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El. knyga: Applications of Reference Materials in Analytical Chemistry

(Laboratory of the Government Chemist), (Laboratory of the Government Chemist), (LGC Limited, UK), (Laboratory of the Government Chemist), Prepared for publication by (Laborator), (Laboratory of the Government Chemist, UK), (Laboratory of the Government Chemist)
  • Formatas: 160 pages
  • Išleidimo metai: 31-Oct-2007
  • Leidėjas: Royal Society of Chemistry
  • Kalba: eng
  • ISBN-13: 9781847559388
Kitos knygos pagal šią temą:
Applications of Reference Materials in Analytical ChemistryDidesnis paveikslėlis
  • Formatas: 160 pages
  • Išleidimo metai: 31-Oct-2007
  • Leidėjas: Royal Society of Chemistry
  • Kalba: eng
  • ISBN-13: 9781847559388
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Certified reference materials are a major way that laboratories can check the results of their analysis against the results of the same analysis conducted at different times and places. Speculating that more laboratories do not use them because there is not sufficient guidance available, Roper and colleagues from the Laboratory of the Government Chemist, Teddington, Britain explain how they can be best used to achieve analytical measurement results that are fit for their purpose. They describe the primary applications to instrument calibration, method validation, checking laboratory performance, and assessing the accuracy of analytical data. Annotation c. Book News, Inc., Portland, OR (booknews.com)

Reference materials play an important role in analytical chemistry, where they are used by analysts for a variety of purposes, including: checking and calibrating instruments; validating methods and estimating the uncertainty of analytical measurements; checking laboratory and analyst performance; and internal quality control. This book provides guidance and information for the users of certified reference materials (CRMs), explaining how they can best be used to achieve valid analytical measurements and improve quality in the analytical laboratory. General information on CRMs and how they are produced sets the scene for readers. The statistics relating to CRM use are then explained in an easy-to-understand manner, and this is followed by sections covering the main uses of CRMs. Detailed worked examples are used throughout. Structured and comprehensive in coverage, this book will be welcomed by all users of certified reference materials.


Structured and comprehensive in coverage, this book will be welcomed by all users of certified reference materials.

Recenzijos

"This handbook could serve equally well at the desk or bench, both in providing information and promoting good laboratory practice...Clearly laid out and with liberal, well-labelled illustrations this is an up-to-date, comprehensible reference that I recommend highly." * Chemistry in Britain, February 2002, p 51 * "... a very useful and well presented contribution to the QA/QC literature ..." * The Analyst Website, 2001 *

Introduction
1(7)
Certified Reference Materials and the VAM Principles
1(1)
Definitions and Hierarchy of Reference Materials
2(2)
Types of Reference Material
4(1)
Uses of Reference Materials in Analytical Chemistry
5(1)
Interpretation of Results Obtained with CRMs
5(1)
Availability of Reference Materials
6(1)
Quality of Certified Reference Materials
6(1)
References
7(1)
CRM Production
8(7)
Assessment of Priority Needs and Confirmation of Demand
8(1)
Literature Search and Project Plan
8(1)
Raw Material Selection and Processing
9(1)
Homogeneity Testing
10(1)
Stability Testing
10(1)
Characterisation
11(2)
Characterisation Using Gravimetric Preparation Data
11(1)
Characterisation Using a Primary (Definitive) Method
12(1)
Characterisation Using Independent Measurement Methods
12(1)
Characterisation by Inter-laboratory Studies
12(1)
Preparation of the Certification Report and Certificate
13(1)
References
14(1)
Simple Statistics for Users of CRMs
15(26)
Rules for Collecting Data from CRMs
15(2)
Concepts of Trueness, Precision and Accuracy
17(2)
Number of Required Replicates
19(1)
Detection of Outliers
20(3)
Assessment of Precision
23(1)
Assessment of Bias
24(1)
Converting Expanded Uncertainties into Standard Uncertainties
25(1)
Using CRMs to Detect other Forms of Bias
25(6)
Some Assumptions Behind Significance Testing
26(1)
t-Tests
27(1)
The F-test
28(3)
Using Statistical Software (What Is a p-Value?)
31(1)
Concepts of Measurement Uncertainty
31(1)
Principles of Least Squares Linear Regression
32(8)
Least Squares Linear Regression Statistics
33(4)
Confidence Intervals
37(1)
Extrapolation and Interpolation
38(1)
Bias, Leverage and Outliers
39(1)
References
40(1)
The Use of CRMs for Instrument Calibration
41(44)
Instrument Calibration
41(1)
Examples of CRMs Used for Instrument Calibration
42(4)
A Note on Terminology
42(1)
Pure Substance with a Documented Purity Value
43(1)
Pure Substance with a Documented Physical Property
43(1)
A Solution of a Substance with a Documented Concentration Value
44(1)
A Solution of a Substance with a Documented Property Value
44(1)
A Mixture of a Substance in a Solid Matrix with a Documented Concentration Value
45(1)
A Mixture of a Substance in a Gaseous Matrix with a Documented Concentration Value
45(1)
Instrument Calibration as Part of the Analytical Process
46(3)
Sample Matrix Effects
46(1)
The Accuracy Required in the Calibration Procedure
47(2)
Choosing a CRM for Use as a Calibration Standard
49(6)
Documentation for the CRM
49(1)
The Magnitude and Uncertainty of the Property Values
50(1)
How the Property Value Is Characterised
51(1)
The Traceability of the Property Value
52(1)
Physical/Chemical Form - Pure Substance or Matrix Material?
53(2)
Storage Requirements and Shelf Life/Expiry Date
55(1)
The Preparation of a Calibration Solution using a CRM
55(4)
Calibration Models
59(4)
Calibration Model 1
59(1)
Calibration Model 2
60(1)
Calibration Model 3
60(1)
Calibration Model 4
61(2)
Experimental Investigation of the Linear Calibration Model
63(4)
Experimental Conditions
63(1)
Instrument Stability
64(1)
Choice of CRMs
64(1)
Range of Property Values to be Covered
64(1)
Number of Calibration Points to be Obtained
64(1)
Spacing of the Calibration Points
65(1)
Number of Replicate Measurements
65(1)
Treatment of Results
65(2)
Using Linear Regression to Calculate the Calibration Line
67(4)
Combining Calibration Uncertainty with Analytical Uncertainty
71(1)
Assumptions in the Use of Linear Regression
72(3)
Abridged Methods of Calibration
75(2)
Single Point Calibration
75(1)
Two Point Calibration
75(1)
Uncertainty of Single Point and Two Point Calibrations
76(1)
Calibration by Bracketing
77(1)
Matrix Effects and Calibration
77(3)
Sample Dilution
78(1)
Matrix Matching
78(1)
Standard Additions
78(2)
Detection of Non-Linearity
80(4)
References
84(1)
Use of CRMs for Assessing the Accuracy of Analytical Data
85(21)
The Importance of CRMs in Routine Analysis
85(1)
The Selection of Matrix CRMs
86(2)
Documentation for the CRM
86(1)
Physical/Chemical Form
86(1)
Documented Property Values
87(1)
Uncertainty of the Documented Property Values
87(1)
Storage Requirements and Shelf Life/Expiry Date
87(1)
Quantity Taken for Analysis
88(1)
The Number of Different Matrix CRMs to be Used
88(1)
Principles Involved in Assessing the Accuracy of Routine Data
88(6)
What Is Accuracy?
88(1)
Procedures for the Assessment of the Precision of a Measured Result on a Matrix CRM
89(1)
The Rationale for Combining sb and sw
90(1)
Is the Within-laboratory Precision Acceptable?
91(1)
How Is a Value for the Bias Calculated?
92(2)
Issues Involved in Assessing the Accuracy of Routine Data
94(9)
Should a Result Obtained on a Matrix CRM Lie Within the Uncertainty Range of the Documented Reference Value?
94(1)
When Is the Uncertainty of the CRM Important?
95(2)
What Is the Uncertainty of the Bias Estimate?
97(1)
What Is the Bias Detection Limit?
98(3)
Why Is the Bias Detection Limit (3.7σ) Greater than the Acceptability Criterion of 2σ?
101(1)
How May a Fitness-for-Purpose Criterion be Used to Calculate Acceptability Limits?
101(2)
Action to Take When a Bias Is Detected
103(2)
Check the Calibration Standards
103(1)
Check Other Possible Sources of Bias
103(1)
Check the Precision of the Measurements
104(1)
Apply a Correction Factor?
105(1)
References
105(1)
Use of CRMs in Method Validation and Assessing Measurement Uncertainty
106(25)
What Is Method Validation?
106(1)
Why Is Method Validation Necessary?
107(1)
When Do You Validate a Method?
108(1)
How Do You Validate a Method?
108(1)
Method Performance Parameters
109(1)
The Tools of Method Validation
110(1)
The Role of CRMs in Method Validation
111(7)
What is Meant by Method Accuracy, Bias and Trueness?
111(1)
Measuring Bias Against CRMs
112(1)
How Bias Is Normally Expressed
113(1)
Measuring Bias Against a Reference Method
113(1)
Statistical Treatment of Results from a Study of Bias: Comparison with a Certified or Reference Value
114(2)
Statistical Treatment of Results from a Study of Bias: Comparison with a Reference Method
116(2)
Using Bias Information
118(1)
Use of CRMs in Estimating Method Recovery and Measurement Uncertainty
118(12)
Outline of Method for the Determination of Vitamin A and Vitamin E in Infant Formula
119(1)
Precision Study
119(1)
Bias (Recovery) Study and its Associated Uncertainty
120(1)
Estimating Rm and u(Rm) Using a Representative CRM
121(1)
Estimating the Contribution of Rm to u(R)
122(2)
Calcualtion of Rs and u(Rs) from Spiking Studies
124(1)
Calculating R and u(R)
125(1)
Calculation of Combined Standard and Expanded Uncertainties
126(2)
Expanded Uncertainty
128(2)
Summary
130(1)
References
130(1)
Annex A List of Reference Material Producers 131(5)
Annex B Statistical Tables 136(7)
Subject Index 143


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