

5. Measuring analyte concentration

6. Reporting and interpretation: 신뢰도(유효 숫자),

정확도

7. Drawing conclusions: 올바른 정책결정, 반영 유도


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