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Handbook for Process Safety in Laboratories and Pilot Plants Effectively manage physical and chemical risks in your laboratory or pilot plant In Handbook for Process Safety in Laboratories and Pilot Plants: A Risk-based Approach, the Center for Chemical Process Safety delivers a comprehensive and authoritative presentation of process safety procedures and methods for use in laboratories and pilot plants (LAPPs). Of the four broad hazard categories -- chemical, physical, biological, and ionizing radiation -- this book focuses on the two most common: chemical and physical hazards. It addresses the storage and handling of the hazardous materials associated with activities commonly performed in LAPPs and presents many of the physical and chemical analytical techniques used to verify and validate the efficacy of safety management systems. This book will present tools and techniques for effectively managing the risks in any laboratory or pilot plant using engineered and administrative controls, as well as the CCPS Risk Based Process Safety (RBPS) Management Systems. Readers will also find: * A thorough introduction to process safety * Comprehensive explorations of understanding hazards and risks, as well as managing risk with engineered controls, administrative controls, and RBPS Management Systems * Practical discussions of how to learn from the experiences of your own LAPP and others * Detailed case reports and examples, as well as practical tools, control banding strategies, and glass equipment design Perfect for any LAPP staff member working with or managing hazardous materials, Handbook for Process Safety in Laboratories and Pilot Plants: A Risk-based Approach will also benefit LAPP engineering and scientific professionals, LAPP technical support staff, and LAPP managers. The Center for Chemical Process Safety is a world leader in developing and distributing information on process safety management and technology. Since 1985, CCPS has published over 100 books in its process safety guidelines and concept series, 33 training modules as part of its Safety in Chemical Engineering Education series, and over 220 online offerings.

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Table of Contents

Cover

Table of Contents

Title Page

Copyright

List of Figures

List of Tables

Abbreviations and Acronyms

Glossary

Acknowledgments

Dedication

Online Materials Accompanying this Handbook

Preface

Part 1 – Introduction and Overview

1 Purpose and Scope

1.1 Purpose

1.2 Scope of Book and Target Audience

1.3 Terms for Laboratories and Pilot Plants

1.4 Distinctions between Laboratories and Pilot Plants

1.5 Organization of This Handbook

2 Managing Risk to Prevent Incidents

2.1 Some LAPP Characteristics

2.2 Safety in Laboratories and Pilot Plants

2.3 Where to Start with a Risk‐based Approach in the LAPP

2.4 Gain Leadership Support to Implement Risk Based Process Safety

2.5 Laboratory Safety Management System Considerations

2.6 Resources for Risk Based Process Safety Management System

3 Leaks and Spills in the LAPP

3.1 Leaks of Hazardous Materials

3.2 Spills of Hazardous Materials

Part 2 – Committing to Process Safety

4 LAPP Risk Management Concepts

4.1 Occupational Safety and Process Safety

4.2 Hierarchy of Controls

4.3 Inherently Safer Design (ISD)

4.4 Basic Risk Concepts

4.5 A Risk Management Program

4.6 Anatomy of an Incident

4.7 Preventive and Mitigative Safeguards

4.8 Applying a Risk‐Based Approach in a LAPP

5 Process Safety Culture in the LAPP

5.1 RBPS Element 1: Process Safety Culture

5.2 Leaders’ Responsibilities for Positive Safety Culture

5.3 Resources and Examples for Process Safety Culture

6 Standards for the LAPP

6.1 RBPS Element 2: Compliance with Standards

6.2 Risk Management Focus

6.3 Different Codes and Standards When Scaling Up from Laboratory to Pilot Plant

6.4 Jurisdictional Requirements

6.5 Resources for Compliance with Standards

7 Process Safety Competency and Training in the LAPP

7.1 RBPS Element 3: Process Safety Competency

7.2 RBPS Element 12: Training and Performance Assurance

8 Workforce Involvement and Stakeholder Outreach in the LAPP

8.1 RBPS Element 4: Workforce Involvement

8.2 RBPS Element 5: Stakeholder Outreach

Part 3 – Understanding Hazards and Risks

9 Process Safety Knowledge Management in the LAPP

9.1 RBPS Element 6: Process Knowledge Management

9.2 Overview of Information and Data Needs

9.3 Sources of Information and Data

9.4 Process Safety Information during Scale‐up

10 Types of Hazards

10.1 Reactive Chemistry Hazards

10.2 Toxicity Hazards

10.3 Flammability and Combustibility Hazards

10.4 Temperature Hazards

10.5 Overpressure Hazards

10.6 Other Common LAPP Hazards

11 Hazard Identification and Risk Analysis (HIRA) in the LAPP

11.1 RBPS Element 7: Hazard Identification and Risk Analysis

11.2 HIRA Team Members

11.3 HIRA Approaches Used in LAPPs

11.4 Qualitative versus Quantitative Analysis of Risks in LAPPs

11.5 ACS Hazard Analysis Tools

11.6 Evaluating the Effort Level for HIRAs

11.7 Determining the Extent of the HIRAs

Part 4 – Managing Risk: Engineered Controls

12 Spill and Leak Protection

12.1 Containment

12.2 Flexible hose and tubing

13 Fire and Over‐Temperature Protection

13.1 Fire Prevention

13.2 Fire Mitigation

13.3 Over‐Temperature Protection

14 Overpressure Prevention and Protection

14.1 Pressure Protection for Equipment

14.2 Pressure and Vacuum Relief for Atmospheric Pressure Vessels

14.3 Process Conditions/Situations to Consider in Pressure Relief Device Design

14.4 Blast Containment Cells and Pressure Relief for Building Areas

14.5 Venting Location and Downstream Treatment of Material Vented

15 Ventilation Controls

15.1 Ventilation Systems

15.2 Laboratory Chemical Fume Hoods

15.3 Pilot Plant Ventilation

15.4 Permanent Total Enclosures for Containment in the LAPP

16 Automated Shut‐down Systems

16.1 Selection and Design Based on Hazard Identification and Risk Analysis

16.2 Basic Control Systems and Safety Shut‐down Systems

16.3 Independent Automated Safety Shut‐down Systems

16.4 Fail‐Safe Design Considerations

16.5 Important Design Features for Control Systems

16.6 Control of Changes and Maintenance for Engineered Safeguards

16.7 Additional References

17 Engineered Controls for Common Hazards

17.1 Cryogenic Fluids and Compressed Gases

17.2 Cryogenic Fluids and Compressed Gas Cylinders

17.3 Glass Equipment

17.4 Gloveboxes

Part 5 – Managing Risk: Administrative Controls

18 Administrative Fire and Explosion Safeguards

18.1 Standards and Guidance for Fire Prevention

18.2 Ignition Source Control: Procedures

18.3 Manual Fire Suppression

19 Administrative Safeguards for Hazards in LAPPs

19.1. Good Practices for Compressed Gas and Cryogenic Cylinders

19.2 Regulations and Standards for Compressed Gases and Cryogenic Fluids

19.3 Procedures and Best Practices for Compressed Gases

19.4 Good Practices for Storage, Movement, and Use of Cryogenic Fluids

19.5 Good Practices For Handling Glass

19.6 Administrative Controls for Reactive Hazards

Part 6 – Managing Risk: RBPS Management Systems

20 Operating Procedures and Conduct of Operations in the LAPP

20.1 RBPS Element 8: LAPP Operating Procedures

20.2 RBPS Element 15: Conduct of Operations

21 Safe Work Practices and Contractor Management in the LAPP

21.1 RBPS Element 9: Safe Work Practices

21.2 RBPS Element 11: Contractor Management

22 Asset Integrity and Reliability in the LAPP

22.1 RBPS Element 10: Asset Integrity and Reliability

22.2 A Management Approach for Assuring Asset Integrity and Reliability

22.3 Examples of Asset Integrity and Reliability Management System Failures

22.4 Glass Equipment—Asset Integrity and Reliability Challenge for LAPPs

23 Management of Change (MOC) and Operational Readiness in the LAPP

23.1 RBPS Element 13: Management of Change

23.2 RBPS Element 14: Operational Readiness

24 Emergency Management in the LAPP

24.1 RBPS Element 16: Emergency Management

24.2 Emergency Planning

24.3 Implementing an Emergency Management Plan

24.4 Emergency Equipment

24.5 Training and Drills

24.6 Deficiencies in Emergency Planning and Response in LAPP Cases

24.7 Controlling Unattended Experimental Work and Working Alone in LAPPs

Part 7 – Learning from Experience

25 Investigating Incidents

25.1 Incident Terminology

25.2 Incident Investigation

25.3 Steps of an Incident Investigation

25.4 Ensure Lessons Are Learned and Remembered

25.5 Learn from Experience of Others

26 Metrics, Auditing, and Management Review in the LAPP

26.1 RBPS Element 18: Measurement and Metrics

26.2 RBPS Element 19: Auditing

26.3 RBPS Element 20: Management Review and Continuous Improvement

Part 8 – Conclusion

References

Appendix A: Cases

Appendix B: Examples

Appendix C: Control Banding Strategies

C.1. Laboratory Fire Hazard Ratings

C.2. Laboratory Chemical Safety Level (CSL) Ratings

C.3. Toxicity Hazard Ratings

C.4. Biosafety Level Ratings

C.5. Other Hazards in Biological Research Labs

Appendix D: Glass Equipment Design

D.1. Glass Equipment Integrity Challenges

D.2. General Glass Properties and Performance Characteristics

Index

End User License Agreement

List of Tables

Chapter 1

Table 1-1 Framework for this Handbook

Table 1-2 The CCPS Risk Based Process Safety (RBPS) Management System

Chapter 2

Table 2-1 Fatal Incidents in LAPPs Resulting from Fires and Explosions

Table 2-2 Fatal Incidents in LAPPs Resulting from Exposure to Toxic Chemica...

Table 2-3 Fatal Incidents in LAPPs Resulting from Exposure to Biological Ag...

Table 2-4 Fatal Incidents in LAPPs Resulting from Other Causes

Table 2-5 Fire Losses in Laboratory Buildings

Table 2-6 Comparison of LAPP Activities to the RBPS Elements

Table 2-7 Leader Accountabilities for Process Safety

Chapter 4

Table 4-1 Description of Inherently Safer Design Strategies

Table 4-2 Argonne NL WPC Process Compared to the CCPS RBPS Model

Chapter 5

Table 5-1 Incident Warning Signs to Detect Drift from Safety Management Sys...

Chapter 7

Table 7-1 Training for Select RBPS Elements

Chapter 8

Table 8-1 US DOE Berkeley Lab Safety Culture

Chapter 9

Table 9-1 Technical Information for Each Phase

Table 9-2 Control Banding Strategies

Chapter 10

Table 10-1 Oxidizing Chemicals

Table 10-2 Pyrophoric Substances

Table 10-3 Decomposition Energies

Table 10-4 Toxicity Values for Selected Chemicals Commonly in Use in Indust...

Table 10-5 Standards and Guidance for Specific Gases

Table 10-6 Classes of Hazardous Compressed and Liquefied Gases

Table 10-7 Guidance on Storage and Cleaning of Laboratory Glassware

Chapter 11

Table 11-1 Hazard Analysis: High Temperature in Laboratory Reactor

Table 11-2 Reactive Chemical Hazards Questions for a Chemical Synthesis Pro...

Table 11-3 Hazards Analysis Methodologies Used in LAPPs

Chapter 13

Table 13-1 NFPA Standards for Fire and Explosion Control

Table 13-2 Laboratory Cold Storage Unit Types

Chapter 17

Table 17-1 Cryogenic Fluids and Typical Temperatures for Storage

Chapter 18

Table 18-1 Standards for Explosions and Combustible Dusts

Chapter 19

Table 19-1 Estimated Compressed Gas Delivery System Purging Cycles

Chapter 20

Table 20-1 Skill, Rule, Knowledge Based Approach

Table 20-2 Procedural Statements to Address Deviations

Table 20-3 Checklist with Validation Steps (excerpt)

Chapter 25

Table 25-1 Incident Investigation Steps

Appendix A

Table A-1 Example Format for Case Reports

Appendix C

Table C-1 Protection Guidelines Based on Chemical Safety Levels[54]

Table C-2 Occupational Exposure Limits For Toxic Compounds

Table C-3 HHECBs for small molecules

Table C-4 Application of Biosafety Levels to LAPPs

Table C-5 Mapping of RBPS and Biosafety Rules

Appendix D

Table D-1 Desirable Characteristics of Glass

Table D-2 Key Shortcomings of Glass

Table D-3 Types of Glass

Table D-4 Selected Thermal Parameters for Three Classes of Glass

List of Illustrations

Chapter 1

Figure 1-1 Format for Case Summaries in Chapter

Chapter 2

Figure 2-1 Laboratory Explosion and Fire Damage

Figure 2-2 Laboratory Fire and Water Damage

Figure 2-3 Laboratory Hood Fire Damage

Figure 2-4 Stages in the Risk‐Based Journey to Process Safety Excellence

Chapter 4

Figure 4-1 A Qualitative Risk Matrix

Figure 4-2 The “Swiss Cheese” Model

Figure 4-3 Bow Tie Diagram

Chapter 10

Figure 10-1 Fire Triangle

Figure 10-2 Analysis of Heat Production and Removal for Exothermic Process...

Figure 10-3 A Cryogenic Fluid Storage Dewar and Components

Figure 10-4 Damage Following the Explosion of a Liquid Nitrogen Dewar

Chapter 11

Figure 11-1 The Steps in a Hazard Identification and Risk Analysis (HIRA)

Chapter 13

Figure 13-1 Manual Restart after Alarm Shutdown

Chapter 14

Figure 14-1 Typical Pressure Relief Valve

Figure 14-2 Rupture Disk

Figure 14-3 Failed Rupture Disk in Holder from Supplier

Figure 14-4 Cross Section View of Typical Pressure Vacuum Protection Devices...

Figure 14-5 Blast cell in a small standalone building

Figure 14-6 Barricade around a high pressure unit

Chapter 17

Figure 17-1 Components and Markings on Compressed Gas Cylinders

Figure 17-2 Covered and Segregated Storage Areas for Compressed Gas Cylinder...

Figure 17-3 Storage Examples for Gas Cylinders

Figure 17-4 Multiple cylinder hot box

Figure 17-5 Compressed Gas Cylinder Connection Design

Figure 17-6 Inert Gas Glovebox

Figure 17-7 Anaerobic Chamber for Biological Research

Chapter 19

Figure 19-1 A CO

2

cylinder fell, sheared its valve and went through the roof...

Figure 19-2 Poor Location of Supply Station for Gas Cylinders

Figure 19-3 Compressed Gas Supply Stations on Exterior of Lab Building

Figure 19-4 Utility Service Corridor with Compressed Gas Cylinder Storage...

Figure 19-5 Individual Gas Cabinet Bank for Compressed Gas Supply

Figure 19-6 Walk‐in or Floor‐Mounted Ventilation Hood [78]

Figure 19-7 Compressed Gas Cylinders with Fire Barrier and Chain Restraints ...

Figure 19-8 Liquid Nitrogen Storage Vessel Located Outside Lab Building

Chapter 23

Figure 23-1 Review Stages in an MOC Program

Appendix A

Figure 1986‐1A Damage to masonry walls of Dow chemical synthesis pilot plant...

Figure 1986‐1B An Illustration comparing the expected and actual vapor space...

Figure 2000‐2 Hood after the Incident

Figure 2002‐1 Fume hood after the fire.

Figure 2003‐2A Explosion and fire damage to the laboratory oven

Figure 2003‐2B Fire damage to the laboratory ceiling

Figure 2006‐1 Evaporator apparatus after the explosion

Figure 2007‐1 Gas chromatography unit after explosion and fire

Figure 2007‐2 Charred material on heat transfer coil

Figure 2007‐3A Aerial view of the T2 Laboratories site after explosion

Figure 2007‐3B Portion of the reactor from the T2 Laboratories explosion

Figure 2008‐1 The damaged syringe used for the transfer

Figure 2008‐3A The contaminated detector area.

Figure 2008‐3B Broken plutonium compound radiation source bottle

Figure 2010‐3 Lab Bench after Detonation of NHP Derivative

Figure 2010‐4 The laboratory after the explosion

Figure 2011‐2A Before the Incident

Figure 2011‐2B After the Incident

Figure 2011‐4A: The fume hood after the fire

Figure 2012‐1A Igniter Autoclave Test Stand 1. Ignition autoclave 2. Mixing ...

Figure 2012‐1B Cross Section of Igniter Autoclave Pressure and Temperature S...

Figure 2012‐1C Igniter Insert in Base of Igniter Autoclave Stainless steel (...

Figure 2012‐1D Igniter Inserted in Bottom of Ignition Autoclave before Incid...

Figure 2012‐1E Hole Where Igniter Had Originally Been Inserted into Bottom o...

Figure 2012‐3A Laboratory chemical fume hood after explosion

Figure 2012‐3B Damaged oven used to the heat high pressure autoclave

Figure 2012‐3C Damaged high pressure autoclave after explosion

Figure 2012‐4 The fume hood following the explosion.

Figure 2012‐5: The refrigerator after the fire

Figure 2013‐2A Liquid/Liquid Extraction Pilot Plant Process Flow Diagram

Figure 2013‐2B Raffinate Receiver in Liquid/Liquid Extraction System

Figure 2014‐2 Fume hood after explosion at University of Minnesota

Figure 2016‐1A The lab benchtop bioreactor

Figure 2016‐1B Pressure vessel used to feed gas mixture to bioreactorSourc...

Figure 2016‐1C The damaged lab after the explosion

Appendix C

Figure C-1 Representation of the NFPA Diamond

Figure C-2 Health Hazard Exposure Control Band (HHECB) Limits

Figure C-3 Low Level Biological Hazards Benchtop

Figure C-4 PPE for BSL‐4 Lab

Figure C-5 Four Biosafety Levels (BSLs)

Guide

Cover

Table of Contents

Title Page

Copyright

List of Figures

List of Tables

Abbreviations and Acronyms

Glossary

Acknowledgments

Dedication

Online Materials Accompanying this Handbook

Preface

Begin Reading

References

Appendix A: Cases

Appendix B: Examples

Appendix C: Control Banding Strategies

Appendix D: Glass Equipment Design

Index

End User License Agreement

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This book is one in a series of process safety guidelines, handbooks, and concept books published by the Center for Chemical Process Safety (CCPS). Refer to www.wiley.com/go/ccps for full list of titles in this series.

It is sincerely hoped that the information presented in this document will lead to a better safety record for the entire industry; however, neither the American Institute of Chemical Engineers, its consultants, CCPS Technical Steering Committee and Subcommittee members, their employers, nor their employers' officers and directors warrant or represent, expressly or by implication, the correctness or accuracy of the content of the information presented in this document. As between (1) American Institute of Chemical Engineers, its consultants, CCPS Technical Steering Committee and Subcommittee members, their employers, and their employers' officers and directors and (2) the user of this document, the user accepts any legal liability or responsibility whatsoever for the consequence of its use or misuse.

Handbook for Process Safety in Laboratories and Pilot Plants

A Risk‐based Approach

 

Center for Chemical Process Safety

American Institute of Chemical Engineers

New York, NY

 

 

 

 

Copyright © 2023 by the American Institute of Chemical Engineers, Inc. All rights reserved.

A Joint Publication of the American Institute of Chemical Engineers and John Wiley & Sons, Inc.

Published by John Wiley & Sons, Inc., Hoboken, New Jersey.Published simultaneously in Canada.

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Library of Congress Cataloging-in-Publication Data Applied for:

Hardback ISBN: 9781119010135

Cover design: WileyCover images: © natros/Adobe Stock Photos; Alex_Traksel/Adobe Stock Photos

List of Figures

Figure 1‐1 Format for Case Summaries in Chapter

Figure 2‐1 Laboratory Explosion and Fire Damage

Figure 2‐2 Laboratory Fire and Water Damage

Figure 2‐3 Laboratory Hood Fire Damage

Figure 2‐4 Stages in the Risk‐Based Journey to Process Safety Excellence

Figure 4‐1 A Qualitative Risk Matrix

Figure 4‐2 The “Swiss Cheese” Model

Figure 4‐3 Bow Tie Diagram

Figure 10‐1 Fire Triangle

Figure 10‐2 Analysis of Heat Production and Removal for Exothermic Process

Figure 10‐3 A Cryogenic Fluid Storage Dewar and Components

Figure 10‐4 Damage Following the Explosion of a Liquid Nitrogen Dewar

Figure 11‐1 The Steps in a Hazard Identification and Risk Analysis (HIRA)

Figure 13‐1 Manual Restart after Alarm Shutdown

Figure 14‐1 Typical Pressure Relief Valve

Figure 14‐2 Rupture Disk

Figure 14‐3 Failed Rupture Disk in Holder from Supplier

Figure 14‐4 Cross Section View of Typical Pressure Vacuum Protection Devices

Figure 14‐5 Blast cell in a small standalone building

Figure 14‐6 Barricade around a high pressure unit

Figure 17‐1 Components and Markings on Compressed Gas Cylinders

Figure 17‐2 Covered and Segregated Storage Areas for Compressed Gas Cylinders

Figure 17‐3 Storage Examples for Gas Cylinders

Figure 17‐4 Multiple cylinder hot box

Figure 17‐5 Compressed Gas Cylinder Connection Design

Figure 17‐6 Inert Gas Glovebox

Figure 17‐7 Anaerobic Chamber for Biological Research

Figure 19‐1 A CO

2

cylinder fell, sheared its valve and went through the roof

Figure 19‐2 Poor Location of Supply Station for Gas Cylinders

Figure 19‐3 Compressed Gas Supply Stations on Exterior of Lab Building

Figure 19‐4 Utility Service Corridor with Compressed Gas Cylinder Storage

Figure 19‐5 Individual Gas Cabinet Bank for Compressed Gas Supply

Figure 19‐6 Walk‐in or Floor‐Mounted Ventilation Hood

Figure 19‐7 Compressed Gas Cylinders with Fire Barrier and Chain Restraints

Figure 19‐8 Liquid Nitrogen Storage Vessel Located Outside Lab Building

Figure 23‐1 Review Stages in an MOC Program

List of Tables

Table 1‐1 Framework for this Handbook

Table 1‐2 The CCPS Risk Based Process Safety (RBPS) Management System

Table 2‐1 Fatal Incidents in LAPPs Resulting from Fires and Explosions

Table 2‐2 Fatal Incidents in LAPPs Resulting from Exposure to Toxic Chemicals

Table 2‐3 Fatal Incidents in LAPPs Resulting from Exposure to Biological Agents

Table 2‐4 Fatal Incidents in LAPPs Resulting from Other Causes

Table 2‐5 Fire Losses in Laboratory Buildings

Table 2‐6 Comparison of LAPP Activities to the RBPS Elements

Table 2‐7 Leader Accountabilities for Process Safety

Table 4‐1 Description of Inherently Safer Design Strategies

Table 4‐2 Argonne NL WPC Process Compared to the CCPS RBPS Model

Table 5‐1 Incident Warning Signs to Detect Drift from Safety Management Systems

Table 7‐1 Training for Select RBPS Elements

Table 8‐1 US DOE Berkeley Lab Safety Culture

Table 9‐1 Technical Information for Each Phase

Table 9‐2 Control Banding Strategies

Table 10‐1 Oxidizing Chemicals

Table 10‐2 Pyrophoric Substances

Table 10‐3 Decomposition Energies

Table 10‐4 Toxicity Values for Selected Chemicals Commonly in Use in Industry

Table 10‐5 Standards and Guidance for Specific Gases

Table 10‐6 Classes of Hazardous Compressed and Liquefied Gases

Table 10‐7 Guidance on Storage and Cleaning of Laboratory Glassware

Table 11‐1 Hazard Analysis: High Temperature in Laboratory Reactor

Table 11‐2 Reactive Chemical Hazards Questions for a Chemical Synthesis Process

Table 11‐3 Hazards Analysis Methodologies Used in LAPPs

Table 13‐1 NFPA Standards for Fire and Explosion Control

Table 13‐2 Laboratory Cold Storage Unit Types

Table 17‐1 Cryogenic Fluids and Typical Temperatures for Storage

Table 18‐1 Standards for Explosions and Combustible Dusts

Table 19‐1 Estimated Compressed Gas Delivery System Purging Cycles

Table 20‐1 Skill, Rule, Knowledge Based Approach

Table 20‐2 Procedural Statements to Address Deviations

Table 20‐3 Checklist with Validation Steps (excerpt)

Table 25‐1 Incident Investigation Steps

Abbreviations and Acronyms

ACC

American Chemical Council

ACGIH

American Conference of Governmental Industrial Hygienists

ACH

Air Changes per Hour

ACS

American Chemical Society

AIChE

American Institute of Chemical Engineers

API

American Petroleum Institute

APIs

Active Pharmaceutical Ingredients

ASTM

American Society of Testing and Materials

CB

Control Banding

CCPS

Center for Chemical Process Safety

CFM

Cubic feet per minute

COO

Conduct of Operations

CPI

Chemical Process Industry

CSL

Chemical Safety Level

DOE

Department of Energy (US)

DOT

Department of Transportation (US)

EG

Exposure Guidelines

EHS

Environmental, Health, and (Occupational) Safety

ERPG

Emergency Response Planning Guideline

HEPA

High Efficiency Particulate Air [filter]

HHECB

Health Hazard Evaluation Control Band

HIRA

Hazards Identification and Risk Analysis

IDLH

Immediately Dangerous to Life and Health

IPL

Independent Protection Layer

ISO

International Organization for Standardization

LAPP

Laboratories and Pilot Plants

LC

Lethal Concentration

LFL

Lower Flammability Limit

LOPA

Layer of Protection Analysis

NASA

National Aeronautic and Space Administration (US)

NFPA

National Fire Protection Agency (US)

NIOSH

National Institute for Occupational Safety & Health (US)

NIST

National Institute of Science and Technology (US)

NOAA

National Oceanic and Atmospheric Administration (US)

OD

Operational Discipline

OEL

Occupational Exposure Limits (US OSHA)

P&ID

Piping and Instrumentation Diagram

PEL

Possible Exposure Limits (US OSHA)

PHA

Process Hazard Analysis

PI

Principal Investigator

PPE

Personal Protective Equipment

PTE

Permanent Total Enclosure

R&D

Research and Development

RBPS

CCPS Risk Based Process Safety

SDS

Safety Data Sheet

SME

Subject Matter Expert

SOP

Standard Operating Procedure

STEL

Short‐Term Exposure Limit

TAM

Thermal Activity Monitor

TLV

Threshold Limit Value (for toxicity)

TWA

Time‐Weighted Average

UFL

Upper Flammability Limit

US OSHA

US Occupational Safety and Health Administration

WPC

Work, Planning, and Control

Acknowledgments

The American Institute of Chemical Engineers (AIChE) and the Center for Chemical Process Safety (CCPS) express their appreciation and gratitude to all members of the Handbook for Process Safety in Laboratories and Pilot Plants Subcommittee for their generous efforts in the development and preparation of this important handbook. CCPS also wishes to thank the subcommittee members’ respective companies for supporting their involvement during the different phases in this project.

Book Committee Co‐Chairs

Kathy Anderson, Vertellus (retired)

Monica R. Stiglich, 3M (retired)

Core Book Team Members

Bruce D. Bullough, Corden Pharma Colorado (at Pfizer at time of publication)

Jeffrey J. Foisel, Dow Corning (at Dow Chemical Company at time of publication)

Jerry L. Jones, AIChE CCPS Consultant

Richard P. Palluzi, ExxonMobil (retired)

Other Committee Contributors

Michael T. Cleary, DuPont

Randy R. Keller, The Dow Chemical Company (retired)

David Caspary, ChE Department Staff, Michigan Technological University (retired)

Khateeta M. Emerson, Merck & Co.

William Fleming, Bristol Myers Squibb (retired)

Jeffrey A. Grant, Albemarle

Jeffrey A. Hedges, Chevron (retired)

Paul McAllister, Shell Catalysts & Technologies

Andrew G. Minister, US DOE Pacific Northwest National Lab (retired)

Kabier Moideenkutty, Abu Dhabi Oil Refining Company (TAKREER)

Christian Rauchegger, Linde Process Plants Inc.

Sebastien Righini, Solvay

Amy E. Theis, Fauske & Associates (at Acutech at time of publication)

Joel B. Young, BASF

Ronald J. Willey, Professor, Northeastern University

CCPS Staff Contributors for Final Manuscript Preparation

Jennifer Bitz, Lead Process Safety Engineer, Project Manager

Bruce K. Vaughen, Lead Process Safety Subject Matter Expert

Before publication, all CCPS books undergo a peer review process. CCPS gratefully acknowledges the thoughtful comments and suggestions of the peer reviewers. Their work enhanced the accuracy and clarity of this handbook.

Although the peer reviewers provided comments and suggestions, they were not asked to endorse this handbook and did not review the final manuscript before its release.

Peer Reviewers:

Jerry Forest

Celanese and Louisiana State University

Aaron Scurto

University of Kansas

Dan Crowl

Michigan Tech University (Professor Emeritus)

Kim Jeskie

Oak Ridge National Laboratory

Marc Majewski

San Francisco State University

Mike Kivistik

University of Nevada, Reno

Neal Langerman

Advanced Chemical Safety (retired)

Joseph Peters

Technip FMC

Deepak Sharma

Bayer

Louis DiBerardinis

MIT

Daniel Woodie

Cornell University

Emmanuelle Hagey

NOVA Chemicals

Sean P. Lapekas

Pfizer Inc.

Alvin Waller

FMC Corporation

Larry J. Westrum

Boulder Scientific Company

Satish Birajdar

Syngene International Ltd.

Omid Zadakbar

Biovectra

Fernando Silveira

Braskem S.A.

Dedication

CCPS Handbook for Process Safety in Laboratories and Pilot Plants

Is dedicated toJerry Forest

Jerry’s focus and passion for Process Safety shines in his work and life. He is an indispensable contributor to CCPS’s mission and he truly lives its tenets. His contributions on the leadership of the CCPS Planning Board have been and continue to be invaluable, as well.

Jerry’s focus on practical applications shows through his activities. To Jerry, ‘walk the line’ is not a country song or movie, but a process safety initiative he led as Senior Director of Process Safety at Celanese and that he shared with the rest of the industry. Clear and concise communications are at the focus of this initiative. Eliminating errors by improving the conduct of operations is Jerry’s belief—the operators must know with 100% certainty where energy will flow each time a processing unit change is made.

Jerry has been on many CCPS project committees, contributing his expertise to the CCPS body of knowledge. When the COVID‐19 pandemic affected the process industry, Jerry was a key contributor on a CCPS panel on managing Risk Based Process Safety (RBPS) during disruptive times. More recently, Jerry served as committee chair for the book Introduction to Process Safety for Engineers, 2ndEdition. Jerry maintains his status as a CCPS Certified Process Safety Professional (CCPSC).

Jerry is a passionate believer in teaching and giving future engineers process safety knowledge. Currently, he teaches a course on process safety at the Louisiana State University, his Chemical Engineering alma mater.

CCPS is delighted to dedicate this book to Jerry in recognition for his past, present and continuing support of CCPS and the global process safety community.

Anil Gokhale and Jennifer Bitz

Online Materials Accompanying this Handbook

CCPS invites readers to contribute to the incident data by providing laboratory and pilot plant incident summaries.

CCPS Member companies are encouraged to enter these incident cases into the CCPS Process Safety Incident Database (PSID). The PSID submittal procedure may be downloaded from the CCPS webpage [6].

Lessons shared from previous incidents can be used, in part, to improve process safety performance in Laboratories and Pilot Plants (LAPPs). This book presents cases throughout the chapters to illustrate relevant concepts. Appendix A of this handbook contains details of the case studies that are referenced briefly within the chapters.

Each incident is noted in the format shown in Appendix A . The typical incident descriptions provide a brief overview of where, when, and what happened. Since process safety and risk management system deficiencies are often the root causes of the incident, the authors end each case with a summary table of the management system(s) based on the Risk Based Process Safety (RBPS) Elements model, listed in Table 1‐2[7]. The table of root causes at the end of each incident case shows the most relevant management systems that could have helped prevent or mitigate the consequences of the incident.

Appendix A should be used only as a tool to identify incidents with applicable learnings. Since these examples are not from an exhaustive literature search, they are not to be used for statistical or trending information.

An electronic version of the incidents are available for downloading and searching capability. Please download the file from the CCPS website at:

www.aiche.org/ccps/LAPP-incidents

When opening the file, enter the password:

CCPSLAPP

Preface

The Center for Chemical Process Safety (CCPS) has been the world leader in developing and disseminating information on process safety management and technology since 1985. The CCPS, an industry technology alliance of the American Institute of Chemical Engineers (AIChE), has published over 100 books in its process safety guidelines and process safety concepts series, and over a hundred courses, including 33 training modules through its Safety in Chemical Engineering Education (SAChE) series. CCPS is supported by the contributions and voluntary participation of more than 225 companies globally.

The acronym LAPP is used throughout for Laboratories and Pilot Plants for better readability. The reader should recognize that it covers the entire scope of research activities and operations from a gas chromatograph to a pilot plant, or from a simple mixing operation inside a hood to a major processing step. Many process safety‐related issues are applicable to LAPPs, including: hazards identification and risk analysis; the handling and storage of hazardous materials; locating equipment; designing piping; and maintaining adequate emergency response.

Laboratory, pilot plant, and research applications occupy a unique niche within the chemical process industries. Their research activities are intended to develop process information – chemical, safety, operability, and maintainability – to advance the general chemistry understanding, find viable commercial applications or solutions, and ensure safe design and operation of a commercial process. LAPPs often handle similar hazardous materials and energies as a manufacturing plant, yet in smaller quantities and smaller equipment. The unknowns and uncertainties that accompany these activities significantly increases the potential risks. If the hazards are not properly understood and their associated risks not properly mitigated, personnel may be harmed when an incident occurs.

This book grew out a recognition that researchers could benefit from a dedicated CCPS handbook on process safety for LAPPs. This handbook is intended to help the reader identify process safety hazards and risks in a laboratory, pilot plant, or research environment. It offers practical hazard identification and risk analysis guidance to help prevent or reduce the consequences of incidents. Readers will be able to learn from LAPP‐related incidents, as well, reducing the likelihood that they will learn by having a similar incident. This handbook provides examples of typical process safety‐related practices, procedures, and systems, as well as references for more information, as needed.

Part 1 –Introduction and Overview

The purpose of this part of the book is to:

present key points about why taking a risk‐based approach to safety is important

propose some ways to begin the discussion and present the risk‐based approach to colleagues and leaders

provide an introduction to hazards and their controls

present the Risk Based Process Safety elements in a way that labs, pilot plants, and other research facilities can implement

provide some resources and examples to help implement a risk‐based management system for safety

1Purpose and Scope

1.1 Purpose

The purpose of this book is to help organizations better control hazards and risks in Laboratories and Pilot Plants (LAPPs). Hazards control starts with hazards identification, consequence evaluation, likelihood estimation and then risk analysis and assessment. This book provides methods for determining the controls needed to manage the risk in a LAPP. For example, when designing, operating, maintaining, and changing experimental and testing equipment, the CCPS Risk Based Process Safety (RBPS) concepts and related good management practices can be applied to help reduce the LAPP's risk. In particular, this book shows how to prevent LAPP incidents and helps LAPP staff identify the specific engineered and administrative controls that are needed to prevent the loss of control of hazardous materials and stored energies. Since the overall risk includes the impact of the release, this book also identifies the controls can be used to help reduce the impact of a release if it occurs.

This book is intended to supplement available information and guidance for identifying the hazards, controlling the risks, and managing process safety in LAPPs. It describes the proven risk management systems and approaches that have evolved at industrial facilities over since the 1980's. These industrial practices help eliminate or reduce many of the causes and impact of process safety incidents. The factors that were weak or missing altogether, identified as contributors to severe incidents in LAPPs include:

Having a sense of vulnerability to the hazards and their associated risks

Understanding the potential severity of an incident

Using established design practices

Having robust engineered and administrative safeguards

Having robust operating and maintenance procedures

Having robust training for operations and maintenance personnel

Adhering to procedures (e.g., strong operational discipline; recognizing and preventing normalization deviance)

Having robust change management practices

Planning and preparing for emergencies

Evaluating and addressing human factors issues

The CCPS RBPS practices described in this book will help eliminate or reduce the inherent factors in laboratories and pilot plants that may contribute to incidents in a LAPP. When applied effectively, these practices will help prevent the loss of control of hazardous materials or energies, will help significantly reduce the impact of the consequences if the loss of control does occur, and reduce the potential for injuries, fatalities, equipment damage, and program delays.

1.2 Scope of Book and Target Audience

When people work with hazardous materials and energies in a laboratory or pilot plant, their experimental designs from benchtop to full‐scale manufacturing should include equipment and methods that help prevent the loss of control of their hazards. This handbook identifies four broad hazard categories in LAPPs as: 1) Chemical; 2) Physical; 3) Biological, and 4) Ionizing radiation. The primary scope of this book is on how LAPP staff manage the material’s chemical and physical hazards. Biological and ionizing radiation management practices are outside this handbook's scope.

However, it is worth noting that this handbook does include summaries of incidents that resulted in the loss of control of biological or ionizing radiation hazards. In addition, a description of a biological hazard management control approach, Biosafety Control Banding, is included as Appendix C.

All LAPP staff will work with some level of chemical and physical hazards. This handbook presents approaches that can be used to help manage the risks associated with these hazards. This handbook will show how process safety practices and systems can help prevent the loss of control of hazardous materials and energies in LAPPs. They are based on the experience of researchers around the world and can be applied to the following activities:

Chemical and biochemical transformations

catalytic and non‐catalytic chemical synthesis reactions

bio‐transformations involving viable cells or immobilized enzymes;

thermal or catalytic cracking or decomposition

smelting of mineral ores

electrochemical reactions

partial or complete oxidation

neutralization reactions

chemical precipitation

chemical vapor deposition

Changes in physical state, concentration, or form

dissolving

evaporation

drying

size reduction of solids

agglomeration of solids or pelletizing

solids melting and solidification

encapsulation of particles or fluids

coating of films, parts, or components

thermal forming or extrusion of polymers

Physical mixing

gases

vapors

solids

liquids

Physical separation and purification

phase changes

distillation

drying

absorption

ion exchange

size selective or affinity type chromatography

size selective membranes

crystallization

precipitation

solvent extraction

In addition, this handbook addresses the storage and handling of the hazardous materials associated with these activities, and presents some of the physical and chemical analytical techniques that help verify and validate the effectiveness of the safety management system.

The target audience for this book is any LAPP staff working with or managing hazardous materials. In particular, for staff in either on‐site chemical processing facility laboratories or off‐site product Research and Development (R&D) laboratories. Other types of laboratories include other industry laboratories (e.g., electronics, agriculture, food, etc.), government laboratories (e.g., energy, agriculture, food production, etc.) and university laboratories (i.e., chemistry, chemical engineering, and material science departments). LAPP engineering and scientific professionals, LAPP technical support staff and LAPP managers will benefit from the approaches described in this handbook, as well.

Managing the risks of any laboratory or pilot plant requires diligent attention to how changes in experiments and experimental set‐ups can (and do) change the risk. The authors hope that the “Where to Start” discussion, presented in Section 2.3, will help the reader apply the CCPS the Risk Based Process Safety (RBPS) Management approach to their LAPP, either reinforcing the systems already in place or provide a proven approach for reducing their risks.

1.3 Terms for Laboratories and Pilot Plants

The following terminology will be used throughout this book:

LAPP

: Describes all Laboratories And Pilot Plants. Thus, “LAPP” includes all laboratories, pilot plants, and research facilities that stand‐alone or are a part of a commercial manufacturing site, government establishment, or academic institution.

Worker

: any laboratory or pilot plant worker including principle investigators, supervisors, students, lab technicians, pilot plant operators, staff, etc.

Incident

[8]

:

an unusual, unplanned, or unexpected occurrence that either resulted in, or had the potential to result in harm to people, damage to the environment, or asset/business losses, or loss of public trust or stakeholder confidence in a company’s reputation

Accident

[8]

:

an incident that results in a significant consequence involving:

human impact,

detrimental impact on the community or environment,

property damage, material loss,

disruption of a company’s ability to continue doing business or achieve its business goals

Near‐miss

[8]

:

an incident in which an adverse consequence

could potentially have resulted if circumstances had been slightly different.

This book includes many examples of actual incidents that have occurred in laboratories and pilot plants. The book will use the term “incident” when describing these events. Thus, all incidents described will include all LAPP “incidents.”

Because distinctions are often made between laboratories and pilot plants, including definitions in regulations or consensus standards, selected terms and definitions are provided. Regardless of whether specific process equipment or systems are considered “lab scale” or “pilot plant scale”, the practices described in this book should apply to both types of operations.

Multiple terms have been used to describe laboratories and pilot plants and to distinguish between the two types of facilities or activities. Definitions include amount of hazardous materials in use and the scale of chemical process equipment and apparatus. In this book, the acronym “LAPP” (Laboratories and Pilot Plants) will refer to all types of laboratories and pilot plants. The terms “staff” or “worker” are used throughout the book to refer to lab technicians, researchers, pilot plant workers, and other LAPP personnel who operate the equipment.

NFPA 45: Standard on Fire Protection for Laboratories Using Chemicals [4], used for design of laboratory facilities, draws a distinction between laboratories and pilot plants. NFPA 45 applies to laboratory buildings, laboratory units, and laboratory work areas in which chemicals, as defined, are handled or stored. The standard covers laboratory unit hazard classification, design, and construction; fire and explosion hazard protection; ventilating systems and chemical fume hoods; chemical storage, handling, and waste disposal; flammable and combustible liquids; compressed and liquefied gases; operations; and hazard identification.

The research laboratory has an ever‐changing environment, with research experiments changing frequently and may involve different hazards, such as chemical, physical, or biological. In NFPA 45 standard, laboratories and pilot plants are defined as follows: