# Sample Analysis Design Step 2 Calibration/Standard Preparation Choice of calibration method dependent upon several factors:

Save this PDF as:

Size: px
Start display at page:

Download "Sample Analysis Design Step 2 Calibration/Standard Preparation Choice of calibration method dependent upon several factors:"

## Transcription

1 Step 2 Calibration/Standard Preparation Choice of calibration method dependent upon several factors: 1. potential matrix effects 2. number of samples 3. consistency of matrix across samples

2 Step 2 Calibration/Standard Preparation EXTERNAL CALIBRATION: Prepare a set of standard solutions to cover the expected range of analyte concentrations Fit a least squares regression line y = mx + b and calculate analyte concentration in unknowns

3 Step 2 Calibration/Standard Preparation 23 Na calib curve (Medium resolution) y = 17557x R 2 = cps conc ppb

4 Step 2 Calibration/Standard Preparation 44 Ca calib curve (Medium resolution) y = x R 2 = cps conc ppb

5 Step 2 Calibration/Standard Preparation Advantages of External Calibration Easy to prepare Quick Widely used technique

6 Step 2 Calibration/Standard Preparation Disadvantages of External Calibration: Need to matrix match calibration solutions and samples If standards containing <2000 ug/ml (ppm) are being used, then preparing the standards as simple aqueous solutions using the acid matrix (5% HNO 3 ) employed for the samples is sufficient HOWEVER, if the samples contain a very high concentration of one (or more) elements, then this may not be adequate

7 Step 2 Calibration/Standard Preparation Preparation of External Calibration Solutions: Need to evenly space calibration concentrations If the highest concentration is much higher than the rest, linear regression introduces bias favoring the high point X = independent variable = concentration Y = dependent variable = counts/second

8 Standard Addition Method Aliquots of spike are added to unknown samples to increase the ion signal intensities for elements of interest Typically use at least three aliquots of sample spiked with evenly spaced amounts of analyte These spiked aliquots of sample are used to generate a calibration line and calculate the concentration in the sample

9 Standard Addition Method S0 = unspiked sample S1 = sample spiked with analyte at concentration x S2 = sample spiked with analyte at concentration 2x S3 = sample spiked with analyte at concentration 3x S4 = so on and so on

10 Standard Addition Method AMT y = 29387x R 2 = Cps Concentration (ppb)

11 Standard Addition Method The concentration of the unknown solution is then determined by dividing the y-intercept value by the slope of the sample-spike mixing line. From example on previous slide, Conc. sol n = / = 9.5 ppb If the original sample was a solution, then this is the concentration of the analyte in question in the solution

12 Standard Addition Method If the original sample was in solid form that you digested and subsequently converted into a solution; then in order to determine the concentration of the analyte in question, you must factor in the amount of total analyte in the solution and the dry weight of the sample powder

13 Standard Addition Method If we continue with the same example, the solution has a concentration of 9.5 ppb, and the original volume of the unknown solution was 10 ml (g) prior to aspirating some of it into the plasma for analysis, then the total amount analyte in the solution is: = 10 g x 9.5 ng/g (ppb) = 95 ng, or = µg If the amount of powder weighed out was 0.1 g, then the concentration of the element in question is: Conc. = µg/0.1 g = 0.95 µg/g or ppm

14 Standard Addition Method This method works best if the slope of the calibration line is not too shallow This will create more uncertainty in the location of the intersection between the cps of your unknown and the calibration line

15 Standard Addition Method For maximum precision it s necessary that the amount of sample be the same in each aliquot Also want the amount of spike added to be the same for each aliquot Amount of spike added should be as small as possible (usually 0.1 ml to 10 ml total volume)

16 Standard Addition Method Ideally, the highest spike concentration should be approximately equal to the concentration of analyte in the unknown Need to have some idea of the concentration in the sample prior to analysis

17 Advantages: Sample Analysis Design Standard Addition Method Overcomes matrix differences More precise and accurate than external calibration Disadvantages: Requires at least three aliquots for each sample Run lengths become much longer and more preparation time is required

18 Isotope Dilution Most accurate and precise calibration method available Requires analyte with two stable isotopes Monoisotopic elements cannot be determined via isotope dilution Spike natural sample with enriched isotope spike of analyte

19

20

21 Isotope Dilution The amount of spike is selected so that the resulting ratio between spiked isotope and unspiked isotope is near unity maximizes precision Typically use the most abundant isotope as the reference -- maximizes sensitivity

22 Isotope Dilution Check isotope ratio in unspiked sample to determine if the natural ratio in the sample matches with the predicted ratio If not -- interference in acting on one or both of the isotopes Always attempt to use interference free isotopes

23 Isotope Dilution Prepare the spike to desired concentration Add spike as early as possible after equilibration of spike and sample you don t have to have complete sample recovery During any stage of the process complete equilibration is absolutely necessary

24 Isotope Dilution Analyze the solution on the ICP using many repetitive scans (to maximize precision) Need to measure isotopic ratios on standards of a known ratio in order to correct for machine mass discrimination Use previous equation to calculate concentrations!

25 Advantages: Sample Analysis Design Isotope Dilution Most accurate and precise method for quantitative elemental concentrations Partial loss of analyte during preparation is compensated for since physical and chemical interferences are not an issue -- will cancel out as they will affect each isotope identically Ideal form of internal standardization since another isotope of the same element is used in this capacity

26 Isotope Dilution Disadvantages: Generally only applicable to multiple-isotopic elements Need an enriched isotope spike for the analyte of interest - not always available or sometimes at very high cost Need two interference free isotopes VERY time consuming

27 Sample Analysis Design STEP 3 INTERNAL STANDARDIZATION & INSTRUMENT DRIFT CORRECTION

28 Internal Standard Every sample should be analyzed with an internal standard (IS) What is an internal standard (IS)? element that is added to EVERY sample/ blank/calibration standard/qa sample/etc., that is not expected to be in the sample in appreciable quantities and is not an element of interest use IS to monitor machine drift (both short and long term) and matrix effects

29 Internal Standard Choice of IS depends upon which elements you are quantifying The IS should have similar properties in the plasma as element(s) of interest ICP-MS: similar in mass/ionization potential

30 Example: Sample Analysis Design Internal Standard attempting to quantify U - use Th attempting to quantify most transition metals - use As attempting to quantify REEs - use Re 115 In and 103 Rh are common IS for general use alternatively, you can add several IS to each sample

31 Internal Standard From previous slide, we assume that samples have little or no Th, As, or Re It s important to have an idea of what s in your sample prior to quantitative analysis Solid samples can use a naturally occurring element as IS, provided that you know the concentration in each sample

32 Procedure for IS use: Sample Analysis Design Internal Standard Calculate the concentration of the IS in each centrifuge tube the latter will contain an aliquot of your sample and an aliquot of the IS Divide the measured ion signal (CPS) by the concentration of your IS to derive the factor = CPS/ppb Divide CPS/ppb of each tube by the CPS/ppb for those measured for the blanks since these are not influenced by possible effects due to sample matrices The latter yields a dimensionless correction factor (I refer to it as a normalization factor) Use correction factor to adjust analyte counts for drift or matrix effects

33

34

35 Advantages: Sample Analysis Design Internal Standard Fluctuations are monitored in each sample/ calibration / blank Disadvantages: Assume that behavior of IS is the same as the analyte

36 Instrumental Drift Correct for instrument drift with: Internal standardization is a common procedure Use of drift corrector solutions (DCS)

37 Instrumental Drift Drift Corrector Solutions (DCS): Measure the same solution intermittently throughout the course of the analytical session Change in ion signal is assumed to be linear between each DCS measurement

38 Instrumental Drift The DCS should contain all elements of interest and can be matrix matched to samples Example: use standard reference materials (SRMs) for DCS

39 Instrumental Drift Apply a linear correction to samples between DCS solutions DCS 1 + ((DCS 2 - DCS 1 )*F) F = position dependent fraction

40 Instrumental Drift Advantages of DCS correction: all analytes are monitored for drift nothing added to sample solutions Disadvantages of DCS correction: assume change is linear cannot easily monitor matrix effects

41 Background & blanks Standard blank - blank used to monitor polyatomic ion interferences, gas peaks, and contamination from reagents; used for background subtraction Procedural blank - blank used to monitor contamination acquired during all stages of sample preparation; grinding, digestion, acidification, powdering, etc

42 Background & blanks Use of blanks during an analytical session: ALWAYS begin an analytical session with at least one standard blank Analyze standard blanks periodically throughout the course of the session in particular to monitor memory effects Process and analyze at least one procedural blank at some point during your research study; for its analysis, it s preferable to measure it early in order to avoid any potential memory effects

43 Background & blanks The more standard blanks that are run during an analytical session, the more information you will have with regards to monitoring change(s) in background levels throughout the entire session

44 Background & blanks How to determine the background : 1. just use the first standard blank 2. average all standard blanks 3. take median of all standard blanks 4. apply statistical analysis to standard blanks and select some of them

45 Outlier tests: Sample Analysis Design Background & blanks 1. I know the truth 2. Looks different 3. Statistical proof

46 Background & blanks Option 1 should be avoided - unscientific and invalid Option 2 is better but only if the measurement is repeated Option 3 is the best approach, but needs to be carried out carefully in order to avoid false negatives and positives

47 Background & blanks Huber Outlier Test take median of all values calculate absolute deviation x i -x m take mean of absolute deviations (MAD) multiply MAD by coefficient (k = 3-5) anything higher than k*mad is rejected as outlier

48 Background & blanks Calculation of Limit of Detection (DL) and Limit of Quantification (QL) Easy way: LOD = 3*STDEV blank ; LOQ = 10*STDEV blank

49 SUMMARY A good analytical method will: 1. provide the means to calculate an accurate background level 2. allow for correction of instrument drift 3. use Internal standardization to monitor matrix effects 4. provide some method for monitoring/ correcting interferences 5. Use a proper calibration strategy

50

51

52

53 Example Calculation Determination of Ca and Na in beetle blood Using External Calibration Method

### Sample Analysis Design Isotope Dilution

Isotope Dilution Most accurate and precise calibration method available Requires analyte with two stable isotopes Monoisotopic elements cannot be determined via isotope dilution Spike natural sample with

### Graphite Furnace AA, Page 1 DETERMINATION OF METALS IN FOOD SAMPLES BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY (VERSION 1.

Graphite Furnace AA, Page 1 DETERMINATION OF METALS IN FOOD SAMPLES BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY I. BACKGROUND (VERSION 1.0) Atomic absorption spectroscopy (AAS) is a widely used

### Quantitative & Qualitative HPLC

Quantitative & Qualitative HPLC i Wherever you see this symbol, it is important to access the on-line course as there is interactive material that cannot be fully shown in this reference manual. Contents

### 2013 Laboratory Conference: Unraveling the Mystery of Pharmaceutical Laboratory Science Mission Impossible Low Level Detection Challenges

2013 Laboratory Conference: Unraveling the Mystery of Pharmaceutical Laboratory Science Mission Impossible Low Level Detection Challenges Jerry Dalfors JD Technologies Jdalfors@aol.com 888-884-7828 Limit

### Determination of challenging elements in ultrapure semiconductor grade sulfuric acid by Triple Quadrupole ICP-MS

Determination of challenging elements in ultrapure semiconductor grade sulfuric acid by Triple Quadrupole ICP-MS Application note Semiconductor Authors Junichi Takahashi Agilent Technologies, Japan Introduction

### Analysis of Sulfuric Acid Using a Single Set of Operating Conditions with HR-ICP-MS

APPLICATION NOTE Analysis of Sulfuric Acid Using a Single Set of Operating Conditions with HR-ICP-MS No 30105 Julian D Wills, Torsten Lindemann, Thermo Fisher Scientific, Bremen, Germany Key Words Mineral

### 4.2 Bias, Standards and Standardization

4.2 Bias, Standards and Standardization bias and accuracy, estimation of bias origin of bias and the uncertainty in reference values quantifying by mass, chemical reactions, and physical methods standard

### Analytical Method Validation

Analytical Method Validation A. Es-haghi Ph.D. Dept. of Physico chemistry vaccine and serum research institute a.eshaghi@rvsri.ir http://www.rvsri.ir/ Introduction Test procedures for assessment of the

### VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND METHODOLOGY Q2(R1)

INTERNATIONAL CONFERENCE ON HARMONISATION OF TECHNICAL REQUIREMENTS FOR REGISTRATION OF PHARMACEUTICALS FOR HUMAN USE ICH HARMONISED TRIPARTITE GUIDELINE VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND METHODOLOGY

### Mass Spectrometry Signal Calibration for Protein Quantitation

Cambridge Isotope Laboratories, Inc. www.isotope.com Proteomics Mass Spectrometry Signal Calibration for Protein Quantitation Michael J. MacCoss, PhD Associate Professor of Genome Sciences University of

### Environmental Water Testing: Surface Water, Groundwater, Hard Water, Wastewater, & Seawater

Document: AND Sol Env 08 2013 Environmental Water Testing: Surface Water, Groundwater, Hard Water, Wastewater, & Seawater Matrix specific sample preparation and testing methods for environmental waters

### Mass spectrometry. What are the principles behind MS? What do all MS instruments have in common?

Mass spectrometry What are the principles behind MS? What do all MS instruments have in common? What are the different types of MS? Lecture outline: 1) Introduction to mass spectrometry 2) sample introduction

### Guidance for Industry

Guidance for Industry Q2B Validation of Analytical Procedures: Methodology November 1996 ICH Guidance for Industry Q2B Validation of Analytical Procedures: Methodology Additional copies are available from:

### Introduction to method validation

Introduction to method validation Introduction to method validation What is method validation? Method validation provides documented objective evidence that a method measures what it is intended to measure,

### Analysis of Pharmaceutical Products for their Elemental Impurities with the Thermo Scientific icap RQ ICP-MS

Analysis of Pharmaceutical Products for their al Impurities with the Thermo Scientific icap RQ ICP-MS Julian Wills and Daniel Kutscher Thermo Fisher Scientific, Bremen, Germany Application Note 43325 Key

### TEST REPORT: SIEVERS M-SERIES PERFORMANCE SPECIFICATIONS

TEST REPORT: SIEVERS M-SERIES PERFORMANCE SPECIFICATIONS. PURPOSE The purpose of this report is to verify the performance characteristics of the Sievers M-Series TOC Analyzers. Performance was quantified

### METHOD 9075 TEST METHOD FOR TOTAL CHLORINE IN NEW AND USED PETROLEUM PRODUCTS BY X-RAY FLUORESCENCE SPECTROMETRY (XRF)

METHOD 9075 TEST METHOD FOR TOTAL CHLORINE IN NEW AND USED PETROLEUM PRODUCTS BY X-RAY FLUORESCENCE SPECTROMETRY (XRF) 1.0 SCOPE AND APPLICATION 1.1 This test method covers the determination of total chlorine

### Analytical Method Validation for Assay, Related substances & Dissolution. N A Y A N K S H A T R I 1 8 / 0 1 /

Analytical Method Validation for Assay, Related substances & Dissolution. N A Y A N K S H A T R I 1 8 / 0 1 / 2 0 1 3 Definitions The objective of validation of an analytical procedure is to demonstrate

### Ultra-low level determination of phosphorus, sulfur, silicon and chlorine using the Agilent 8900 ICP-QQQ

Ultra-low level determination of phosphorus, sulfur, silicon and chlorine using the Agilent 8900 ICP-QQQ Application note Semiconductor Author Kazumi Nakano, Agilent Technologies, Japan Introduction Quadrupole

### ICH Topic Q 2 (R1) Validation of Analytical Procedures: Text and Methodology. Step 5

European Medicines Agency June 1995 CPMP/ICH/381/95 ICH Topic Q 2 (R1) Validation of Analytical Procedures: Text and Methodology Step 5 NOTE FOR GUIDANCE ON VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND

### Standard Operation Procedure. Elemental Analysis of Solution samples with Inductively Coupled Plasma Mass Spectrometry

Standard Operation Procedure Elemental Analysis of Solution samples with Inductively Coupled Plasma Mass Spectrometry Soil & Plant Analysis Laboratory University of Wisconsin Madison http://uwlab.soils.wisc.edu

### Analysis of Riboflavin in a Vitamin Pill by Fluorescence Spectroscopy

Analysis of Riboflavin in a Vitamin Pill by Fluorescence Spectroscopy Objectives In this lab, you will use fluorescence spectroscopy to determine the mass of riboflavin in a vitamin pill. Riboflavin fluorescence

### ANALYSIS OF TRACE LEVEL OF HEAVY METALS IN NOODLES AND FLAVOR SACHET USING THE AGILENT 7900 ICP-MS

FOOD ANALYSIS ANALYSIS OF TRACE LEVEL OF HEAVY METALS IN NOODLES AND FLAVOR SACHET USING THE AGILENT 7900 ICP-MS Solutions for Your Analytical Business Markets and Applications Programs Authors Gaurav

### PRINSIP FISIOLOGIS BERBAGAI MACAM ESAI HORMON

PRINSIP FISIOLOGIS BERBAGAI MACAM ESAI HORMON Kuliah 4 Rahmatina B. Herman Bagian Fisiologi Fakultas Kedokteran Universitas Andalas Hormones 1. Hormones are chemical messengers that enter the blood, which

### Understanding Analytical Chemistry (Weighing, Mixing, Measuring and Evaluating)

Name: Date: Understanding Analytical Chemistry (Weighing, Mixing, Measuring and Evaluating) High School Environmental Science AP Module 1 Environmental Lab NGSSS Big Ideas: This module is a laboratory-based

### NANOCOMPOSIX'S GUIDE TO ICP-MS MEASUREMENT

NANOCOMPOSIX'S GUIDE TO ICP-MS MEASUREMENT AND ANALYSIS SEPTEMBER 2012, V 1.1 4878 RONSON CT STE K SAN DIEGO, CA 92111 858-565 - 4227 NANOCOMPOSIX.COM Note to the Reader: We at nanocomposix have published

### Method Validation. Ross Molinaro, PhD, MT(ASCP), DABCC, FACB Emory University Atlanta, GA

Method Validation Ross Molinaro, PhD, MT(ASCP), DABCC, FACB Emory University Atlanta, GA Learning Objectives After this presentation, you should be able to: 1. Define method evaluation. 2. List the steps

### UNITED STATES CONSUMER PRODUCT SAFETY COMMISSION DIRECTORATE FOR LABORATORY SCIENCES DIVISION OF CHEMISTRY 5 RESEARCH PLACE ROCKVILLE, MD 20850

UNITED STATES CONSUMER PRODUCT SAFETY COMMISSION DIRECTORATE FOR LABORATORY SCIENCES DIVISION OF CHEMISTRY 5 RESEARCH PLACE ROCKVILLE, MD 20850 Test Method: CPSC-CH-E1001-08.2 Standard Operating Procedure

### Validation and Calibration. Definitions and Terminology

Validation and Calibration Definitions and Terminology ACCEPTANCE CRITERIA: The specifications and acceptance/rejection criteria, such as acceptable quality level and unacceptable quality level, with an

### ASSURING THE QUALITY OF TEST RESULTS

Page 1 of 12 Sections Included in this Document and Change History 1. Purpose 2. Scope 3. Responsibilities 4. Background 5. References 6. Procedure/(6. B changed Division of Field Science and DFS to Office

### Determination of Impurities in Semiconductor-Grade Nitric Acid with the NexION 300S/350S ICP-MS

APPLICATION NOTE ICP - Mass Spectrometry Author Kenneth Ong PerkinElmer, Inc. Singapore Determination of Impurities in Semiconductor-Grade Nitric Acid with the NexION 300S/350S ICP-MS Introduction Semiconductor

### Radiometric Dating and Lead Isotopes Lab

Radiometric Dating and Lead Isotopes Lab To instructors While quadrupole ICP-MS is not the best way to do radiometric dating, it can be done to limited precision with relatively little trouble for the

### Lead Testing and On Site Calibration for Water Testing Detection Range: 2 100ppb

Document: AND Lead 100 7 2013 Lead Testing and On Site Calibration for Water Testing Detection Range: 2 100ppb July, 2013 Edition 1 ANDalyze, Inc., 2012. All rights reserved. Printed in USA. Table of Contents

### Analysis of Riboflavin in a Vitamin Pill by Fluorescence Spectroscopy**

Analysis of Riboflavin in a Vitamin Pill by Fluorescence Spectroscopy** Objectives In this lab, you will use fluorescence spectroscopy to determine the mass and percentage of riboflavin in a vitamin pill.

### NUTC R304. Use of Absorption Mechanisms to Decrease Heavy Metal Mobility

Use of Absorption Mechanisms to Decrease Heavy Metal Mobility by Jianmin Wang Honglan Shi Joe G. Burken NUTC R304 A National University Transportation Center at Missouri University of Science and Technology

### Quantitative work in HPLC

Quantitative work in HPLC Dr. Shulamit Levin Medtechnica www.forumsci.co.il/hplc Dr. Shulamit Levin, Medtechnica 1 Quantitative work in HPLC Dr. Shulamit Levin Medtechnica Data Handling Analytical Chemistry

### ACID-BASE TITRATIONS: DETERMINATION OF CARBONATE BY TITRATION WITH HYDROCHLORIC ACID BACKGROUND

#3. Acid - Base Titrations 27 EXPERIMENT 3. ACID-BASE TITRATIONS: DETERMINATION OF CARBONATE BY TITRATION WITH HYDROCHLORIC ACID BACKGROUND Carbonate Equilibria In this experiment a solution of hydrochloric

### An example: helium isotopes. An example: helium isotopes. Limits to Detection/Measurement. Lecture 14 Measurements II: Mass spectrometry

Limits to Detection/Measurement Ionization is fundamentally a Probabilistic Process Just like radioactive decay So is transmission through the analyzer There is an intrinsic statistical uncertainty Proportional

### Analysis of Vanadium, Nickel, Sodium, and Iron in Fuel Oils using Flame Atomic Absorption Spectrophotometry

application Note Atomic Absorption Author Stan Smith PerkinElmer, Inc. Shelton, CT 06484 USA Analysis of Vanadium, Nickel, Sodium, and Iron in Fuel Oils using Flame Atomic Absorption Spectrophotometry

### Multi-elemental determination of gasoline using Agilent 5100 ICP-OES with oxygen injection and a temperature controlled spray chamber

Multi-elemental determination of gasoline using Agilent 5100 ICP-OES with oxygen injection and a temperature controlled spray chamber Application note Energy & chemicals, petrochemicals Authors Elizabeth

### 2008 USPC Official 12/1/07-4/30/08 General Chapters: <1225> VALIDATION OF C...Page 1 of 10

2008 USPC Official 12/1/07-4/30/08 General Chapters: VALIDATION OF C...Page 1 of 10 1225 VALIDATION OF COMPENDIAL PROCEDURES Test procedures for assessment of the quality levels of pharmaceutical

### Quantitation of Drugs in Dried Bloodstains. Thomas Meyer Anna Gomenyuk Nadiah Lester

Quantitation of Drugs in Dried Bloodstains Thomas Meyer Anna Gomenyuk Nadiah Lester Objective To find the quantitative value of drugs in dried bloodstains Currently Cloth With Dried Bloodstain Containing

### High Precision Isotope Ratio Measurements of Sr, Nd and Hf

Application Note: 30158 High Precision Isotope Ratio Measurements of, and Key Words NEPTUNE Multicollector ICP-MS Hafnium Neodymium Strontium Introduction Multicollector-ICP-MS has been established as

### Application of ICP-MS as a Tool for Environmental Monitoring. Bill Spence Environmental Market Specialist

Application of ICP-MS as a Tool for Environmental Monitoring Bill Spence Environmental Market Specialist Introduction Knowledge of the concentration of metallic species in the environment has been important

### The Determination of the Quinine Content of Water- Lab Report

The Determination of the Quinine Content of Water- Lab Report Introduction This experiment aims to use a UV-Vis spectrophotometer to analyse the amount of quinine in tonic water, and study the effects

### Analytical method Validation: ICP-OES

Electronic Supplementary Material (ESI) for Journal of Analytical Atomic Spectrometry. This journal is The Royal Society of Chemistry 2015 Prepared by Jonathan Fitzsimmons Analytical method Validation:

### Analysis of Testosterone in Serum using LC/Triple Quadrupole MS/MS

Analysis of Testosterone in Serum using LC/Triple Quadrupole MS/MS Application Note Authors M.P. George Agilent Technologies, Inc. Santa Clara, CA USA Andre Szczesniewski Agilent Technologies, Inc. Schaumburg,

### Signal, Noise, and Detection Limits in Mass Spectrometry

Signal, Noise, and Detection Limits in Mass Spectrometry Technical Note Chemical Analysis Group Authors Greg Wells, Harry Prest, and Charles William Russ IV, Agilent Technologies, Inc. 2850 Centerville

### Method Validation/Verification. CAP/CLIA regulated methods at Texas Department of State Health Services Laboratory

Method Validation/Verification CAP/CLIA regulated methods at Texas Department of State Health Services Laboratory References Westgard J. O.: Basic Method Validation, Westgard Quality Corporation Sarewitz

### Introduction. The following definitions may help you better understand the components of the data report.

Introduction This document is designed to help our clients understand the quality control requirements and limitations of data reporting. There are three sections to this document. The first section will

### Elemental Analyses by ICP-AES

Elemental Analyses by ICP-AES Henry Gong, Senior Analytical Chemist September 10, 2008 ICP-AES inductively coupled plasma atomic emission spectrophotometry Electrons of an atom absorb energy and jump to

### Ecology Quality Assurance Glossary

Ecology Quality Assurance Glossary Edited by William Kammin, Ecology Quality Assurance Officer Accreditation - A certification process for laboratories, designed to evaluate and document a lab s ability

### Copper, atomic absorption spectrophotometry, graphite furnace

1. Application Copper, atomic absorption spectrophotometry, graphite furnace Parameters and Codes: Copper, dissolved, I-2274-89 (µg/l as Cu): 01040 Copper, whole water recoverable, I-4274-89 (µg/l as Cu):

### Content Sheet 7-1: Overview of Quality Control for Quantitative Tests

Content Sheet 7-1: Overview of Quality Control for Quantitative Tests Role in quality management system Quality Control (QC) is a component of process control, and is a major element of the quality management

### HS 1003 Part 2 HS 1003 Heavy Metals Test

HS 1003 Heavy Metals Test 1. Purpose This test method is used to analyse the heavy metal content in an aliquot portion of stabilised hot acetic acid extract by Atomic Absorption Spectroscopy (AAS). Note:

### To avoid potential inspection

Good Analytical Method Validation Practice Deriving Acceptance for the AMV Protocol: Part II To avoid potential inspection observations for test method validations by the regulatory agencies, it has become

### Determination of trace elements in ultrapure semiconductor grade sulfuric acid using the Agilent 8900 ICP-QQQ in MS/MS mode

Determination of trace elements in ultrapure semiconductor grade sulfuric acid using the Agilent 8900 ICP-QQQ in MS/MS mode Application note Semiconductor Authors Michiko Yamanaka, Kazuo Yamanaka and Naoki

### Absolute and Relative Gas Concentration: Understanding Oxygen in Air. Bruce Bugbee and Mark Blonquist

Absolute and Relative Gas Concentration: Understanding Oxygen in Air Bruce Bugbee and Mark Blonquist Absolute and Relative Gas Concentration Gas concentration is described in two ways, absolute and relative

### EL-V1M Rev0.1: Chemical Testing Working Draft Standard; Sections and (Calibration) June 2012 page 1 of 5

page 1 of 5 1.7 Technical Requirements 1.7.1 Initial Calibration 1.7.1.1 Instrument Calibration This module specifies the essential elements that shall define the procedures and documentation for initial

### Experiment 10. Radioactive Decay of 220 Rn and 232 Th Physics 2150 Experiment No. 10 University of Colorado

1 Radioactive Decay of 220 Rn and 232 Th Physics 2150 Experiment No. 10 University of Colorado Introduction Some radioactive isotopes formed billions of years ago have half- lives so long that they are

### Chemistry 321, Experiment 8: Quantitation of caffeine from a beverage using gas chromatography

Chemistry 321, Experiment 8: Quantitation of caffeine from a beverage using gas chromatography INTRODUCTION The analysis of soft drinks for caffeine was able to be performed using UV-Vis. The complex sample

### KINETIC DETERMINATION OF SELENIUM BY VISIBLE SPECTROSCOPY (VERSION 1.8)

Selenium Determination, Page 1 KINETIC DETERMINATION OF SELENIUM BY VISIBLE SPECTROSCOPY I. BACKGROUND. (VERSION 1.8) The majority of reactions used in analytical chemistry possess the following characteristics:

### Quality Assurance/Quality Control in Acid Deposition Monitoring

Quality Assurance/Quality Control in Acid Deposition Monitoring Acid Deposition and Oxidant Research Center (Network Center of EANET) Introduction Wet deposition data are used for -assessments of spatial

### Equations and Inequalities

Rational Equations Overview of Objectives, students should be able to: 1. Solve rational equations with variables in the denominators.. Recognize identities, conditional equations, and inconsistent equations.

### The Determination of Low Levels of Benzene, Toluene, Ethylbenzene, Xylenes and Styrene in Olive Oil Using a Turbomatrix HS and a Clarus SQ 8 GC/MS

application Note Gas Chromatography/ Mass Spectrometry Author A. Tipler, Senior Scientist PerkinElmer, Inc. Shelton, CT 06484 USA The Determination of Low Levels of Benzene, Toluene, Ethylbenzene, Xylenes

### Karolina Carpenter, Applications Chemist; Teledyne Leeman Labs Page 1

Application Note - AN1606 Determination of Heavy Metals in Reagent Chemicals Using the Teledyne Leeman Lab s Prodigy7 ICP-OES Following Procedures Developed by the ACS Committee Karolina Carpenter, Applications

### Development of Headspace Gas Chromatography-Mass Spectrometry for Determination of Residual Monomer in Polymer Latex

Journal of Metals, Materials and Minerals, Vol.20 No.3 pp.145-149, 2010 Development of Headspace Gas Chromatography-Mass Spectrometry for Determination of Residual Monomer in Polymer Latex Nopparat THAWEEWATTHANANON

### GUIDELINE FOR THE ACCREDITATION OF LABORATORIES TESTING FOR GENETICALLY MODIFIED ORGANISMS (GMO)

GUIDELINE FOR THE ACCREDITATION OF LABORATORIES TESTING FOR GENETICALLY MODIFIED ORGANISMS (GMO) ESYD G-GMO/01/00/20-10-2016 1/9 ESYD G-GMO Issue: 01 Revision: 00 Issue Date: 20-10-2016 Revision Date:

### Determination of mercury in aqua regia and nitric acid digests with cold-vapour atomic spectrometry or cold-vapour atomic fluorescence spectrometry

Determination of mercury in aqua regia and nitric acid digests with cold-vapour atomic spectrometry or cold-vapour atomic fluorescence spectrometry 1 Scope This horizontal standard specifies a method for

### Limit of detection, limit of quantification and limit of blank

Eurachem A FOCUS FOR ANALYTICAL CHEMISTRY IN EUROPE Limit of detection, limit of quantification and limit of blank Elvar Theodorsson LoB, LoD, LoQ Limit of blank (LoB), limit of decision, limit of detection

### Method validation and quality control procedures

Method validation and quality control procedures Department of Food Chemistry and Analysis, ICT Prague Vladimír Kocourek Prague, 2012 WHAT IS VALIDATION? Validation is a process, within which the method

### Colorimetric Determination of Iron in Vitamin Tablets

Cautions: 6 M hydrochloric acid is corrosive. Purpose: To colorimetrically determine the mass of iron present in commercial vitamin tablets using a prepared calibration curve. Introduction: Iron is considered

### The Analysis of Drinking Waters by U.S. EPA Method Using the NexION 300D/350D ICP-MS in Standard, Collision and Reaction Modes

APPLICATION NOTE ICP - Mass Spectrometry Authors Ewa Pruszkowski, Ph.D. Senior ICP-MS Application Scientist Cynthia P. Bosnak Senior Product Specialist PerkinElmer, Inc. Shelton, CT USA The Analysis of

### Ordered Pairs. Graphing Lines and Linear Inequalities, Solving System of Linear Equations. Cartesian Coordinates System.

Ordered Pairs Graphing Lines and Linear Inequalities, Solving System of Linear Equations Peter Lo All equations in two variables, such as y = mx + c, is satisfied only if we find a value of x and a value

### DETERMINATION OF CHLORINATED HYDROCARBON CONCENTRATIONS IN SOIL USING A TOTAL ORGANIC HALOGEN METHOD

DTR-17-01 1 DETERMINATION OF CHLORINATED HYDROCARBON CONCENTRATIONS IN SOIL USING A TOTAL ORGANIC HALOGEN METHOD T.B. Lynn, J.C. Kneece, B.J. Meyer, A.C. Lynn, Dexsil Corporation, Hamden, Connecticut Presented

### SPIKE RECOVERY AND DETERMINING A METHOD DETECTION LIMIT Pamela Doolittle, University of Wisconsin Madison, pssemrad@wisc.edu 2014

SPIKE RECOVERY AND DETERMINING A METHOD DETECTION LIMIT Pamela Doolittle, University of Wisconsin Madison, pssemrad@wisc.edu 2014 This experiment explores quality assurance practices which are commonly

### What is ICP-MS? and more importantly, what can it do?

What is ICP-MS? and more importantly, what can it do? Inductively Coupled Plasma Mass Spectrometry or ICP-MS is an analytical technique used for elemental determinations. The technique was commercially

### Separation and Determination of Liposomal and Non-Liposomal (Free) Doxorubicin from Human Plasma by SPE and LC-MS/MS

Separation and Determination of Liposomal and Non-Liposomal (Free) from Human Plasma by SPE and LC-MS/MS Krishna Rao Dara, Dr. Tushar N. Mehta, Tim Liddicoat, Asia Pacific Center of Excellence, Thermo

### Sodium Chloride - Analytical Standard

Sodium Chloride - Analytical Standard Determination of Calcium and Magnesium Former numbering: ECSS/CN 185-1979 & ESPA/CN-E-114-1998 www.eu.com 1. SCOPE AND FIELD OF APPLICATION The present EuSalt Analytical

### Chemistry 1215 Experiment #10 The Reaction of Zinc and Iodine: The Combination of Two Elements

Chemistry 1215 Experiment #10 The Reaction of Zinc and Iodine: The Combination of Two Elements Objective The objective of this experiment is to perform a combination reaction by reacting elemental zinc

### RayBio Human Fibronectin ELISA Kit

RayBio Human Fibronectin ELISA Kit Catalog #: ELH-FN1 User Manual Last revised April 15, 2016 Caution: Extraordinarily useful information enclosed ISO 13485 Certified 3607 Parkway Lane, Suite 100 Norcross,

### Determination of Lead and Cadmium in Foods by Graphite Furnace Atomic Absorption Spectroscopy

APPLICATION NOTE Atomic Absorption Author: Kenneth Ong PerkinElmer, Inc. Shelton, CT Determination of Lead and Cadmium in Foods by Graphite Furnace Atomic Absorption Spectroscopy Background Humans can

### Calcium Analysis by Atomic Absorption

Calcium Analysis by Atomic Absorption In this experiment, your unknown calcium solution from last week's experiment will be analyzed for calcium by atomic absorption analysis and the results compared with

### Upper left: typical dark blue fecal coliform colonies on a membrane filter after incubation on M-FC agar. Lower center (purple): M-FC agar before

KIMIA ANALISA 3 SKS Prof. Dr. Heru Setyawan Jurusan Teknik Kimia FTI ITS The Language of Analytical Chemistry Analysis, Determination, and Measurement Analysis: A process that provides chemical or physical

### The Empirical Formula of a Compound

The Empirical Formula of a Compound Lab #5 Introduction A look at the mass relationships in chemistry reveals little order or sense. The ratio of the masses of the elements in a compound, while constant,

### Systems of Linear Equations - Introduction

Systems of Linear Equations - Introduction What are Systems of Linear Equations Use an Example of a system of linear equations If we have two linear equations, y = x + 2 and y = 3x 6, can these two equations

### USING CLSI GUIDELINES TO PERFORM METHOD EVALUATION STUDIES IN YOUR LABORATORY

USING CLSI GUIDELINES TO PERFORM METHOD EVALUATION STUDIES IN YOUR LABORATORY Breakout Session 3B Tuesday, May 1 8:30 10 am James Blackwood, MS, CLSI David D. Koch, PhD, FACB, DABCC, Pathology & Laboratory

### Evaluating Laboratory Data. Tom Frick Environmental Assessment Section Bureau of Laboratories

Evaluating Laboratory Data Tom Frick Environmental Assessment Section Bureau of Laboratories Overview of Presentation Lab operations review QA requirements MDLs/ PQLs Why do we sample? Protect physical,

### A New Approach for Nitrate Cadmium Reduction by Discrete Analysis NO 3. Application Note

A New Approach for Nitrate Cadmium Reduction by Discrete Analysis Application Note 25380206 Keywords Cadmium Reduction DA 3500 Discrete Analysis Nitrate Nitrogen Nitrite Nitrogen Abstract The discrete

### ATOMIC ABSORTION SPECTROSCOPY: rev. 4/2011 ANALYSIS OF COPPER IN FOOD AND VITAMINS

1 ATOMIC ABSORTION SPECTROSCOPY: rev. 4/2011 ANALYSIS OF COPPER IN FOOD AND VITAMINS Buck Scientific Atomic Absorption Spectrophotometer, Model 200 Atomic absorption spectroscopy (AAS) has for many years

### Lab #11: Determination of a Chemical Equilibrium Constant

Lab #11: Determination of a Chemical Equilibrium Constant Objectives: 1. Determine the equilibrium constant of the formation of the thiocyanatoiron (III) ions. 2. Understand the application of using a

### Application Note. Authors. Abstract. Na Pi Parra, Yanan Yang, Lisa Zang Agilent Technologies, Inc. Santa Clara, CA, USA

Quantitative Analysis of Underivatized Glutamine, Glutamic Acid, Asparagine, and Aspartic Acid in Cell Media using Agilent 66 Triple Quadrupole LC/MS Application Note Authors Na Pi Parra, Yanan Yang, Lisa

### RayBio Human ADAM9 ELISA Kit

RayBio Human ADAM9 ELISA Kit Catalog #: ELH-ADAM9 User Manual Last revised April 15, 2016 Caution: Extraordinarily useful information enclosed ISO 13485 Certified 3607 Parkway Lane, Suite 100 Norcross,

### Chemistry 111 Laboratory Experiment 7: Determination of Reaction Stoichiometry and Chemical Equilibrium

Chemistry 111 Laboratory Experiment 7: Determination of Reaction Stoichiometry and Chemical Equilibrium Introduction The word equilibrium suggests balance or stability. The fact that a chemical reaction

### ACETALDEHYDE and ISOVALERALDEHYDE (Gas Chromatography)

ACETA.02-1 ACETALDEHYDE and ISOVALERALDEHYDE (Gas Chromatography) PRINCIPLE Isovaleraldehyde (IVA) and acetaldehyde are released from the syrup with the aid of dilute phosphoric acid and heat. The liberated

### Measurement and Calibration

Purpose To gain an understanding of the relationships that exist between density, mass, and volume while calibrating laboratory glassware. Introduction Measurement is a regular part of life. For example,

### 1.1 This test method covers the qualitative and quantitative determination of the content of benzene and toluene in hydrocarbon wax.

Standard Method for Analysis of Benzene and Toluene Content in Hydrocarbon Waxes by Headspace Gas Chromatography EWF METHOD 002/03 (Version 1 Reviewed 2015) 1 Scope 1.1 This test method covers the qualitative

### Austin Peay State University Department of Chemistry CHEM The Use of the Spectrophotometer and Beer's Law

Caution Potassium permanganate solution is a skin irritant and may stain skin and clothing. Purpose To become familiar with using a spectrophotometer and gain an understanding of Beer s law and its relationship

### HRMS in Clinical Research: from Targeted Quantification to Metabolomics

A sponsored whitepaper. HRMS in Clinical Research: from Targeted Quantification to Metabolomics By: Bertrand Rochat Ph. D., Research Project Leader, Faculté de Biologie et de Médecine of the Centre Hospitalier

### The Analysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300Q/350Q ICP-MS in Standard Mode

APPLICATION NOTE ICP - Mass Spectrometry Authors Ewa Pruszkowski, Ph.D. Senior ICP-MS Application Scientist Cynthia P. Bosnak Senior Product Specialist PerkinElmer, Inc. Shelton, CT USA The Analysis of