NMR樣品置備與數據X軸校正

NMR樣品置備

1.使用專屬NMR樣品管，將待測液體以玻璃滴管小心注入至樣品管底部
2.樣品液面高度至少3公分


數據X軸校正

取得數據後欲用ORGIN作圖得先進行X軸校正
orgin column校正公式為

Col(A) = Col (title) x [(first X- last X)/ B ] + last X

B 為X 軸第一個數字
first X 與 last X 為原始NMR scan 的範圍，可向技術員詢問

超實用材料資料庫網站推薦---Material project

由加州大學柏克萊分校創立的材料資料網站，材料分析時找參考資料的好網站



網站連結https://materialsproject.org/

GITT量測設置範例

Reference :https://onlinelibrary.wiley.com/action/downloadSupplement?doi=10.1002%2Fadma.201705580&file=adma201705580-sup-0001-S1.pdf

• A cell was charged or discharged at 30 mA g-1 rate for 20 min, followed by a 3 h open circuit step to allow relaxation back to equilibrium (defined as dE/dt < 0.2 mV h-1). 
• The procedure was continued until the charge (or discharge) voltage reached 1.8 V (0.2 V).
• The Zn2+ ion diffusion coefficients could be calculated using the following equation first outlined by Weppner and Huggins:

where, I is the current (A); 

Vm is the molar volume of the ZVO (cm3 mol-1); 

ZA is the charge number;

F is the Faraday’s constant (96485 C mol-1); 

S is the electrode/electrolyte contact area (cm2); 

dE/dδ is the slope of the coulometric titration curve, found by plotting the steady state

voltages E (V) measured after each titration step δ; 

dE/d√t is the slope of the linearized plot of the potential E (V) during the current pulse of duration t (s).

If sufficiently small currents are applied for short time intervals, so that dE/d√t can be considered linear and the coulometric titration curve can be also considered linear over the composition range involved in that step, the above equation can be simplified into:

Here, τ is the duration of the current pulse (s); 

nm is the number of moles (mol); 

Vm is the molar volume of the electrode (cm3 mol-1); 

S is the electrode/electrolyte contact area (cm2);

ΔEs is the steady-state voltage change, due to the current pulse and ΔEt is the voltage change during the constant current pulse, eliminating the iR drop.

XPS資料庫網站

1. NIST XPS database
https://srdata.nist.gov/xps/Default.aspx

2. Thermo Scientific 
https://xpssimplified.com/periodictable.php

3.Handbook of X-ray Photoelectron Spectroscopy
https://www.cnyn.unam.mx/~wencel/XPS/MANXPS.pdf

量測鋰電池中鋰離子擴散係數方法

參考資料連結: http://www.cailiaoniu.com/35490.html

方法一：循環伏安法（Cyclic Voltammetry, CV）

方法特點
①要求是可逆體系（電化學步驟可逆）②優點是設備簡單，數據處理容易③缺點1：得到的只是表觀的擴散係數④缺點2：濃度變化△Co的確切值很難求得。

方法二：交流阻抗法（Electrochemical Impedance Spectroscopy, EIS）

方法特點
①可以直觀的看出是否受擴散控制②缺點1：得到的結果也只是一個表觀的擴散係數③缺點2：要求所測體系的摩爾體積V _m不發生變化。

方法三：恆電位間歇滴定法（Potentiostatic Intermittent Titration Technique, PITT

方法特點
只需測電極的厚度，避開了電極的真實面積的大小和摩爾體積的變化。

方法四：電位弛豫法（Potential Relax Technique, PRT）

方法特點
①同PITT一樣只需測電極活性物質的厚度d②與PITT不同的是，PRT記錄的是電極電位隨時間變化的曲線，而PITT記錄的是電流隨時間變化曲線。

方法五：恆電流間歇滴定法（Galvanostatic Intermittent Titration Technique, GITT）

Standard Reduction potentials of all elements

Standard Reduction Potentials of Organic Species

Standard Reduction Potentials (E^0'), 25^oC

oxidant	reductant	n (electrons)	Eo´ (volts)
Acetate + carbon dioxide	pyruvate	2	-0.70
succinate + CO2 + 2H+	a-ketoglutarate + H2O	2	-0.67
acetate	acetaldehyde	2	-0.60
glycerate-3-P	glyceraldehyde-3-P + H2O	2	-0.55
O2	O2-	1	-0.45
ferredoxin (ox)	ferredoxin (red)	1	-0.43
Carbon dioxide	formate	2	-0.42
2H+	H2	2	-0.42
a-ketoglutarate + CO2 + 2H+	isocitrate	2	-0.38
acetoacetate	b-hydroxybutyrate	2	-0.35
Cystine	cysteine	2	-0.34
Pyruvate + CO2	malate	2	-0.33
NAD+ + 2H+	NADH  + H+	2	-0.32
NADP+ + 2H+	NADPH  + H+	2	-0.32
FMN (enzyme bound)	FMNH2	2	-0.30
Lipoic acid, ox	Lipoic acid, red	2	-0.29
1,3 bisphosphoglycerate + 2H+	glyceraldehyde-3-P + Pi	2	-0.29
Glutathione, ox	red	2	-0.23
FAD (free) + 2H+	FADH2	2	-0.22
Acetaldehyde + 2H+	ethanol	2	-0.20
Pyruvate + 2H+	lactate	2	-0.19
Oxalacetate + 2H+	malate	2	-0.17
a-ketoglutarate + NH4+	glutamate	2	-0.14
FAD + 2H+ (bound)	FADH2 (bound)	2	0.003-0.09
Methylene blue, ox	Methylene blue, red	2	0.01
Fumarate + 2H+	succinate	2	0.03
CoQ (Ubiquinone - UQ + H+	UQH.	1	0.031
UQ + 2H+	UQH2	2	0.06
Dehydroascorbic acid	ascorbic acid	2	0.06
Ubiquinone; ox	red	2	0.10
Cytochrome b2; Fe3+	Cytochrome b2; Fe2+	1	0.12
Cytochrome c1; Fe3+	Cytochrome c1; Fe2+	1	0.22
Cytochrome c; Fe3+	Cytochrome c; Fe2+	1	0.25
Cytochrome a; Fe3+	Cytochrome a; Fe2+	1	0.29
1/2 O2 + H2O	H2O2	2	0.30
Cytochrome a3; Fe3+	Cytochrome a3; Fe2+	1	0.35
Ferricyanide	ferrocyanide	2	0.36
Cytochrome f; Fe3+	Cytochrome f; Fe2+	1	0.37
Nitrate	nitrite	1	0.42
Photosystem P700	.	.	0.43
Fe3+	Fe2+	1	0.77
1/2 O2 + 2H+	H2O	2	0.816