分析化學之試 藥、儀器與單 元操作 第二章 分析化學的中心是由一組操作單元與儀器裝置所構成的核 心，這一組是訓練過程之實驗工作所必需的，也是分析化學之成 長與研發的基礎。在這張照片中，一位學生正在測量有機物質樣 品中的氮含量，並且將滴定數據記錄在實驗記錄簿中。 在本章中，將介紹分析化學家所使用的工具、技術與 試藥。從兩個世紀前直到今日都一直在進行這些工具的研發 工作。而隨著電子分析天平、自動滴定儀和其他電腦操控儀 器先後問市，而改良了分析化學的技術，分析方法的操作速 率、便利性、準確度與精密度通常也會隨之改善。譬如在 40 年前，測量樣本質量需要花費 5 到 10 分鐘，而如今則只需要 數秒鐘的時間即可。而使用對數表進行 10 到 20 分鐘的計算 過程，現在使用電腦試算表或電子計算機之後，就幾乎可以 立即完成這項工作。因為我們已經習慣了這些偉大的技術性 改善作法之後，對於古典分析化學的一些繁雜技術，通常就 會缺乏耐心進行之。而正因為這種不耐性驅使人們再去研發 出更好的技術方法。事實上，因為追求速率與便利性的興趣 而對古典方法所進行的改良工作，通常並不需要犧牲其準確 度與精密度。 然而必須強調的是，在分析實驗室中，有許多單元操 作是永遠都會被使用到的。在過去兩個世紀以來，這些嘗試 和實際運作的操作都一直被逐漸改良著。有時候，在本章中 所提出的一些指導方針會顯得有點教條式。雖然我們會嘗試 解釋，為什麼單元操作需要以其中所描述的方式來進行之， 然而也是可以試著去改變其中的步驟，或者跳過此處或其他 的一兩個步驟，以節省操作時間和人力。不過要再度提醒的 是，除非已經和指導教師討論過將要進行的改變工作，並且
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-
40
5 10
10 20
-
2-2
100
2A
2A-1
(American Chemical
Society, ACS) 1
ACS
(primary standard)
13A-2
(National Institute of Standards and 1 Committee on Analytical Reagents, Reagent Chemicals, 10th ed. Washington, DC: American Chemical Society, 2005,
(NIST)
(National Bureau of Standards)
-
2-3
Technology, NIST)
(reference
standard)2
2A-2
1.
2.
3.
4.
5.
2 NIST (Standard Reference Materials Program, SRMP) www.nist.gov NIST NIST
-
2-4
6.
7.
2B
()
3
2C
2-1
3 38
2-1
-
2-5
(bumping)
(wet ashing)
2D
2D-1
(analytical balance) 1 g
105
106
(macrobalance)
160 200 g
160 200 g 0 .1
mg
1 g
105
-
2-6
0.1 mg (semimicroanalytical
balance) 10 30 g
0.01 mg (microanalytical balance)
1 3 g 0.001 mg (1 mg)
(equal-arm balance)
(single-pan analytical balance) 1946
(electronic
analytical balance)
2D-2
2D-3
2D-2 4
2-2
(levitate)
1 3 g
0.001 mg
1 g
4 R. M. Schoonover, Anal. Chem., 1982, 54, 973A; DOI: 10.1021/ac00245a003.
10 30 g
0.01 mg
-
2-7
(servo system)
2-3
(cell)
(flexure)
2-3a 2-3b
(taring control)
100
2-2 (a) (b) (a) R. M. Schoonover, Anal. Chem., 1982, 54, 973A. Published 1982 American Chemical Society.
-
2-8
30 g 0.01 mg
2D-3
2-3 (a) (b) (a) R. M. Schoonover, Anal. Chem., 1982, 54, 973A. Published 1982 American Chemical Society. (b) K. M. Lang, Amer. Lab., 1983., 15(3), 72. Copyright 1983 by International Scientic Communications, Inc.
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2-9
2-4
(beam) (knife edge) (A)
(B)
(stirrup)
(beam arrest) (pan
arrest)
2 -4 [
R . M . Schoonover , Ana l . C h e m . , 1 9 8 2 , 5 4 , 973A. Published 1982 American Chemical Society.]
-
2-10
(air damper) (dashpot)
(< 1 mg)
100 mg
2-4
0 100 mg (reticle)
0.1 mg
-
2-11
1.
2.
3. 2E-6
4.
5.
6.
7.
2D-4 5
(buoyancy error)
6
W1 W2 dobj
dwts dair dair
0.0012 g/cm3
2-5 2-1
2 g/cm3 0.1
pH
5 R. Battino and A. G. Williamson, J. Chem. Educ., 1984, 61, 51, DOI: 10.1021/ed061p51.6 M. R. Winward et al., Anal. Chem., 1977, 49, 2126, DOI: 10.1021/ac50021a062.
-
2-12
7.8 8.4 g/cm3 8
g/cm3
10 15 mg 2-6
2-5
= 8 g/cm3
-
2-13
Static-Master
2-6
110
AB 7.5 g KCl
2-1
7.6500 g 0.92 g/cm3
9.9700 g (d = 8.0 g/cm3)
9.9700 _ 7.6500 = 2.3200 g
2.3200 g 2-1 dair
0.0012 g/cm3 dobj 0.92 g/cm3 dwts 8.0 g/cm3
-
2-14
100 mg
2D-5
150 200 g 1 mg
25,000 g
0.05 g
2E
-
2-15
0.2 0.3 mg
2E-1
(weighing bottle)
2-7
2E-2
(desiccator) 2-8
(Drierite)Anhydrone Dehydrite
0.2 0.3 mg
2 -7
-
2-16
2E-3
105 110
2-9
2-8 (a) (b)
2-9
-
2-17
2-10
2E-4
2E-5
2-10
-
2-18
2E-6
2F
2F-1
-
2-19
2-11
2-16
(sintered-glass) (fritted-glass)
fm c
200
(Gooch crucible)
500
2-11
-
2-20
38C-11
9 11 cm
0.1 mg
()
2-1
1
-
2-21
140 260
110
12 16
5 6 7
8
(Meker)
(Tirrill) (Bunsen)
(muffle furnace) 1100
2F-2
7 E. S. Beary. Anal. Chem., 1988, 60, 742, DOI: 10.1021/ac00159a003.8 R. Q. Thompson and M. Ghadradhi, J. Chem. Edu., 1993, 70, 170, DOI: 10.1021/ed070p170.
2-11
-
2-22
2-15
0.3 mg
(decantation)
(washing) (transfer)
2-12a
2-12b
2-12(a) (b)
-
2-23
(rubber
policeman)
(creeping)
Triton X-100
2F-3
2-13 60 deg
(a)
(b) (c)
(d)
(e)
(f)
-
2-24
2-13 (a) (b) (c) (d) (e) (f)
2-14
(a) (b)
(c) (d)
(e)
-
2-25
2-14 (a) (b) (c) (d) (e)
1 cm
2-15
2-15
-
2-26
2-16
2F-4
1.
2.
3.
4.
2G
2-16
-
2-27
2G-1
(liter) (L)
(milliliter) (mL) (0.001 L)
(mL) 10_6 L
10_3 mL
2G-2
0.025%/5
10_3 L
5 40.00 mL
20
20
20
1
2G-3
(pipet) (buret) (volumetric
A B PyrexKimax
A 2 - 2 9 2-31 B
A
2-2
-
2-28
flask)
TD TC
2-17
2-2 (volumetric)
(transfer) 2-17a 0.5 200 mL
2-17 (a ) (b) (c ) (d) Eppendorf (e) (f)
-
2-29
(measuring pipet) 2-17b c
0.1 25 mL
2-2
Eppendorf 2-17d
2-18a
1
* TDTC**
-
2-30
2-18b
LCD
10 L 20 mL
2-18 (a) 100 1000 L 100 L 3.0% 0.6% 1000 L 0.6% 0.2% 525 L
-
2-31
2-19a
Teon
2-19b
5 mL 5 L
(TC)
2-20
(TD)
2G-4
-
2-32
2-19 (a)(b)
2-20
(meniscus)
(parallax)
-
2-33
2-21 (a)
12.58 mL (b)(c)
12.62 mL (d)(e)
12.67 mL (f)
(c) (d)
2-21
-
2-34
Propipette (B) AC D
A B A C C D D
2G-5
2
3 cm
2-22a 2-22b
2-22c
-
2-35
2-22 (a) (b)
(c) (d) (e)
(f) (g) (h)
2-22d 2-22e
2-22f
10
2-22g, h
-
2-36
2G-6
(1)
(2)
(3)
1.
2.
3.
5 10 mL
0.01 mL
-
2-37
(~ 1 min)
0.01 mL
2-23
1 mL
2
3 30
0.01 mL
1.
2.
3
3.
2-23
-
2-38
2G-7
(~ 1 min)
-
2-39
2H
2D-4
2-1
(T) 2-2
20
2-3
2-3
T (1)
(2) 20
-
2-40
2H-1
2-3
25 mL 25
24.976 g 2-3 25 20
*
-
2-41
2-3
1
0.00 mL
10
125 mL
10 mL/min
10 mL
1
2-3
-
2-42
0.02 mL
20 mL
10 mL
2-3
50 mL 500 mL
50 mL 500 mL
2I
-
2-43
2I-1
1.
2.
3.
4.
5.
2I-2
9
2-24
1.
2.
3.
9 Howard M. Kanare, Writing the Laboratory Notebook. Washington, DC: American Chemical Society, 1985.
-
2-44
4.
1.
2.
3.
2-24
-
2-45
2J
1.
2.
(Ofce of Safety and Health Administration, OSHA)
3.
4.
5.
6.
7.
-
2-46
8.
9.
10.
11.
12.
13.
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