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CHEMICAL HYGIENE PLAN Building: J.M. Patterson, #083 Room(s): 2225, Lab. for Advanced Materials Processing Department: Materials Science and Engineering Approved as UM Policy September 1994 Revised April 2002 Revised September 2004 Revised July 2006

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Page 1: CHEMICAL HYGIENE PLAN - LAMP Home · 2006-07-25 · CHEMICAL HYGIENE PLAN Building: J.M. Patterson, #083 Room(s): 2225, Lab. for Advanced Materials Processing Department: Materials

CHEMICAL

HYGIENE

PLAN

Building: J.M. Patterson, #083

Room(s): 2225, Lab. for Advanced Materials Processing

Department: Materials Science and Engineering

Approved as UM Policy September 1994

Revised April 2002

Revised September 2004 Revised July 2006

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Table of Contents

POLICY STATEMENT ............................................................................................................. 1

EMERGENCY TELEPHONE NUMBERS ............................................................................... 4 (to be completed by the Laboratory Supervisor)

STANDARD OPERATING PROCEDURES ............................................................................ 5

MEDICAL CONSULTATION AND EXAMINATIONS ......................................................... 7

IDENTIFICATION OF HAZARDOUS MATERIALS........................................................... 10

INFORMATION AND TRAINING......................................................................................... 13

EXPOSURE MONITORING ................................................................................................... 14

PRIOR APPROVALS .............................................................................................................. 16

LABORATORY SAFETY GUIDE AND REFERENCES...................................................... 18

UM FIRE EMERGENCY PROCEDURE..................................................................Appendix I

LAB-SPECIFIC PRIOR APPROVALS....................................................................Appendix II

LAB-SPECIFIC STANDARD OPERATING PROCEDURES.............................. Appendix III

(to be supplied by the Laboratory Supervisor)

CHEMICAL INVENTORY AND MATERIAL SAFETY DATA......................... Appendix IV (to be supplied by the Laboratory Supervisor)

Page 3: CHEMICAL HYGIENE PLAN - LAMP Home · 2006-07-25 · CHEMICAL HYGIENE PLAN Building: J.M. Patterson, #083 Room(s): 2225, Lab. for Advanced Materials Processing Department: Materials

UM Policy on Occupational Exposure to

Hazardous Chemicals in Laboratories Approved by the President September 19, 1994

A. Purpose.

This is a statement of official University policy to establish the process for compliance

with the Occupational Safety and Health Administration (OSHA) regulation

"Occupational Exposure to Hazardous Chemicals in Laboratories."

B. Policy.

The University is dedicated to providing safe and healthful laboratory facilities for

students and employees, and complying with federal and state occupational health and

safety standards. Laboratory administrators, managers, faculty, staff and students all

share responsibility for minimizing their exposure to hazardous chemical substances

which, for purposes of this policy, shall be defined as chemicals which are carcinogens,

toxic or highly toxic agents, reproductive toxins, irritants, corrosives, sensitizers,

hepatotoxins, nephrotoxins, neurotoxins, agents which act on the hematopoietic systems,

and agents which damage the lungs, skin, eyes, or mucous membranes.

The Chemical Hygiene Plan shall be implemented for all facilities at the University of

Maryland, College Park, where hazardous chemicals are handled or used under all of

the following conditions: (i) chemical manipulations are performed in containers

designed to be easily and safely manipulated by one person; (ii) multiple chemical

procedures or chemicals are used; and (iii) demonstrably effective laboratory practices

and equipment are available and in common use to minimize the potential for

employee exposure to hazardous chemicals.

The Chemical Hygiene Plan shall be reviewed and evaluated for its effectiveness at

least annually, and updated as necessary.

C. Responsibilities.

1. Department of Environmental Safety shall:

(a) Appoint a Chemical Hygiene Officer to develop and coordinate

administration of the UM Chemical Hygiene Plan (CHP);

(b) Prepare the CHP with annual review and revisions as needed;

(c) Distribute the CHP to each affected department for each Laboratory

Supervisor or Principal Investigator (LS/PI);

(d) Provide consultation, worksite monitoring (sampling), advisory

assistance and information concerning use of hazardous materials;

(e) Investigate, document and report to the BACH Committee,

significant chemical exposure or contamination incidents;

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(f) Collect and dispose of hazardous, radioactive and other regulated

wastes;

(g) Direct periodic laboratory safety audits to determine regulatory

compliance, and recommend action to correct conditions generating

release of toxic chemicals;

(h) Provide training to all laboratory workers concerning:

(1) Provisions of the Chemical Hygiene Plan;

(2) Physical and health hazards of chemicals in the work area;

(3) Measures to protect employees from chemical hazards;

(4) Signs and symptoms associated with hazardous chemical

exposure;

(5) Location of reference materials on the hazards, safe handling,

storage and disposal of laboratory chemicals;

(6) The contents of the OSHA standard and its appendices;

(7) The permissible exposure limits (PELs) for OSHA regulated

substances or recommended exposure limits if no PEL is

listed; and

(8) The methods and observations used to detect the presence or

release of a hazardous chemical.

2. Laboratory Supervisors/Principal Investigators (LS/PI) shall:

(a) Implement all provisions of the Chemical Hygiene Plan for

laboratory facilities under their control;

(b) Develop and maintain a customized Chemical Hygiene Plan for

laboratory operations under their control to include:

(1) Alphabetized inventory of all hazardous chemical substances,

(2) Written Standard Operating Procedures to address safety and

health issues associated with work practices, protective

equipment, in laboratory facilities under their control;

(3) Identification of occurrences or operations that may be

encountered by laboratory employees and that require that the

LS/PI be advised (prior approval).

(c) Prepare and implement laboratory-specific Standard Operating

Procedures (SOPs) to include work practices, protective equipment,

engineering controls, emergency procedures and waste disposal

procedures;

(d) Demarcate and indicate on SOP all areas designated for the use of

particularly hazardous chemicals (i.e., select carcinogens, reproductive

toxins and acute toxins);

(e) Train laboratory workers regarding the specific practices and provisions

contained in the laboratory SOP;

(f) Ensure that all lab employees have access to Material Safety Data

Sheets for hazardous chemicals that are purchased or otherwise

acquired for use in the lab facility;

(g) Ensure that all necessary personal protective equipment is available and

used by lab employees;

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(h) Notify the designated UM contact points when any of the University of

Maryland prior notification conditions are anticipated;

(i) Comply with necessary documentation requirements; and

(j) Submit a current copy of their Chemical Hygiene Plan(s) including all

required components to the Department of Environmental Safety and

Departmental Compliance Officer.

3. Biological and Chemical Hygiene (BACH) Committee shall:

Review and approve all aspects of the Chemical Hygiene Plan and

provide technical guidance for implementation of campus policy concerning

chemical and biological safety.

4. University Health Center shall:

(a) Coordinate and direct all required or recommended medical

surveillance programs;

(b) Provide medical consultations and examinations for laboratory workers

who have been overexposed, or suspect overexposure, to hazardous

chemical substances; and

(c) Maintain medical records relating to consultations, examinations and

medical surveillance as required by law.

5. Departmental and College Compliance Officers shall:

(a) Assist Environmental Safety and laboratory supervisors with

implementation of the Chemical Hygiene Program; and

(b) Maintain current copies of Chemical Hygiene Plans.

6. Department Chairs and College Deans shall:

(a) Require implementation of the Chemical Hygiene Program for affected

laboratories under their control.

7. Individual Researchers and Laboratory Users shall:

(a) Adhere to the requirements of the Chemical Hygiene Plan and

SOPs;

(b) Complete all safety training requirements and comply with

documentation procedures;

(c) Notify the PI/LM if any prior notification situations or occurrences are

anticipated; and

(d) Report all workplace injuries, chemical exposure incidents or unsafe

conditions to their LS/PI as soon as possible.

D. Information

Assistance will be provided by the Department of Environmental Safety to any

Department requesting guidance or training to satisfy implementation of this

policy.

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Emergency Telephone Numbers

UM Emergency (FIRE - POLICE - RESCUE) - 24 hour # 911

CALL IMMEDIATELY FOR ANY EMERGENCY INCLUDING

INJURED OR SICK PERSON, CHEMICAL SPILL OR FIRE

Environmental Safety (Main Office) (301) 405-3960

(Industrial Hygiene, Hazardous Waste Management,

Fire Protection, Hazard Communication, Safety

Education)

Chemical Hygiene Officer (301) 405-3980

(Program Consultation and Administration)

Biological Safety (301) 405-3960

(Biological Safety, Regulated Pathogen Consultation)

Radiation Safety (301) 405-3985

(Health Physics, Radioactive Materials Procurement)

University Health Center Occupational Health (301) 314-8172

(Medical Consultation and Evaluation)

Workers' Compensation Office (301) 405-5466

Facilities Management Work Control (301) 405-2222

(Repair of Facility Equipment Deficiencies, e.g.,

fume hoods, emergency eyewashes, ventilation, etc.)

Laboratory Supervisor(s): Business-hours # After-hours #

Laurent Lecordier Cell # (301) 602 9858, office (301) 405 5858, home (301)602 9858

Gary Rubloff Office # (301) 405 2949, (cell) 301 785 2751

Laboratory Personnel: Business-hours # After-hours #

Erin Robertson(GRA), Office #(301) 405 2971, (cell) 919 345 5367

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Standard Operating Procedures (SOPs)

A comprehensive health and safety program should include documents that provide

descriptions of standard methods or operations used within the facility. They should describe

in clear and precise language the means and methods to be used by laboratory workers to

minimize the risk of hazardous exposure while using hazardous chemicals.

These documents, commonly referred to as standard operating procedures (SOPs), should

be followed by all laboratory employees.

The LS/PI is responsible for preparation of lab-specific SOP documents for attachment

to the CHP. The LS/PI is responsible for determining the adequacy of the SOPs prepared.

The lab-specific SOPs shall be incorporated in the on-site copy of the Chemical Hygiene Plan

and placed in a designated location within the laboratory for immediate access by employees.

A good SOP is one that is clearly stated and realistic in scope. A laboratory LS/PI

should prepare SOPs for all routine and repetitive operations as well as for general laboratory

operations. The format of all SOPs should be consistent and should incorporate:

1. Facility name, department and section affected by or using the procedure;

2. Subject;

3. Issue date of the original document or current revision;

4. Any indication that revisions replace an earlier procedure;

6. Signature or initials of the SOP preparer as well as any reviewing authority;

and

7. Concise instructions for safe and healthful performance of laboratory activities

and procedures.

SOPs should indicate the measures that will be used to reduce or prevent employee

exposure to hazardous chemicals, including engineering controls, hygiene practices. and

the use and maintenance of personal protective equipment.

SOPs should include provisions for additional employee protection for work with

particularly hazardous substances, including select carcinogens, reproductive toxins, and

substances which have a high degree of acute toxicity. (See "Identification of Hazardous

Materials, below.) Where appropriate, these additional measures should include:

1. Establishment of a designated area;

2. Use of containment devices such as fume hoods or glove boxes;

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3. Procedures for safe removal of contaminated waste; and

4. Procedures for site and personal decontamination.

SOPs shall also indicate circumstances under which certain laboratory procedures,

operations or activities require prior approval from the LS/PI before implementation (e.g.,

use of radioactive materials, bench top manipulation of volatile carcinogenic solvents

without use of engineering controls, night or weekend work performed alone, reagent

substitutions, etc.).

Examples of SOPs are available on the DES website at:

http://www.umd.edu/des/ls/index.html

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Medical Consultation and Examinations

Employees who work with hazardous chemicals in the laboratory should be referred

for medical consultation, examination, and/or surveillance (as appropriate to the

circumstances) whenever:

1. An employee develops signs or symptoms associated with a hazardous

chemical to which the employee may have been exposed in the laboratory;

2. An event takes place in the work area to create a likelihood of hazardous

exposure; or

3. Exposure monitoring reveals an exposure level routinely above the action level

(or in the absence of an action level, the Permissible Exposure Limit) for an

OSHA-regulated substance for which there are exposure monitoring and

medical surveillance requirements. (See "Exposure Monitoring" section,

below.)

Examples of events or circumstances which might result in hazardous exposure

include:

1. A spill or leak which rapidly releases a hazardous chemical in an uncontrolled

manner;

2. Direct skin or eye contact with a hazardous chemical;

3. Symptoms such as headache, rash, nausea, tearing, irritation or redness of eyes,

irritation of nose or throat, dizziness, loss of motor dexterity or judgement

which disappear when the employee is removed from the exposure area and

which reappear when the employee returns to working with the same

hazardous chemical;

4. Two or more employees in the same laboratory work area exhibit similar

symptoms; or

5. Exposure monitoring indicates exposures above regulated or recommended

limits.

The University has established procedures for responding to job-related injuries.

These procedures should be followed in the event of hazardous exposure due to the use of

hazardous chemicals in the laboratory. Instructions and forms for reporting injuries and

chemical exposures are available through the DES web page:

http://www.umd.edu/des/risk_comm/wcomp/

In the event of life-threatening injuries or illnesses, the UM Emergency Dispatcher

should be immediately notified. All injury or illness occurring as a result of work activities

should be reported to the Workers' Compensation Office, immediately after the incident

occurs or the injury is treated. All incidents of hazardous exposure, including their

disposition, should be reported to the Chemical Hygiene Officer.

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The following information should be provided at the time that an employee is referred

for medical consultation and/or examination:

1. Identity of the chemical(s) to which the employee may have been exposed;

2. Description of the conditions under which the exposure occurred, including

any quantitative exposure data, if available; and

3. A description of the signs and symptoms of exposure that the employee

experienced, if any.

A written report must be provided to the employer from any physician to whom the

employee is referred for medical consultation or examination in connection with hazardous

exposure. The physician's report(s) should indicate ONLY the specific findings of diagnoses

related to occupational exposure and should include the following information:

1. Any recommendation for further medical follow-up;

2. The results of the medical examination and any associated test(s);

3. Any medical condition which may be revealed in the course of the examination

which may place the employee at increased risk as a result of exposure to a

hazardous workplace; and

4. A statement that the employee has been informed by the physician of the

results of the consultation or medical examination and any medical

condition that may require further examination or treatment.

As indicated above, all incidents of hazardous exposure (including disposition) should

be reported to, and documented by, the Chemical Hygiene Officer (CHO). If no further

assessment of the incident is deemed necessary, the reason for that decision should be

included in the documentation. If the event is determined to require investigation, a formal

exposure assessment will be initiated by the CHO. The purpose of an exposure assessment is

not to determine whether there was a failure to follow proper procedures, but to identify the

hazardous chemical(s) involved and determine whether an exposure might have caused harm

to an employee. An exposure assessment may include the following items:

1. Interviews with the employee and complainant (if different);

2. Obtaining the following information:

- the names of chemicals which may be involved

- other chemicals used by the employee

- all chemicals used by others in the immediate area

- other chemicals stored in the immediate area

- symptoms exhibited or claimed by the employee

- comparison of symptoms with those referenced in the Material Safety

Data Sheet for each involved chemical

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- observation of control measures and personal protective equipment in use

during the event

- notation of any on-site exposure monitoring performed previous to or

during event

3. Monitoring or sampling the air in the area for suspect chemicals; and

4. Determination of whether the current control measures were adequate

during the time of the incident.

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Identification of Hazardous Materials

A hazardous chemical is defined by the OSHA laboratory standard as "a chemical for

which there is statistically significant evidence based on at least one study conducted in

accordance with established scientific principles that acute or chronic health effects may occur

in exposed employees." Hazardous chemicals include carcinogens, toxic or highly toxic

agents, reproductive toxins, irritants, corrosives, sensitizers, hepatotoxins, nephrotoxins,

neurotoxins, agents which act on the hematopoietic system and agents which damage the

lungs, skin, eyes or mucous membranes.

Laboratory supervisors have certain responsibilities for the management of these

hazardous chemicals, including:

1. Inventory of all hazardous chemical substances which are used in their

laboratories, and attaching the inventory to this CHP;

2. Maintenance of the labels on incoming containers of hazardous chemicals

to ensure that they are not removed or defaced;

3. Maintenance of any Material Safety Data Sheets (MSDSs) that are received

with incoming shipments of hazardous chemicals, and ensuring that the

MSDSs are readily accessible to laboratory employees; and

4. Determination of whether chemical substances which are developed in the

laboratory are hazardous chemicals within the definition of this CHP. If

the chemical substance is a byproduct for which the composition is

unknown, the substance should be deemed to be a hazardous chemical.

Laboratory supervisors also are responsible for identifying the following hazardous

chemicals which are required to be used in an area specially designated for such use:

1. Select carcinogens: Any substance which meets one of the following

criteria:

- it is regulated by OSHA as a carcinogen;

- it is listed under the category, "known to be carcinogens," in the Annual

Report on Carcinogens published by the National Toxicology Program

(latest edition);

- it is listed under Group 1 ("carcinogenic to humans") by the International

Agency for Research on Cancer (IARC) Monographs (latest edition); or

- it is listed in either Group 2A or 2B by the IARC, or under the category,

"reasonably anticipated to be carcinogens" by NTP, and causes

statistically significant tumor incidence in experimental animals in

accordance with criteria specified in the OSHA laboratory standard.

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2. Reproductive toxins: Chemicals which affect the reproductive capabilities,

including chemicals which are mutagenic and teratogenic;

3. Acute toxins; and

4. Unknowns: Chemicals which are synthesized in the laboratory and which

are byproducts for which the composition is unknown.

Information concerning the health effects of chemical substances can be located in the

following reference sources:

1. Material Safety Data Sheets (MSDS)

MSDSs are available through:

(A) The Department of Environmental Safety (DES):

1. Web Page (http://www.umd.edu/des),

2. Telephone (301-405-3960), or

3. After normal hours through UM Emergency Dispatcher at 911),

and

(B) the vendor, manufacturer or distributor. (A MSDS must be provided at

the time of initial purchase by the vendor, manufacturer or distributor

without charge. A nominal fee may be assessed for additional copies.)

2. Registry of Toxic Effects of Chemical Substances (available through the DES

Web Page:

(http://www.umd.edu/des/os/ccinfo/index.html)

3. National Toxicology Program (Chemistry Library or DES)

4. International Agency for Research on Cancer (Chemistry Library or DES)

5. DES maintains an Internet database of the Select Carcinogens as well as

chemical substances that may be considered acute and reproductive toxins.

This list may be accessed at:

www.umd.edu/des/ls

Use of any of the following materials may be subject to specific occupational safety

and health standards as shown:

Asbestos, tremolite, anthophyllite and actinolite 29 CFR 1910.1001

4-Nitrobiphenyl .1003

alpha-Naphthylamine .1004

4,4'-Methylene bis(2-chloroaniline) .1005

Methyl chloromethyl ether .1006

3,3'-Dichlorobenzidine (and salts) .1007

bis-Chloromethyl ether .1008

beta-Naphthylamine .1009

Benzidine .1010

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4-Aminodiphenyl .1011

Ethyleneimine .1012

beta-Propiolactone .1013

2-Acetylaminofluorene .1014

4-Dimethylaminoazobenzene .1015

N-Nitrosodimethylamine .1016

Vinyl Chloride .1017

Arsenic (inorganic) .1018

Lead .1025

Cadmium .1027

Benzene .1028

Cotton dust .1043

1,2-Dibromo-3-chloropropane .1044

Acrylonitrile .1045

Ethylene oxide .1047

Formaldehyde .1048

4,4'-Methylenedianiline .1050

Methylene Chloride .1052

Non-Asbestiform tremolite, anthophyllite and actinolite .1101

These standards are not replaced by the Occupational Exposure to Hazardous Chemicals in

Laboratories standard. Users of these materials are expected to adhere to the provisions of all

applicable substance-specific standards if employee exposure routinely exceeds the OSHA-

mandated permissible exposure limit (or Action Level, if specified). Copies of these

standards may be obtained from the Department of Environmental Safety or through the

OSHA website at:

www.osha.gov

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Information and Training

All UM employees must assume an active role in maintaining a safe working

environment by reporting any problems or noncompliance with policies to the LS/PI. All

employees should fully utilize any information provided during formal and informal training

sessions. Any staff member who does not understand a policy or procedure should consult the

LS/PI, departmental safety committee or DES for clarification.

All employees shall be provided with information and training regarding the hazards

of the chemicals in their work area. Employees shall be informed of:

1. The contents of the OSHA standard and its appendices;

2. The location and availability of the CHP;

3. The permissible exposure limits (PELs) for OSHA regulated substances or

recommended exposure limits if no PEL is listed;

4. The methods and observations used to detect the presence or release of a hazardous

chemical;

5. The physical and health hazards of chemicals in the work area;

6. The measures employees can take to protect themselves from chemical hazards,

including specific procedures (SOPs) to be used;

7. Signs and symptoms associated with exposures to hazardous chemicals used in the

laboratory; and

8. The location of known reference material on the hazards, safe handling, storage, and

disposal of chemicals found in the laboratory.

Distribution of training materials to LS/PIs and members of departmental safety

committees is coordinated through the Department of Environmental Safety. Training of

laboratory workers in general laboratory safety and the provisions of the OSHA laboratory

standard's requirements shall be conducted by UM Chemical Hygiene Officer (or designee)

during training sessions scheduled through the Department of Environmental Safety or

through special arrangement with DES. An on-line Chemical Hygiene training course is also

available to UM laboratory employees at the following website:

http://des.umd.edu/TrainingClass/index.cfm

The LS/PI shall be responsible for training of all supervised laboratory employees as

to specific operations, safety equipment, emergency procedures, SOPs and chemical use

which apply to the laboratory facilities. Documentation of general laboratory safety and CHP

training conducted by the Department of Environmental Safety shall be maintained within

each department and by the Department of Personnel Services as part of the employee's

permanent record. Documentation of laboratory-specific training provided by the LS/PI

shall be maintained within each department and laboratory.

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Exposure Monitoring

OSHA has established "Permissible Exposure Limits" (PELs) for laboratory

employees' exposures to certain regulated substances. Exposure levels must be determined

and monitored under certain circumstances. A medical surveillance program has been

established for certain specified employees whose work assignments involve regular and

frequent handling of toxicologically significant quantities of a chemical. In addition, the

Department of Environmental Safety is responsible for making determinations regarding the

requirements for area and/or personal exposure monitoring in specific circumstances.

PELs are specified in the OSHA regulation 29 CFR 1910, Subpart Z Toxic and

Hazardous Substances. In addition, PELs are usually indicated on the MSDSs, and can be

obtained from the Department of Environmental Safety.

These limits are defined as:

- Eight-hour time weighted average (TWA)

The average concentration to which an employee may be exposed to a

particular chemical for up to eight hours per day, five days per week.

- Short Term Exposure Limit (STEL)

The average concentration to which an employee may be exposed to a

particular chemical for up to fifteen minutes per day.

- Ceiling (C)

The maximum concentration to which an employee may be exposed to a

particular chemical at any time.

Often, a notation of "Skin" is printed with an exposure limit. This indicates that skin

absorption of that chemical occurs readily which would contribute to an employee's overall

exposure. Employee exposure to dermal absorption of chemical substances can often be

monitored through the use of biological testing.

Employee exposure should be monitored in the following circumstances:

1. Initially, where there is reason to believe that exposure levels to any

chemical substance regulated by a standard routinely exceed the action level

(or in the absence of an action level, the PEL) for an OSHA-regulated

substance for which there are exposure monitoring and medical surveillance

requirements; and

2. Periodically, where the initial monitoring discloses employee exposure over

the action level (or in absence of an action level, the PEL).

The general training provided by the Department of Environmental Safety will include

information regarding the identification of situations where employee exposure might exceed

the PEL, TLV or STEL. TLVs (Threshold Limit Values) are eight-hour time-weighted

average inhalation exposure limits recommended by the American Conference of

Governmental Industrial Hygienists. The Department of Environmental Safety will perform

area and/or personal exposure monitoring at the request of any LS/PI or laboratory worker.

The employee will be provided written notification of monitoring results, within 15 working

days after receipt of monitoring results by the University.

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Where initial monitoring discloses employee exposure over the action level (or in the

absence of an action level, the PEL), the affected employee must be provided with personal

protective equipment, unless engineering controls are available as a feasible means of

controlling exposure. The LS/PI is responsible for ensuring that appropriate protective

equipment is available to laboratory employees.

Monitoring will be terminated when appropriate in accordance with the relevant

standard.

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Prior Approvals

The Principal Investigators/Laboratory Supervisors (LS/PI) is responsible for

providing institutional notifications as defined below:

1. Any purchase, possession or use of explosive materials (as defined by the US

Department of Alcohol, Tobacco & Firearms) must be approved by the UM Fire

Marshal (301-405-3970). A comprehensive list of explosive materials may be

accessed from the ATF Website at:

http://www.atf.treas.gov/pub/fire-explo_pub/listofexp.htm

2. Any modification to a chemical fume hood or other laboratory local exhaust system

must be reviewed and approved by the Department of Facilities Management (301-

405-0255) and/or the Department of Environmental Safety (405-3960) before it may

be used as a means to control exposure to hazardous materials.

3. Any use of hazardous chemicals that may present a hazardous condition due to

inadequate ventilation must be reviewed and approved by the Chemical Hygiene

Officer prior to initiation of the operation.

4. Any research involving animals must be reviewed and approved by the Institutional

Animal Care and Use Committee. Additional information is available at the following

Website:

http://www.umresearch.umd.edu/IACUC/

5. Any possession or use of radioactive materials or radiation-producing devices must be

reviewed and approved by the Radiation Safety Officer. Additional information may

be obtained by calling (301) 405-3985.

6. Any research work involving human subjects must be reviewed and approved by the

Institutional Review Board. Additional information is available at the following

Website:

www.umresearch.umd.edu/IRB

7. Any purchase, possession or use of etiologic agents must be reviewed and approved by

the UM Biosafety Officer. Additional information may be obtained by calling (301)

405-3975 or from the following website:

http://www.umd.edu/des/biosafety/infectious/index.html

8. Treatment (e.g., neutralization) or drain disposal of any hazardous waste must be

reviewed and approved by the Environmental Affairs section of the Department of

Environmental Safety. Additional information may be obtained by calling (301) 405-

3163.

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9. Any use of respirators must be reviewed and approved by the UM Respiratory

Protection Program Administrator. Additional information may be obtained by calling

(301) 405-3980 or from the following website:

http://www.umd.edu/des/os/respirator/index.html

10. The use of extremely toxic gases must be reviewed and approved by the Chemical

Hygiene Officer prior to initiation of work. These gases include:

Arsine and gaseous derivatives

Chloropicrin in gas mixtures

Cyanogen chloride

Cyanogen

Diborane

Germane

Hexaethyltetraphosphate

Hydrogen cyanide

Hydrogen selenide

Nitric oxide

Nitrogen dioxide

Nitrogen Tetroxide

Phosgene

Phosphine

Laboratory employees are responsible for obtaining approval from the LS/PI if any of the

following operations will occur:

1. Laboratory operations that will be left unattended.

2. Modification of any established laboratory procedure.

3. Modification to laboratory chemical inventory.

4. Continuation of any laboratory procedure if unexpected results occur.

5. Use of Particularly Hazardous Materials in locations where no engineering controls

(e.g., fume hood) are to be used.

6. Any operation for which employees are not aware of the hazards nor are confident in

their ability to be adequately protected.

The LS/PI is also required to evaluate these specific laboratory operations and include in

Appendix II any additional conditions that require prior approval.

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Laboratory Safety Guide and References

The Laboratory Safety Guide is a separate document prepared and distributed by the

Department of Environmental Safety which is available on-line at:

http://www.umd.edu/des/ls/index.html

The Guide was assembled to assist laboratory supervisors and workers in their daily

operations at UM and to provide a means to lessen employee exposure to hazardous materials

and operations. It can supply much of the information needed to provide laboratory workers a

safe working environment. However, laboratory workers should not assume that this guide

will supply sufficient information to prevent injury and protect the environment. The nature

of the work that is performed in many research and testing laboratories increases the necessity

for safety planning and awareness. The Principal Investigator and other faculty often have

special expertise in the unique or specific experimental processes used in laboratories under

their control, and the prepared SOP may supersede general laboratory safety guidelines.

Recommended reference sources concerning safe operations in laboratories include:

CRC Handbook of Laboratory Safety

CRC Press, Inc.

Guide for Safety in the Chemical Laboratory

Van Nostrand Reinhold Company

Improving Safety in the Chemical Laboratory

John Wiley and Sons

Prudent Practices for Handling Hazardous Chemicals in Laboratories

National Academy Press

Safe Storage of Laboratory Chemicals

John Wiley and Sons

Safety in Academic Chemistry Laboratories

American Chemical Society

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Appendix I

X-7.00(A) UM POLICY CONCERNING FIRE EMERGENCIES

APPROVED BY THE PRESIDENT MARCH 6, 1993

A. Purpose. This is a statement of official University policy for the reporting of fire emergencies and for

the evacuation of campus buildings during fire emergencies, in compliance with local, state,

and federal regulations.

B. Policy. A fire emergency exists whenever:

1. A building fire evacuation alarm is sounding;

2. An uncontrolled fire or imminent fire hazard occurs in any building or area of the campus;

3. There is the presence of smoke, or the odor of burning;

4. There is spontaneous or abnormal heating of any material, an uncontrolled release of

combustible or toxic gas or other material, or a flammable liquid spill.

C. Procedures. Campus Buildings shall be immediately and totally evacuated whenever the building

evacuation alarm is sounding.

1. Upon discovery of evidence that a fire emergency exists, an individual shall accomplish, or

cause to be accomplished, the following actions:

(a) SOUND AN ALARM. Activate the building fire alarm in buildings equipped with a

manual fire alarm system. Shout a warning and knock on doors as you evacuate in

buildings not equipped with a fire alarm.

(b) SHUT OFF ALL MACHINERY AND EQUIPMENT IN YOUR AREA.

(c) LEAVE THE BUILDING AT ONCE.

(d) CALL THE FIRE DEPARTMENT FROM A SAFE PLACE.

(1) On-Campus phones DIAL 911

(2) Off-Campus phones and campus pay phones DIAL 911

(3) Use Campus emergency phones;

Indoors - Yellow wall phones with red "EMERGENCY" markings (some

corridors)

Outdoors - Yellow phone boxes with red "EMERGENCY" markings, under

blue lights.

(4) When the emergency operator answers, ask for the fire department, give as

much specific information as possible. State that you are from UMCP and

include the proper name of the building and room number, floor, or other

specific area. Do not hang up until released by the dispatcher. A PHONE

CALL MUST BE MADE! ALL BUILDING FIRE ALARMS DO NOT

NOTIFY THE FIRE DEPARTMENT.

(e) MEET THE FIRE DEPARTMENT OUTSIDE AND DIRECT THEM TO THE

EMERGENCY.

(f) ALL FIRES, EVEN IF EXTINGUISHED OR FOUND EXTINGUISHED, MUST BE

REPORTED.

(g) ALL FIRE ALARMS, EVEN IF SUSPECTED TO BE FALSE OR ACCIDENTAL,

MUST BE REPORTED TO THE FIRE DEPARTMENT.

2. The evacuation procedures shall be as follows:

(a) It shall be the responsibility of every person to immediately leave a University

building whenever the fire alarm is activated or a fire emergency exists.

All students, faculty, and staff are required to leave the building and remain outside

until the emergency is over. No one shall restrict or impede the evacuation.

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(b) Department heads are expected to review annually fire prevention and fire survival

information with faculty and staff, or to schedule such a presentation with the

Department of Environmental Safety. Such information is available from the

Department for use and distribution.

3. Whenever it is brought to the attention of the staff of residential buildings, or departmental

personnel, that the fire alarm or sprinkler system is inoperable or has been placed out of

service, a firewatch shall be established.

(a) Responsible personnel (residential staff, safety committee, etc.) shall be assigned to

the firewatch.

(b) The entire building shall be toured at least one time during each hour of the firewatch.

(c) The emergency dispatcher (405-3555) shall be notified each hour that the watch has

been performed.

(d) The firewatch shall be maintained at all times that the building is occupied until the

fire protection system is repaired.

4. INTERRUPTION OF FIRE ALARM:

(a) No person may shut off any fire protection or alarm system during a fire emergency

incident without the permission of the fire department officer in charge.

(b) No person may shut off any fire protection or alarm system during a bomb threat

emergency without the permission of the police officer in charge.

(c) It shall be the responsibility of the Department of Facilities Management Department

to reset or repair any fire protection or alarm system after an emergency incident

when notified by the fire or police department in charge. The Department of Facilities

Management shall inspect each such system immediately after every emergency

incident and place the system in serviceable condition.

(d) The fire and police departments may reset an alarm system only if there is no damage

to the system and when it is within their technical capabilities to do so.

(e) Any person desiring to interrupt service to any fire protection or alarm system must

obtain permission from the Department of Facilities Management, Work Control

Center (405-2222) which shall notify the fire and police departments of every such

interruption.

(f) Fire or police department must request the Facilities Management to repair or rest a

fire protection system, via the Work Control Center (405-2222).

5. INFORMATION RELEASE TO MEDIA AND THE PUBLIC:

All information regarding University fires will be released through the Department of

Environmental Safety in cooperation with the Public Information Office. No other University

agency or employee may release official statements regarding the cause, origin, or nature of

campus fires.

D. Information

Assistance will be provided by the Department of Environmental Safety to any Department requiring

help and advice in its implementation of this UM policy.

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Appendix II

Prior Approval Criteria

The LS/PI shall indicate any circumstances under which a particular laboratory operation,

procedure or activity shall require prior approval from the LS/PI (or designee) before

implementation. If no circumstances are identified, the LS/PI shall write “none” in the first

provided space. Additional pages may be added as determined necessary by the LS/PI.

1. Circumstance: Introduction of any new chemicals (solid, liquid or gas) not listed on

the lab chemicals inventory. To be approved by the lab manager, the requester will have to

supply all necessary documents for safe operation, including Materials Safety Data Sheets and

Standard Operating Procedure if needed.

Prior approval to be obtained from: Lab manager

2. Circumstance: Installation/removal of any new piece of equipment.

Prior approval to be obtained from:_Lab manager

3. Circumstance: Repair of lab equipment. Notice: no lab users are allowed to perform

electrical work involving voltages above 24V.

Prior approval to be obtained from:_Lab manager

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4. Circumstance: Installation / replacement of gas cylinders.

___________________________________________________

Prior approval to be obtained from: Lab manager

5. Circumstance: “Plumbing” work on existing gas supply lines. Opening any gas line in

LAMP is strictly forbidden in the absence of the lab manager.

Prior approval to be obtained from: Lab manager

6. Circumstance: Maintenance of process vacuum pumps. Opening a pump for

maintenance (e.g., oil change) can present serious hazards due to the potential

presence of the residual toxic gases.

Prior approval to be obtained from: Lab manager

7. Circumstance: _______________________________________________________

___________________________________________________________________

___________________________________________________________________

___________________________________________________________________

Prior approval to be obtained from:______________________________________

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Appendix III

Standard Operating Procedures

(to be attached by Laboratory Supervisor)

Notice: Standard Operating Procedures are listed on the LAMP website at

http://www.enma.umd.edu/LAMP/lamp_SOPs.htm

These documents include:

- LAMP general operating procedure and guidelines is a 51 slide power point document

providing general guidelines and procedures when working in LAMP. It reviews

LAMP access procedure, operating hours, personal protective equipment

requirements, work with chemicals, chemical waste management, authorization for use

of equipment, general safety and emergency procedures.

- LAMP SOP for process gases is a 17 pages pdf document that provides a review of

safety features and emergency procedures related to the use of semiconductor process

gases in LAMP. It details gas detection units, sensor integration and alarm protocols,

procedures to install or replace gas cylinders.

- LAMP emergency table is a one page pdg file that summarizes the types of safety and

gas detection sensors, their locations, the associated alarm protocol and the procedure

to disengage these alarms.

- Hydrofluoric acid SOP

- Piranha solution SOP

- PZT sol gel materials SOP

- Handling of tungsten hexafluoride WF6 gas manifold SOP

- MAS 400 mask aligner SOP

- Automated four point probe station SOP

A printout of all these SOPs is located in LAMP, in the Chemical Hygiene Plan binder located

on the access door to the clean room.

Lab users must follow safety guidelines listed on LAMP website at

http://www.enma.umd.edu/LAMP/safety.htm

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Standard Operating Procedure #1

LAMP General safety guidelines Facility: Laboratory for Advanced Materials Processing 2225 JM Patterson bldg, Materials Science and Engineering University of Maryland, College Park MD 20742 (301) 405 7250 Lab Director: Gary Rubloff 2145 AV Williams Bldg (301) 405 2949 Lab Manager: Laurent Lecordier 2147 AV Williams Bldg (301) 405 5858, cell (301) 602 9858 Scope: This SOP reviews the general safety issues related to the work in LAMP as well as emergency

procedures and chemicals handling and disposal.

This SOP is adapted from the content of the safety guidelines on the LAMP website at http://www.enma.umd.edu/LAMP

Last revision: 09/08/04 by Laurent Lecordier

Safety is paramount in LAMP. Due to the nature of semiconductor and microsystems processing, activities within LAMP must be undertaken with extreme care and a full understanding of all proper safety procedures. Violations of safety protocols will result in temporary expulsion from the lab. Permanent expulsion will result from gross negligence of the safety rules. This can mean serious delays or even the end of your thesis. You have been warned!

Outline of the LAMP safety reference guide

1- Before you begin: link to safety overview documents: general concepts about chemical handling, storage and disposal 2- "The 10 Commandments of LAMP" 3- General rules of operation for the LAMP cleanroom: rules that must be followed by any user of the clean-room facility 4- Safety policy 5- Emergency procedures 6- Chemicals safety issues 7- Gas safety issues

There are several important online safety resources you must be aware of:

• The University of Maryland Department of Environmental Safety (DES)

• Online Material Safety Data Sheets ( MSDS) from the University of Maryland website and our MSDS web page where you can retrieve MSDS for the chemicals used in LAMP.

This guide is intended to help in understanding proper chemical handling and basic cleanroom safety issues. It also present important issues related to the use of hazardous gases in LAMP. Every user of the LAMP facility must take the following training:

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• Take the DES New Laboratory Researcher Training course - required training for all new laboratory research personnel, including information on applicable regulations and guidelines, recommended work practices, selection of personal protective equipment, and proper disposal of hazardous chemicals and biological waste. This training is offered every month.

• Take the DES Chemical Hygiene Training course - All personnel who work with chemicals in laboratories are required to have Chemical Hygiene Training. For your convenience, this training class is offered on-line (see the DES web page).

• Read carefully this LAMP Safety Reference Guide , the safety overview document and the LAMP general operating procedures and guidelines.

• Pass the LAMP safety quiz.

• It is also strongly recommended to attend the Safety workshop offered annually at the start of the fall semester by DES, as well as to take the on-line training for Hazardous Waste Management.

1. Before you begin:

Carefully read the safety overview document . This guide offers general safety notes when working in a clean room, especially about chemical handling and storage.

2. The "10 Commandments of LAMP"

• Safety is non negotiable. Safety must be your primary concern at all time.

• Be proactive about safety. If you see a safety hazard, you are responsible to report it to the lab manager even if it implies other users of the lab. Each person have the right to question a procedure that he/she considers inherently unsafe.

• Never leave the lab without cleaning or in unsafe conditions

• If you break something, you must report it. Occasional accidents are understandable and forgivable. Secrets or continuing mal practice are not acceptable

• Never assume that other users are knowledgeable about your activities. Make sure to clearly label or mark any recipient, chemical solution, source of potential hazard... you leave unattended (even for a few minutes).

• Each user must take responsibilities in the training and organization of the lab. It is everyone's responsibility to maintain LAMP in order. If you see something wrong, do not assume somebody else will fix it for you.

• Learn from your colleagues and teach them in return.

• Document your activities or problems in the log books put at your disposition in LAMP.

• Report ideas to improve work in LAMP

• Most of all, respect other people's work. Your work is valuable so is other people's work! Be clean, be safe, be considerate and professional.

3. General rules of operation for the LAMP

(adopted from the Cornell CNF, CAMD & Micralyne ) :

In this section, you will find general rules that must be known and applied by any users of the LAMP facility. More details regarding chemicals and gas handling can be found in the section 5 and 6 of this guide.

• Dress code and general issues

• Inside the cleanroom clothing, shoe covers, Tyvek coat (or bunny suit if you are wearing a short or skirt), hair net must be worn at all time.

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• Gloves and safety glasses must be worn all the time when you are in the cleanroom, no matter what you are doing.

• No Sandals and open-toed shoes.

• Smoking, food, drinks, chewing-gum are prohibited anywhere in the LAMP facility (cleanroom and pre-cleanroom). They all are huge sources of dust and can present serious safety risks.

• Torn or dirty coats and shoe covers must be discarded after use. Hair nets are not to be reused.

• It is not allowed to leave the facility wearing the garments

• Use of equipment

• Non-authorized users are not allowed to work on any of the cleanroom equipment. To be authorized to work on a specific piece of equipment, you must imperatively contact the tool supervisor in charge (see LAMP Management Team)

• General storage

• Because cleanroom space is a premium, make sure to follow these rules or your items will be discarded without notice.

• Tools, samples and other small belongings can only be stored in the yellow plastic boxes that have been allocated to your group and stored on the metallic shelves in the cleanroom. If you need additional storage space inside the cleanroom, you must contact the LAMP manager.

• Additional storage space is also available in the LAMP annex (room 2229). As in the cleanroom, specific spaces have been allocated to each group. All items there must be labeled with name, date and phone extension or they will be taken out of the annex.

• Chemicals storage For safety concerns, chemicals inventory is managed by a student supervisor (see LAMP management). He will make sure that all the Materials Safety Data Sheets and product inventory are up to date. You must get the approval of the lab manager or the student in charge of the chemical inventory before importing any new chemicals in the LAMP facility. The chemicals inventory is divided into 2 main categories:

• chemicals for general use that are shared by all the groups (i.e. acetone, methanol, DI water, nitrogen gas...). The supervisor in charge of the chemicals will manage the supply of these chemicals. You are welcome to contact him if re-supply is necessary.

• chemicals that are used specifically by a research group. After pre-approval, chemicals brought to LAMP must be very clearly labeled with the name of chemicals, the date of introduction and the user name. Make sure they are stored safely in the designated area.

• Wet processes and other work in LAMP

• Never use specific chemicals, glassware or other equipment that are used and labeled by another group.

• Always clean up your work area before you leave. Thoroughly rinse the beakers you used with DI water and then store upside-down in their appropriate locations.

• Wash thoroughly any chemical bottle you used. Use cleanroom wipes to dry and then store in the appropriate cabinet.

• Label all the glassware or fluoroware you are using and specify the contents, your name and the date. If you have to leave the area for a little while, let people know what you are doing in the cleanroom and what chemicals are in the beakers. This also goes for any processing that needs to be carried out over night or more (leave a written note at the work station indicating your return time, a contact name and phone

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number).

• Chemicals disposal

• All disposed items have to be labeled with the name(s) of chemical(s), the date of disposal and the name of user. If you use recyclable bottle, make sure you remove or scratch away old label.

• Thoroughly rinse empty chemical bottles with regular tap water. Fill and dump at least 3 times. Put a scratch through the original label and mark it with "WASHED BOTTLE" and place in the designated area beneath the eye wash station.

• No unauthorized solutions

• No unlabeled solutions

• No chemicals in waste baskets

• No unwashed bottles in waste baskets

• Never touch exposed skin with your gloves, avoid transfer of oils to the glove surface.

The above rules are essential for maintaining normal cleanroom operation. Any one violating the rules will be subject to a warning, suspension of access to cleanroom for one month, or loss of privilege to work in the cleanroom altogether.

Short and Simple Consequences: You can lose access to the LAMP facility if you violate any safety rule or cause injury or damage to persons or equipment.

4. Safety Policy

All LAMP users are encouraged to report all incidents, near misses, and unsafe acts they encounter while working at the lab. It is not intended to criticize or 'pick on' any person. By reporting these incidents, corrective actions may be recommended to prevent similar or more catastrophic incidents from happening. "Incident Report" forms are available in the cleanroom. Notify the lab manager by sending an e-mail.

Incident Report

Date: Name:

Report:

5. Emergency Procedures

5.1 Emergency procedure resulting from the leak of silane (see gas safety issues)

As in most semiconductor research facilities, LAMP houses a variety of hazardous gases. Therefore it is equipped with an integrated alarm system that includes a MDA System 16 gas detector (located in front of the middle door in the hallway). This system can detect traces of silane, a highly ignitive gas, at concentration as low as 2 ppm in four different locations of the LAMP facility. It also integrate other sensors (HF, H2, overpressure, overflow...) to provide an appropriate alarm response. If a positive detection occurs, the MDA system 16 will automatically activate the J.M. Patterson building alarm and notify the UM police department. 2 red flash lights inside LAMP will also be triggered.

In case of such an alarm, anyone present in the lab must:

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1. Evacuate the LAMP facility IMMEDIATELY.

2. If the building alarm is not already sounding, pull the manual emergency station located in the hallway for general evacuation of the building.

3. Call 911 to confirm that they have been notified by the automated supervisory unit.

4. Call the lab director (Gary Rubloff @ 301 405 2949) and Laurent Henn-Lecordier @ 301 602 9858 (cell) or 55858 (office).

The LAMP facility is equipped with an emergency push button located to the left of the main entrance door that can be activated manually. By pushing this button, the J.M. Patterson building alarm will be triggered and the UM police department automatically notified.

Please make sure to review the paragraph related to Gas safety issues.

5-2 General emergency procedure

• In case of fire

Pull fire alarm and follow evacuation procedures Notify LAMP staff

• Injuries

All injuries should be immediately reported to the LAMP staff All users are expected to cease work to assist an injured user. If large chemical exposure is involved, another user must accompany the injured person to the hospital emergency. If deemed necessary, phone 911 and request an ambulance to be sent to the J.M. Patterson bldg (083), room 2225 An incident report must be completed ("Incident Report")

• Chemical Spills and Exposure

In the event of chemical spill, first ensure that all injuries are being treated. If chemical exposure (skin, eyes, etc.) has occurred, immediately get to a source of water, remove contaminated clothing, and flush the contaminated area thoroughly for at least 15 minutes. Then, depending on the size of the spill, do one of the following:

1. If the spill is small enough, then qualified personal may clean it up themselves at their discretion. The incident must be reported ("Incident Report").

2. If you feel that the spill is large enough to warrant LAMP staff response:

• Evacuate the immediate area.

• Clearly mark the area to prevent other users from accidentally entering the spill area. If there are no sufficient tools for marking the area, recruit another user to stand as a "lookout" near any ingress route until LAMP staff (or qualified persons) arrive.

• Show LAMP staff the exact area of the spill and the nature of the spill

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• Fill out the incident report form ("Incident Report").

• If at any time a spill is deemed to be a serious hazard to other building personnel (due to size, fire, toxic threat), pull a fire alarm to evacuate the building.

NB: Make sure that you are aware of the locations of eye wash station and emergency shower before working with hazardous chemicals.

6. Chemical Safety Issues

• Authorization

Only persons who have been trained to handle chemicals at LAMP may use chemicals in the facility.

• Material Safety Data Sheets

MSDS sheets for each chemical we use at LAMP are available (MSDS sheet binder) in the cleanroom area or online for download. If importing a new chemical into the facility, MSDS sheets need to be obtained before purchasing the product. (Link for Online MSDS info).

• Wet processing areas

All the wet etch processes that have been approved by the lab Manager should be done in the wet deck.

• Working with etch solutions requires a "Buddy system"

While working with or preparing chemical etches and baths, another user (Buddy System) must be within range of verbal contact for the purpose of immediate emergency response. For solutions containing HF, another user who has been approved to work with HF, must be in the room.

• Importing chemical into LAMP

No chemical may be brought on-site without prior approval by the manager. The lab manager and the user must determine the safety concerns associated with the chemical (if any) and develop procedures for safely working with this chemical.

• Developing new wet processing recipes

There are inherent dangers when developing new etch recipes. Chemical can react in unexpected ways that can create dangerous situations (causing injury, death to users and damage to equipment). If a new process is needed, you must abide by the following procedures:

1. If the recipe is significantly different than those used previously in the lab, the lab manager must be informed (verbally). You need this approval for any significant recipe modifications.

2. Before mixing any chemicals, it is your responsibility to look into any reactions that might take place (intentionally or by accident).

3. When you first mix the new recipe, use first small volumes (<50 ml) of solutions or additives. This will ensure that if the chemicals react in unforeseen ways, the possible explosions or gas releases are small.

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• Chemicals: Storage and Handling

• a-Storage

Table 1 below lists some of the more common chemicals used in the lab and their concentrations. Many of these chemicals can cause severe damage to human tissue and life. Therefore, you must be alert and cautious when using these chemicals to avoid all "direct" contact with them. The risk of injury will be minimized if the safety procedures are followed. Acids, bases, and solvents must be stored in separate marked cupboards.

Chemical Type Chemical name Formula Concentration

Hydrofluoric Acid HF 49%

Hydrochloric Acid HCl 36%

Nitric Acid HNO3 HNO3 68%

Sulfuric Acid H2SO4 H2SO4 96%

Acids and Oxidizers

Hydrogen Peroxide H2O2 30%

Bases Potassium Hydroxide KOH 45%

2-propanol CH3CHOHCH3 100%

Acetone CH3COCH3 100% Solvents

Methanol CH3OH 100%

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Table1: Concentration of common chemicals in the microfab

• b-Handling

1. Users who handle hydrofluoric acid or HF-containing solutions (BOE) must be authorized by the lab manager prior to handle these chemicals.

2. Know which chemicals and containers are compatible. Some chemicals or mixtures can not be used in plastic (hot Piranha) or in glass (HF).

3. Always work with chemicals under fumehood.

4. Heavy-duty rubber gloves, chemical apron and a face shield must be worn when handling hazardous chemicals.

5. When mixing chemicals, use only one bottle at a time. Do not open a new bottle unless an existing bottle is completely empty. Pour the chemical slowly. Do not let it gulp. Remember the triple A rule: Always Add Acid to water never do the reverse. This prevent violent splashing.

6. DO NOT mix organic solvent with inorganic chemicals. This can result in violent reaction or explosion.

7. Never work with acids and bases side by side because violent reactions can occur.

8. DO NOT pour chemicals back into the storage bottle. If you pour too much, dispose of it appropriately.

9. Put the cup back on each chemical bottle securely.

10. Be Cautious all times !!. Because most chemicals used in the lab look like water, always assume any liquid is dangerous if not labeled.

11. Table 2 lists some of the flammable chemicals encountered in the cleanroom.

12. When using hot-plates, check that your beaker is both suitable for hot plate use and smaller than the area of the plate.

13. Always monitor the temperature of the chemicals on a hot-plate with a Teflon coated thermometer.

14. Rinse the heavy chemical gloves with DI water before you take them off.

15. Never touch your skin (face) with your gloves on.

16. A fire extinguisher is located outside the cleanroom. The eye wash station and emergency shower are located in the cleanroom..

17. Hydrofluoric acid (HF) is more dangerous than it seems. Because HF does not hurt when it makes contact with skin, people get careless. READ carefully the Standard Operating Procedure related to hydrofluoric acid prior to any work involving this chemical. Calcium Gluconate Gel is available to treat HF burns. You will find it in the First Aid Kit located next to the lab entrance door.

• Chemicals: Waste Disposal

Contact the student in charge of waste disposal. For general information on Hazardous and regulated waste procedures, please check the DES website.

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Please be aware that the disposal of hazardous waste down drains, sinks, etc. is prohibited.

1. Waste Containers

• Hazardous waste must be collected in containers that are compatible with the waste.

• Keep all hazardous waste containers closed at all times unless you are adding or removing waste.

• Label each container of hazardous waste with the UM Hazardous Waste Green Tag when you first place waste into a container.

• Do Not store incompatible waste containers side by side

• You may use a washed bottle as a waste container. Make sure you wash it thoroughly to remove all the previous chemicals and scratch away the original label.

2. Waste Pickup

• Request Waste Pickup system via the DES web page.

• You must take the online Hazardous waste generator training before submitting any waste pickup request.

3. Unknown or Unlabeled waste Please be aware that:

• It is the responsibility of each individual generator and department to properly label hazardous materials and identify containers of hazardous waste at the time accumulation begins.

• DES will identify, remove, and dispose of unknown wastes for on-campus waste generators. However, the generator or generating department will incur a $110.00 per bottle fee for all solid and liquid unknown wastes.

• DES will also arrange for a contractor to sample, analyze, and dispose of any unknown cylinders. The generator or generating department will incur the full costs of the contractor's services, which can exceed $2,000.00 per cylinder.

4. Procedure for HF disposal

HF is a very Hazardous chemical. Any person who uses it must receive a special training and authorization. The binding of free fluorine ions with Calcium has been recommended for HF neutralization. Calcium chloride can be used to neutralize HF in 6 parts to 1 part of HF.

• Small amount of HF (<75 ml) can be poured down the drain as long as it is neutralized (with CaCl2) and diluted with large amount of water.

• While neutralizing the HF solution, DO NOT add the two reactants together directly. The reaction will be reasonable vigorous and toxic gas may be released.

• You must know that BOE is not a dilute HF. The ratio given on the BOE container is buffer to HF, so the fluorine content is the same as in HF for any ratio. For this reason, the same amount of Calcium Chloride must be used when neutralizing BOE as when neutralizing HF.

• Large amounts of HF solutions (>75ml) must be collected in a plastic container, properly labeled as a hazardous waste.

• Do not completely fill up the waste container with HF solution.

• Store the waste container in the designed safe area.

• Call for waste pick up

5. Piranha Hazards

A piranha is used to remove organic residues from substrates. Two different solutions are used. The most common is the acid piranha: a 3:1 mixture of concentrated sulfuric acid (H2SO4) with hydrogen peroxide (H2O2). Also used is the base piranha: a 3:1 mixture of ammonium hydroxide ( NH4OH) with hydrogen peroxide (H2O2). Both are equally dangerous when hot, although the reaction in the acid piranha is self-starting whereas the base piranha must be heated to 60 degrees before the reaction takes off. There are many things which will cause the reaction to accelerate out of control. "Out of control" can mean anything from the piranha foaming out of its bin and on the deck, to an

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explosion with a huge shock wave including glove and acid-gown shredding glass sharps. Piranhas burn organic compounds. If you provide sufficient fuel for them (i.e. photoresist, IPA), they will generate enormous quantities of heat and gas.

Important safety notes:

• Never store piranha. Leave it in an open container until completely cool. Then aspirate the cool solution. A piranha stored in a closed container will explode.

• Hot piranhas explode when mixed with acetone and other organic compounds. This includes IPA, photoresist, and anything made out of nylon like spinner and developer chucks.

• If you put any acid (i.e. chrome etch) in the base piranha; it will accelerate due to the heat generated.

• Likewise, if you put any base (i.e. developer solution) in the acid piranha, it will accelerate.

• Photoresist developer is a strong base. It can cause blindness if left in the eye, and can react violently with acids. Be extremely careful in working with developer.

• Water sprayed into either piranha will accelerate the reaction. A single wet wafer doesn't introduce enough water to make a difference, but a boat with 25 wet pieces of glass could.

Instructions for safe use of Piranha:

• Substrate should be rinsed and dried before placing them in a piranha bath. Piranhas are used to remove photoresist and acetone residue, not the compounds themselves.

• Do not store wash bottles containing organic compounds on the piranha deck.

• No crystal bond stripping on the piranha deck.

• No Photoresist stripping near piranha deck.

• Cold acid Piranha can be used to clean glass Chromium photomasks

7. Process Gas Safety Issues

At the exception of nitrogen which is shared by all the users of the lab, other gases are administered by each group for their own needs. Nevertheless because of safety concerns, importing new gas cylinders into LAMP must be approved in advanced by the lab manager.

As explained in the section 5 of this guide (emergency procedures), hazardous gases are used in this lab and therefore every person working in LAMP should be clearly aware of the emergency procedure resulting from an accidental gas release.

MSDS sheets for each gases we use at LAMP are available (MSDS sheet binder) in the cleanroom area. If importing a new chemical into the facility, MSDS sheets need to be obtained before purchasing the product. (Link for Online MSDS info). The MSDS for the gases currently used in LAMP can be viewed at the following link.

Users of LAMP who are directly handling these gases should also read the following Standard Operating Procedures for the use of gases in LAMP. This SOP offers a detailed description of the alarm system put in place in LAMP to detect and annunciate the presence of hazardous gases.

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Standard Operating Procedure #2

Tungsten hexafluoride (WF6) process gas

Facility: Laboratory for Advanced Materials Processing

2225 JM Patterson bldg, Materials Science and Engineering

University of Maryland, College Park MD 20742

(301) 405 7250

Lab Director: Gary Rubloff

2145 AV Williams Bldg

(301) 405 2949

Lab Manager: Laurent Lecordier

2147 AV Williams Bldg

(301) 405 5858, cell (301) 602 9858

Scope: This SOP reviews the main safety issues related to use of tungsten hexafluoride gas as

well as the procedure to install/remove a WF6 cylinder

This SOP is adapted from the content of the WF6 SOP listed in the LAMP

website at http://www.enma.umd.edu/LAMP

Last revision: 07.21.2006 by Laurent Lecordier

1- General notice

1. Any handling of WF6 must be authorized by the lab manager and the lab manager must be present in the lab at the time of the operation. This includes any activities taking place within the gas cabinet (which include cylinder installation or cycle purge of the gas lines) as well as certain activities on the process tool itself such as opening a gas line which has be exposed to WF6 upstream or downstream to the tool.

2. Make sure the WF6 gas cabinet is kept closed at all times.

3. Tungsten hexafluoride WF6 is a toxic, corrosive, nonflammable liquefied compressed gas with a 2.4 psig vapor pressure at room temperature (884 Torr). The gas is colorless but fumes white in moist air. It hydrolyses to very corrosive hydrofluoric HF on contact with moisture. You must review very carefully the WF6 Materials Safety Data Sheet before doing any work involving this gas.

4. WF6 is used in CVD processes to deposit tungsten films, either from the H2 or SiH4 - silane - reduction processes. In contact with moisture, it hydrolyses: WF6+H2O => WOF4+2HF

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The WOF4 tungsten oxide is a white solid at room temperature. Further hydrolysis of WOF4 can produce yellow WO2F2, and WO2F2 can itself hydrolyses to WO3. WOF4 and WO2F2 have a high vapor pressure and will easily sublimate if appropriate heating is provided. However if WO3 is formed, mechanical cleaning of the line is necessary. A thorough downstream N2 purge should be used. Heating the gas lines will allow to keep WOF4 and WO2F2 in the vapor phase and therefore to keep the lines cleaner.

5. WF6 used in LAMP is Semiconductor grade (99.9%) and comes from a 15 lbs D size cylinder from Air Products. A 20 gallon Novapure S407 gas scrubber resin is used downstream to the process pumps in order to convert process gases and byproducts into non-volatile solids. Always check that the scrubber is on before using WF6 and that the pressure to the scrubber pneumatic valves are at least 60 psig (otherwise the valves will not open).

6. Breathing protection (full mask respirator) is required for changing WF6 or when assembling/disassembling gas delivery lines. An HF Lifeline sensor should also be available. Tagouts must be used to notify users of potential risks if the system is under construction/modification. Gas lines that are susceptible to house WF6 (pure or diluted) must be clearly marked. .

7. At least 2 knowledgeable users must be present whenever working with WF6, either during regular process, construction phase or any maintenance activity such as pump oil change .

2 - Process gas handling procedures

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To MFC and Process chamber

WF6

Process pumps

Scrubber

MFCs

Venturi vacuum

generator

Hex cylinder manual valve

Vented WF6 gas cabinet

¼ turn open/close manual valve

Manual valve

Pneumatic valve connected to gas interlock pannel

Pneumatic valve

N2

Regulator

VS1

VS2VS3

PV PV

VS4

VS5

VS6

WF6 gas cabinet – 07/21/2006

Exhaust to roof stack

Notice:

For the Venturi vacuum generator to work properly, the dedicated nitrogen

inlet pressure upstream to the generator must be at least at 120 psi. If the

pressure is below 120 psi, the Venturi will not operate properly and the

vacuum will be insufficient.

2.1 Gas cylinder receiving

Delivery of SiH4 and WF6 cylinders will be coordinated with the supplier (Air Products) and received at the rear entrance of the JM Patterson Building. Before entering the building the cylinder will be inspected for signs of a leak (discoloring or residue) and then will be transported to the LAMP facility and placed in a cabinet until installation.

2.2 First time installation of new cylinder

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This procedure is for installation of a new cylinder on to gas system which has not been previously used with process gases.

2.2.1 Cycle purge and leak check process line

Pump out the line upstream of the regulator using through the process tool.

a) Pump the chamber thru the turbo and monitored by the ion gauge. b) Close VS4 c) Open the process valves (PVs) and set the MFC to full open. d) Pump on the reactor chamber using the turbo pump. e) After reaching a base pressure (pump for at least 15 minutes) at the ion gauge, close the process valve immediately down stream of the MFC. f) After approximately 60 sec open this valve and monitor the effect at the ion gauge.

· A significant pressure jump MAY signify be a leak in the process plumbing. If this is observed, repeat the test after pumping on the chamber for another 15 minutes.

2.2.2 Installing and activation new cylinder

Step 1: Connect the cylinder to the gas panel

a) Secure cylinder in place in the gas cabinet b) Remove cylinder cap c) Install the pig tail and make sure all the valves are closed

Step 2: Cycle purge the gas panel

Starting with all valves closed.

a) Open VS5 to start N2 flow through the venturi element to generate a vacuum at VS2. b) Open VS3 and set the regulator open to near full pressure delivery. c) Open VS1 fill the panel with purge N2 and then close VS1. d) Open VS2 to evacuate the panel, checking for a pressure drop to near 30" Hg at the regulator low P side. e) Close VS2. f) Repeat steps c and d AT LEAST 15 times. g) Complete this procedure with step d. h) Leave the system for overnight noting the pressure at the regulator gauge. i) If the next day the pressure has not rised, close VS3 and proceed to the next step.

Step 3: Cycle purge the process line.

Deliver N2 to the process line from the purge cylinder.

a) Open VS1 to apply pressure to the panel. b) Open VS3 and set pressure at regulator to ~ 10 psi. c) Open VS4 to pressurize the process line with the purge N2. d) Close VS4. e) Put the WF6 MFC in full open and open the upstream PV. f) Open the By-Pass PV to evacuate process line back to the cylinder valve VS4. g) Close the By-Pass PV. h) Open VS4 to fill the process line, then close VS4 i) Repeat steps f through h at least 10 times. j) End the process with step g, evacuating the process line. k) Cycle Purge the panel (see above Step 2) and leave in evacuated state.

Step 4: Open the cylinder

Start with all valves closed. Verify that downstream process valves are closed.

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a) Verify that the electronic switch for the main cylinder valve is OFF. b) Open the WF6 main cylinder valve at the remote panel. c) Open VS3 and check pressure at the panel regulator. d) Open VS4.

2.3 Switching cylinders

2.3.1 Removal of used cylinder

Verify that the gas cylinder main valve is closed.

Disconnect the air line to the pneumatically operated main cylinder valve.

Step 1 Cycle purge the panel.

Starting with all valves closed.

a) Open VS5 to start N2 flow through the Venturi element to generate a vacuum at VS2. b) Set the regulator open to near full pressure delivery. c) Open VS2 to evacuate the panel, checking for a pressure drop to near 30" Hg at the regulator low P side. d) Close VS2. e) Open VS1 to fill the panel with purge N2. f) Close VS1. g) Repeat steps c and d AT LEAST 10 times. h) Open VS1 and pressurize the panel with purge gas to provide outward purge flow when the pigtail connection is disconnected.

Step 2 Disconnect and remove the used cylinder

a) VERIFY that the pneumatic air line to the main cylinder valve is disconnected or that the valve is closed (if manual valve). b) Slowly loosen CGA cylinder fitting and disconnect. c) Place cap over cylinder valve. d) Remove cylinder and store for pick-up.

2.3.2 Installation of new cylinder

Step 1: Connect the cylinder to the gas panel

e) Secure cylinder in place in the gas cabinet f) Remove cylinder cap g) Attach the pigtail fitting to the cylinder.

Step 2: Cycle purge the gas panel

Start with VS1 open, all other valves closed.

a) Open VS5 to start N2 flow through the venturi element to generate a vacuum at VS2. b) Open VS3 and set the regulator open to near full pressure delivery. c) Close VS1 d) Open VS2 to evacuate the panel, checking for a pressure drop to near 30" Hg at the regulator low P side. e) Close VS2. f) Open VS1 g) Repeat steps c and d AT LEAST 10 times. h) Complete this procedure with step e (panel evacuated). i) Leave the system overnight noting the pressure at the regulator gauge. [A pressure rise is associated with a leak in the panel or the CGA connection.]

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j) If no signs of a leak is detected, proceed to step 3.

Step 3: Open the cylinder

Start with all valves closed. Verify that downstream process valves are closed.

a) Verify that the electronic switch for the main cylinder valve is OFF. b) Open the WF6 main cylinder valve at the remote panel. c) Open VS3 and check pressure at the panel regulator. d) Open VS4.

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Standard Operating Procedure #3

Hydrofluoric acid (HF) and other HF-based solutions

Facility: Laboratory for Advanced Materials Processing

2225 JM Patterson bldg, Materials Science and Engineering

University of Maryland, College Park MD 20742

(301) 405 7250

Lab Director: Gary Rubloff

2145 AV Williams Bldg

(301) 405 2949

Lab Manager: Laurent Lecordier

2147 AV Williams Bldg

(301) 405 5858, cell (301) 602 9858

Scope: This SOP reviews the main safety issues related to the use of hydrofluoric acid.

This SOP is adapted from the content of the hydrofluoric acid SOP listed

on the LAMP website at http://www.enma.umd.edu/LAMP

Last revision: 09/08/04 by Laurent Lecordier

1- General notice

(These are not authorized official regulations for general use of HF and HF-based solutions.

But, these are valuable rules to protect your safety and everyone should follow these rules

whenever using HF in the LAMP cleanroom.)

5. Before you start, read the Material Safety Data Sheet for hydrofluoric acid carefully as

well as of solutions containing HF such as Buffered Oxide Etch (BOE)

(http://www.enma.umd.edu/LAMP/lamp_msds.htm).

More details about medical treatment for HF exposure available here (pdf format)

Additional safety information is also listed in the Lab Safety section of this web site.

6. Hydrofluoric acid is not like any other acids. It is considered as extremely hazardous either as a liquid or vapor. HF can cause severe burns which can take

up to 24 hours before being visible or painful. However it will readily be absorbed

into the skin and bind with calcium and magnesium to form insoluble salts. These

insoluble salts will interfere with cellular metabolism, causing cellular necrosis

and death.

7. You must know that BOE is not a dilute HF. The ratio given on the BOE container is

buffer to HF, so the fluorine content is the same as in HF for any ratio

8. Any LAMP users who want to use HF or HF-based solution such as BOE must be

qualified and authorized by the lab manager prior to do any work.

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9. During the qualification process, the lab manager will insure that the Materials Safety

Data Sheets for HF-based chemicals have been carefully read and understood, and that

the procedures detailed in this SOP are thoroughly followed.

10. The list of the authorized users is published on this web site. If your name is not on

this list, you are not allowed to use HF or HF-based solutions at any time.

11. Any accident regarding the use of HF must be reported without delay to the lab

manager.

2 - Protection equipment

1. The handling of HF solutions require special protection equipment in addition to the regular

clean room protection outfit (see Lab Safety page) .

2. The additional protective equipment include: a full face shield, PVC or neoprene gloves

(regular Nitrile gloves used in LAMP will not provide sufficient protection), as well as a PVC

acid apron to wear on top of the lab coat.

Gloves are located in the acid cabinet, apron and mask are available in the fitting room.

3. As a reminder, open-toed shoes are not allowed when working in the lab and bare legs must

be covered by wearing a full size bunny suit.

3 - HF handling

3. HF solutions, as well as any corrosive or hazardous substances, can only be used in

LAMP during operational hours (9 am to 6 pm, Monday to Friday) and requires at all

time the presence of a second knowledgeable user (buddy system).

4. HF vapors are extremely hazardous. Therefore HF solutions can be only handled under

the flow hood dedicated to work with chemicals.

5. Whenever handling HF, all containers used during the experiment must be very clearly

labeled and a warning sign, visible by any user working under the flow hood, must be

posted at all time to indicate that the solutions contains HF.

6. After completion of the work, the user will insure that all surfaces in contact with HF

have been carefully rinsed with DI water and blown dry. The user must also insure that

the HF bottle is perfectly dry before being stored in the acid cabinet.

4 - HF waste disposal

4. You must know that BOE is not a dilute HF. The ratio given on the BOE container is

buffer to HF, so the fluorine content is the same as in HF for any ratio. For this reason,

the same amount of Calcium Chloride must be used when neutralizing BOE as when

neutralizing HF.

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5. HF solutions or BOE must be collected in the dedicated plastic containers, located on

the tray next to the flow hood

6. Do not completely fill up the waste container with HF solution.

7. The waste containers will be discarded by the student in charge of the waste

management according to DES waste management procedure.

5 - Emergency procedure

18. As stipulated earlier HF solutions are considered extremely hazardous because their

effects are not immediate and the fluoride ion will penetrate the skin causing

destruction of the deep tissue layers and even bone. It has been reported that as little as

7 ml of anhydrous HF in contact with the skin untreated can bind on the calcium in a

normal size adult.

19. In case of large exposure, the victim should be removed from the contaminated area,

placed under a safety shower while emergency personal is contacted (911)

In any case, even if the burn appear initially minor, you must seek immediate medical

attention. A copy of the MSDS that contains a note to the physician should be brought

with you.

20. All contaminated clothing should be removed immediately with appropriate gloves

and safely discarded.

21. In case of contact with the skin, the affected area must be immediately rinsed with

large amounts of water for at least 15 min. However washing off the skin will not be

sufficient. A calcium gluconate gel contained in a white tube is available in the LAMP

facility (in the First Aid box located to the right of the lab entrance door). The gel

should be massaged over the affected area. When applying the gel, the washing with

water can be reduced from 15 to 5 min. The gel should be reapplied at regular

intervals.

22. In case of contact with the eye, irrigate the eye for at least 30 minutes, keeping the

eyelids apart and away from eyeballs during irrigation. Place ice pack on eyes until

reaching emergency room.

6 - Supply and storage

1. In order to limit the number of HF containers in the lab, all solutions containing HF are

supplied by the lab. If for specific research purposes, you need your dedicated source of

hydrofluoric acid, you must request the authorization from the lab manager first.

2. Supplied HF solutions are typically diluted to 37%. If you need to adjust this concentration,

you will supply your own container for storage, a polyethylene bottle with a positive closure

(never store in a glass container since HF attacks glass and other silicon containing

compounds)

3. All HF-containing solutions will be stored in the acid cabinet located under the flow hood.

It is not allowed to leave the lab with a HF solution left on the bench top under the flow hood.

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4. If you notice that the supply of HF or BOE is running out, contact the student in charge of

chemicals inventory (do not wait the last minute though since it can take up to 4 weeks to

renew the supply)

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Standard Operating Procedure #4

Piranha solution

Facility: Laboratory for Advanced Materials Processing

2225 JM Patterson bldg, Materials Science and Engineering

University of Maryland, College Park MD 20742

(301) 405 7250

Lab Director: Gary Rubloff

2145 AV Williams Bldg

(301) 405 2949

Lab Manager: Laurent Lecordier

2147 AV Williams Bldg

(301) 405 5858, cell (301) 602 9858

Scope: This SOP reviews the main safety issues related to the use of Piranha solution.

This SOP is adapted from the content of the Piranha solution SOP listed

in the LAMP website at http://www.enma.umd.edu/LAMP

Last revision: 09/08/04 by Laurent Lecordier

1 - General notice

1. A piranha is used to remove organic residues from substrates. Two different solutions are used. The most common is the acid piranha: a 3:1 mixture of concentrated sulfuric acid (H2SO4) with hydrogen peroxide (H2O2). Also used is the base piranha: a 3:1 mixture of ammonium hydroxide ( NH4OH) with hydrogen peroxide (H2O2). Both are equally dangerous when hot, although the reaction in the acid piranha is self-starting whereas the base piranha must be heated to 60 degrees before the reaction takes off. [1] There are many things which will cause the reaction to accelerate out of control. "Out of control" can mean anything from the piranha foaming out of its bin and on the deck, to an explosion with a huge shock wave including glove and acid-gown shredding glass sharps. Piranhas burn organic compounds. If you provide sufficient fuel for them (i.e. photoresist, IPA), they will generate enormous quantities of heat and gas. [1]

2. Any LAMP users who want to use Piranha solutions in LAMP solution must be qualified and authorized by the lab manager prior to do any work.

3. The list of the authorized users is published on this web site. If your name is not on this list, you are not allowed to use Piranha solutions at any time.

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4. Any accident regarding the use of Piranha solutions must be reported without delay to the lab manager.

2 - Protection equipment

1. The handling of Piranha solutions requires special protection equipment in addition to the regular clean room protection outfit (see Lab Safety page) .

2. The additional protective equipment include: a full face shield, heavy duty rubber gloves (regular Nitrile gloves used in LAMP will not provide sufficient protection), as well as an acid apron to wear on top of the lab coat. Gloves are located in the acid cabinet, apron and mask are available next to the wet bench.

3. As a reminder, open-toed shoes are not allowed when working in the lab and bare legs must be covered by wearing a full size bunny suit.

3 - Piranha solution handling

1. Piranha solutions, as well as any corrosive or hazardous substances, can only be used in LAMP during operational hours (9 am to 6 pm, Monday to Friday) and requires at all time the presence of a second knowledgeable user (buddy system).

2. Whenever handling Piranha, only use glass containers (preferably Pyrex). Containers used during the experiment must be very clearly labeled and a warning sign, visible by any user working under the flow hood, must be posted at all time to indicate that the solutions contains Piranha mixture.

3. Mix the solution in the flow hood with the sash between you and the solution. Wear the full protection.

4. When preparing the piranha solution, always add the peroxide to the acid. The H2O2 is added immediately before the etching process because it immediately produces an exothermic reaction with gas (pressure) release. If the H2O2 concentration is at 50% or greater, an explosion could occur.

5. Piranha solution is very energetic and potentially explosive. It is very likely to become hot, more than 100 degrees C. Handle with care.

6. Substrate should be rinsed and dried before placing them in a piranha bath. Piranhas are used to remove photoresist and acetone residue, not the compounds themselves

7. Leave the hot piranha solution in an open container until cool.

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8. Never store hot piranha solutions. Piranha stored in a closed container will likely explode.

9. Adding any acids or bases to piranha or spraying it with water will accelerate the reaction. This includes Photoresist, which is a strong base.

10. Mixing hot piranha with organic compounds may cause an explosion. This includes acetone, photoresist, isopropyl alcohol, and nylon.

11. Do not store wash bottles containing organic compounds on the piranha deck.

4 - Piranha waste disposal

1. The primary hazard from storage of piranha etch waste is the potential for gas generation and over pressurization of the container when the solution is still hot. If you store a hot solution in a air tight container, it will explode!

2. Therefore prior to store the piranha solution, it must be left in an open container in order to cool down for several hours (overnight). It is your responsibility to make sure that the open container is very clearly labeled and left in a safe area for overnight cool down.

3. Once cooled down, the solution can be transferred into a closed glass container for waste storage. The container must be very clearly labeled with the solution name and composition and must include VERY VISIBLE warning signs not to add any other types of chemicals.

5 - Emergency procedure

1. In case of large exposure, the victim should be removed from the contaminated area, placed under a safety shower while emergency personal is contacted (911)

2. All contaminated clothing should be removed immediately with appropriate gloves and safely discarded.

3. In case of contact with the skin, the affected area must be immediately rinsed with large amounts of water for at least 15 min.

4. In case of contact with the eye, irrigate the eye for at least 30 minutes, keeping the eyelids apart and away from eyeballs during irrigation. Place ice pack on eyes until reaching emergency room.

5. In case of inhalation, it may irritate the respiratory tract. Conscious persons should be assisted to an area with fresh, uncontaminated air. Seek medical attention in the event of respiratory irritation, cough, or tightness in the chest. Symptoms may be delayed.

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6 - Supply and storage

1. Do not store piranha. Mix fresh solution for each use. Excess solutions should be disposed as explained in paragraph #4.

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Standard Operating Procedure #5

LAMP hazardous gas detection and emergency system

Facility: Laboratory for Advanced Materials Processing

2225 JM Patterson bldg, Materials Science and Engineering

University of Maryland, College Park MD 20742

(301) 405 7250

Lab Director: Gary Rubloff

2145 AV Williams Bldg

(301) 405 2949

Lab Manager: Laurent Lecordier

2147 AV Williams Bldg

(301) 405 5858, cell (301) 602 9858

Scope: This SOP details the equipment and procedures put in place within LAMP related to

the utilization of hazardous process gases

Last revision: 09/08/04 by Laurent Lecordier

To optimize the safety in LAMP, several safety sensors have been installed in order to

generate a single alarm response in case of an emergency. These sensors and alarm devices

were initially installed in 2001 for the detection of pyrophoric silane. However the silane

cylinder was removed from the lab in June 2003 and the MDA System 16 (for silane

detection) is now shut down. The alarm system is still operational and activated and receives

the signals from the HF detection sensor, smoke detectors, photohelic gauges for vent line

monitoring and EPO button . This report will list the different sensors and the procedures to

respect in case of an alarm within this laboratory. A section regarding the maintenance of this

alarm system is also included.

1 - Alarm Systems

1.1 - CSS E0883 MDA alarm unit

The core of the LAMP alarm system is the MDA alarm unit located above the System 16 gas

monitor.

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This system generates 24 V signals to the different sensor relays (MDA silane gas detector,

HF gas detector, smoke detectors, photohelic gauges, EPO button at the entrance of the lab,

silane pressure switch and silane excess flow switch). If an alarm condition is detected by one

of these sensors, their internal Normally Open relays will be closed and the 24 V signal will

be returned to the MDA alarm interface. An appropriate response will be triggered in function

of the origin (sensor) of the alarm.

In all alarm cases (Level 1 or 2), the gas interlock system will be shutdown (Alarm level 1).

All the pneumatic valves located on the gas cylinder outlets or downstream to the regulators

will be automatically shut down.

If the presence of smoke is detected in the cleanroom or pre-cleanroom, or if the EPO button

at the entrance of the lab is pushed (Alarm Level 2), a visual and audible alarm (remote alarm

enunciators 1 and 2) will be triggered in both rooms, in addition to the gas interlock

shutdown. The MDA alarm unit is also connected to a 24 hour monitoring station that will

notify UM Police Department and trigger an additional enunciator in the hallway (see next

page). The building alarm will also be activated.

Notice: the monitoring station and building alarm are activated via signal from MDA interface

to ESL fire panel (see section 1.2.2 ESL fire panel for additional information)

If the MDA alarm unit or the Lifeline HF sensor stop functioning (power shortage,

breakdown, cell lifetime…), a Normally Open relay will open and shutdown the gas interlock

system.

In case of a power shortage, the MDA alarm unit and the System 16 gas detector are backed

up by a Stabiline SL 1500 uninterruptible power supply whose 1440 max VA will provide

power to these systems for 5 to 10 minutes.

1.2 - Remote alarm enunciators 1 and 2

Two visual (red flashlight) and aural remote alarms are connected to the MDA alarm interface

and will respond to an Alarm level 2. One is located next to the MDA alarm interface above

the System 16, the other on top of the ULVAC system.

The 24V power supply to these units is provided by the MDA alarm unit which means that in

the case of a building power shortage, these alarms will continue to function for a few minutes

via the UPS. These alarms can only be shut down by deactivating the internal relays of the

MDA alarm unit.

1.3 - DSC power 832 24-hour supervisory unit

A 24-hour supervisory unit is connected to the University of Maryland Police Department.

UMPD will immediately notify the fire department. This unit reports any alarm Level 2 from

the MDA alarm unit. If an alarm condition is received by the ESL fire panel, the alert will be

automatically forwarded to UMPD.

Notice: the DSC system remains active and operational even if it is not armed but just in

Ready position. If a test needs to be run, UMPD must be contacted first at #53555.

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A blue flash-light is installed in the hallway on top of the LAMP main entrance door. In

addition to the visual signal, a prerecorded warning message will be annunciated. This

speaker/light warning system is connected to the DSC supervisory unit. To stop the siren or

rearm the system, enter on the keypad: 1 2 3 4

The UMPD phone number to call or to cancel an accidental alarm is ext. #53555.

The manual related to the operation of this unit is included in this report.

UMD contact: Craig Chucker, Bldg Security Systems

1.4 - J.M. Patterson building alarm

In case of Alarm Level 2, the JM Patterson main alarm system will be also triggered. A 4th

zone was added to the ESL fire panel and connected to the MDA alarm unit. In case of alarm,

the zone 4 will be energized and a relay connected to the building alarm circuitry will be

activated. If necessary, the connection to the building alarm can be temporary deactivated by

puling the relay box out of its receptor base.

UMD Contact: Jim Robinson (x 53971)

2 - Safety Sensors and Actuators

2.1 - MDA / Zellweger Analytics System 16 gas detector ALARM LEVEL 2

Notice: the MDA System 16 has been shut down since June 2003. The following information

is therefore facultative.

This system is currently configured for the detection of silane and analyses sequentially the

gas samples in four different locations (silane gas cabinet, ATM gas scrubber, Ulvac gas

delivery system on the roof of the Ulvac cluster tool, cleanroom).

If a silane concentration above 5 ppm (TLV) is detected at any of these locations, it will

activate the MDA alarm interface (Alarm Level 2)

The front panel of the System 16 can be read from the hallway through the glass window.

Thus, in case of an alarm, the printed emergency report can be read without entering the lab.

This system is backed up by a UPS station.

A set of 3 green and 3 red LED’s has been wired on the back panel of the System 16 gas

detector. These LED’s report the following fault detection:

• Maintenance Warning: the instrument needs attention but the instrument is still able to

monitor and operate as programmed. (e.g. chemcassette needs to be changed)

• Loss of Coverage: the monitoring capability is reduced, but not completely absent (failure

of one or more points module)

• Loss of Monitoring: it indicates a complete absence of monitoring.

The bottom line is that these LED’s are easily visible either from the precleanroom or from

the cleanroom. The operators of the ULVAC should systematically make sure that all three

green LED’s are ON before processing with silane.

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(for more details concerning the System 16, cf. Section 3 of this memo)

2.2 - Three-zone ESL Fire Alarm Control unit ALARM LEVEL 2

3 smoke detectors are located near the silane gas cabinet, the ATM scrubber and the ULVAC

CVD cluster tool. They are connected to the three-zone ESL Fire Alarm control unit, located

next to the System 16 and visible from the middle door in the hallway.

If the presence of smoke is detected at any of these three locations:

• An internal audible alarm (from the ESL fire control unit) will go off.

• A double throw relay will activate the MDA alarm interface (Alarm Level 2).

This system is backed up by a 24 V battery.

The building alarm is tied to the ESL Fire panel. In order to have the building alarm activated

in case of a level 2 alarm, a fourth zone has been installed by Physical Plant. This zone is an

input from the MDA alarm interface. If an alarm Level 2 is generated, the A1 N.O.-relay from

the MDA alarm interface will close. A 24 V signal is consequently received to the Zone 4

terminal triggering the Fire alarm and the building alarm.

2.3 - Red “Mushroom” push-button ALARM LEVEL 2

Located at the entrance of the lab (on the left side of the door), it can be manually activated. It

is connected to a 120 V relay located in the mechanical room. The closure of this relay by

pushing on the button will return a 24V signal to the MDA alarm interface (Alarm level 2).

An internal flash light and an aural alarm are also activated (they are located above the

entrance door in the pre-cleanroom. The 120V signal is provided by the building power

supply.

2.4 - Dwyer hi/low-setpoints photohelic gages ALARM LEVEL 1

3 photohelic gauges monitor the proper functioning of the duct exhaust system at the three

following locations: silane gas cabinet exhaust, mechanical pumps and scrubber exhaust,

ULVAC cluster tool exhaust. If the pressure in the exhaust is below 0.2” WG (normal

pressure is between 0.5 and 1”), it will activate the MDA alarm unit that will shutdown the

gas interlock panel (the remote alarm enunciators will not be activated).

2.5 – Honeywell Analytics Lifeline HF sensor ALARM LEVEL 2 One Lifeline 0-10 ppm HF sensor monitors the HF gas concentration in the vicinity of the

programmable CVD reactor. The remote readout transmitter is located near the System 16 on

the left side of the hallway window so that the HF concentration can be read from the hallway.

A relay module is connected to the CSS E0883 MDA alarm unit via Relay 1 and 3. Relay 3 is

a fail-safe relay that will turn off the gas interlock panel (alarm level 1) in case of failure of

the sensor. Relay 2 energize at 8 mA or 2.5 ppm (4-20 mA loop) and will trigger an Alarm

Level 2. The HF Lifeline Sensor are calibrated at the factory and are to be replaced every 6

months. Minimal detection limit is 1.2 ppm.

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3 - Zellweger Analytics System 16 Gas Detector

Notice: the MDA System 16 has been shut down since June 2003. The following information

is therefore facultative

The System 16 is equipped with one 4-point module analyzer that can detect one gas at 4

different locations. This analyzer has a chemcassette formulated to react with silane: the target

gas in the sample reacts with the tape, the reaction produces a stain with a density proportional

to the gas concentration, the stain is measured is optically measured. This chemcassette and

optical sensor must be maintained monthly (cf. Section 3-2).

This system can be programmed either in Sequential Mode (System 16 monitors the sample

from only one point at a time) or in Parallel Mode (the System 16 monitors simultaneously

samples from the 4 points)

3.1 - System configuration

This section is a descriptive list of the current configuration and the different steps followed

by the System 16 in case of silane detection. For more details, cf. System 16 Technical

Handbook.

• System 16 is configured in Sequential Mode.

• Alarm levels for the point group (i.e. 4 points):

TLV1 = 5 ppm � early detection of silane

TLV2 = 10 ppm � for critical levels which may require evacuation

TLV: Threshold Limit Value

Based on the alarm level of the point in the point group with the lowest programmed alarm

level (in our case, each point has the same alarm level)

In our case, all alarms are triggered at TLV1 and will require immediate evacuation.

- If the gas concentration for one point exceeds 5 ppm:

1) The appropriate alarm LEDs lights (Level 2 and/or 1)

2) The point Relay contact activates and triggers the LAMP alarm Level 2 via the MDA

alarm interface.

3) The printer module prints the alarm information with time, alarm levels and

concentrations

3.2 System 16 Scheduled Maintenance

Changing the Chemcassette (i.e. every month):

• Clean with alcohol everywhere the tape is in contact (especially the tape guides)

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• Use the optic verification card to check the optics system (see Section 10 of Syst. 16

Handbook).

• Balance the flow (see Section 9)

• If problem with the flow balance, check the Acid Scrubber filter.

• MDA Service Mode (not in the manual)

Password: 0902

Select Subfunction: Real CC Transducer

140 < S < 205 (operating range)

Adjusting S will probably change the flow meter value (e.g. from 42 to 45 mm). This does not

matter. The transducer data S is the most accurate and is the one that will be processed by the

computer (not the flow meter value)

Bi-annual Maintenance

Optics Calibration

• Enter Service Submenu, and subfunction 9 (Read Raw Optics)

Raw reading should be: 3200 +/- 200

Lower limit 2000 (a lower value will give an Instrument failure)

To clean the optics, remove the 2 screws of the optics block, pull the pipe straight back at the

rear of the panel, remove the black plastic block with the LED’s and clean with alcohol.

When dirty, you can see a white stuff from the band. Also in case of false alarm, the optics

should be always checked)

Filter Maintenance (see section 12 of System 16 Technical Handbook)

• Acid Scrubber Filter (manufactured by Bolston, PN 710235)

If ¾ or more of the acid scrubber turns blue, or the vacuum increases, replace it.

Replacement frequency: 6 months.

• Primary Flow Module Filter (Replacement frequency 6-12 months)

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4 - Alarm System Maintenance and Testing

Only the System 16 gas detector requires a monthly maintenance (cf. Section 3.2).

If you are testing sensors susceptible of triggering an Alarm Level 2 (HF sensor, MDA gas

detector…), you must disable the Zone 4 on the ESL Fire Control Unit. By doing so, only the

internal alarm system (gas interlocks and flashlights) will be triggered without relaying the

alarm to the UM police Departmen and without triggering the building alarms.

If you want to test the response of ESL Fire Control Unit itself (e.g., testing of smoke detectors),

you must deactivate the relay that is connected to the building alarm (see lab manager). You

must also contact UMPD with the account # (written on the DSC unit) to notify them that you

will be running a test (x53555). If you don’t do so, the emergency response team will be notified

MDA System 16 Gas Detector

The alarm LED’s and alarm relays should be tested every month:

- Press the service function key on the System 16 control module.

- Select Subfunction Alarm Test by pressing key 2 twice.

- Press 0, to select a full-system test or 1 if you want to check each point

individually.

- Remote Alarm 1 and 2 should go off and gas interlock should be shutdown.

- Press Service on control module to turn off the alarm.

ESL Fire Alarm Control Unit

The three smoke detectors should be tested individually.

- To test the smoke detectors, use the Smoke Detector Tester. Aim the spray for 2

seconds at detector.

- The related zone relay should be activated: the internal audible alarm will go off as

well as remote alarm 1 and 2. Gas interlock should be shutdown.

- To deactivate the alarm, switch to Reset in the ESL system control unit.

Photohelic gauges

The three photohelic gauges should be tested individually and every month.

- For each photohelic gauges, increase the low setpoint till it reaches the current

pressure in the duct system: Gas interlock should be shutdown.

- To turn off alarm, reset the setpoint to its original value.

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5 - Electrical diagram of the MDA alarm interface and peripherals

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6 - MDA Interface unit: relay connections

Power ON

No alarm

P1 and P3 normally close => V P’2 = 24V => P2 relay closed (gas interlock

OK)

If alarm level 2 conditions (System 16, ESL fire panel, EPO, HF sensor Relay 1)

V P’1 = 24V => P1 opens => P3 is still closed => V P’2 = 0V => P2 opens

(gas interlock shutdown)

V P’1 = V A’1 = V Q’ = 24 V => A1 closes (Alarm level 2), Q opens

(monitoring station, hallway enunciator)

If alarm level 1 condition (photohelic gages, HF sensor Relay 3)

V P’3 = 24 V =>P3 opens => V P’2 = OV => P2 opens (gas interlock

shutdown)

P’1 P’2 P’3 P’4 Q’ A’1 A’2 24 V

NC

NO

NC

NO

P1

P2

P3

A1

24V

Alarm Level 1(gas interlock)

Alarm Level 2Lab enunciators

System 16 (points 1, 2, 3)

ESL Fire panel, EPO, HF sensor

Fail-safe (relay 1) HF sensor

Photohelic gages

Overpressure switch

Rear panel of MDA Alarm unit

Terminal block interface

Electrical connections to MDA alarm interface

Alarm Level 2To Zone 4 ESL panel for

Bldg alarm connection

P’1 P’2 P’3 P’4 Q’ A’1 A’2 24 V

NC

NO

NC

NO

P1

P2

P3

A1

24V

Alarm Level 1(gas interlock)

Alarm Level 2Lab enunciators

System 16 (points 1, 2, 3)

ESL Fire panel, EPO, HF sensor

Fail-safe (relay 1) HF sensor

Photohelic gages

Overpressure switch

Rear panel of MDA Alarm unit

Terminal block interface

Electrical connections to MDA alarm interface

Alarm Level 2To Zone 4 ESL panel for

Bldg alarm connection

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Power OFF

P2 opens => gas interlock shuts down

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7 - Floor plan of LAMP and positioning of sensor and alarm units

Gas

detector

unit

MDA

alarm

unit

Remote

alarm 1

enunciator

ESLFire

Gas scrubber Zone

Remote

alarm 2

enunciator

EPO

EPO flashlightESL Fire

flashlight

HA

LL

WA

Y

CLEANROOM

PRE

CLEANROOM

Floor plan of LAMP and locations of sensor and alarm units

DSC

unit

Gas interlock

panel

Chemicals

H2 gas bottle

Mech. ROOM

Smoke detectors

WF6 sensor

X

8 lbNH3 gas bottle

15 lbWF6 gas bottle

HF Lifeline

readout unit

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Building Security Systems Unit

SECURITY SYSTEM OPERATION FOR DSC SUPERVISORY UNIT

Notice: the notes below were obtained from UMPD and does not reflect the way our unit

is apparently working in the lab. That is, the DSC unit happens to transmit an

alert from the ESL fire panel even if the system is not “armed” but just in its

“ready” mode. Therefore you need to contact UMPD at 53555 prior to run any

test on the alarm system.

1). TO ARM THE SYSTEM:

a). VERIFY THAT THE GREEN “READY” LIGHT IS ON.

b). ENTER YOUR 4-DIGIT CODE 1234 OR PRESS THE “AWAY” BUTTON

UNTIL THE SYSTEM ARMS.

c). EXIT THE BUILDING AND CLOSE THE DOOR WITHIN 45

SECONDS. THE SYSTEM IS NOW ON!!

2). TO DISARM THE SYSTEM: a). UPON ENTERINGTHE BUILDING YOU WILL HEAR A PRE-ALARM

SOUND FROM THE KEYPAD.

b). ENTER YOUR 4-DIGIT CODE INTO THE KEYPAD.

c). THE SOUNDER AND THE ALARM WILL TURN OFF.

d). THE SYSTEM IS NOW OFF!!!

3) WHAT DO I DO IF THE KEYPAD SOUNDER ACTIVATES? a). CHECK THE MESSAGE “READ WHAT IS SAYS AND FOLLOW

DIRECTION ON THE SCREEN”. b). TO SILENCE THE KEYPAD OR ALARM JUST ENTER YOUR CODE.

c). IF ALL ELSE FAILS CALL (301) 405-3286 OR (301) 405-2222

AND ASK FOR BUILDING SECURITY.

4) How do I set the system to arm itself at night ? a). Press the * button then press the number 6.

b). Enter your MASTER CODE.

c). Press the right > arrow until the screen says “ENTER AUTO ARM TIME”

d). Enter the time (Military time) that you want the system to turn on.

e). Then press the right > arrow until the system says ‘AUTO ARM CONTROL”.

f). Press the * button to have the system auto arm. The screen will confirm that the

feature is either on or off. Please read what the system says. Often people will think they

have turned on the auto arm function when in fact they have actually turned it off.

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Appendix IV

Chemical Inventory

and

Material Safety Data

(to be supplied by Laboratory Supervisor)

Notice: Materials Safety Data Sheets are listed on the LAMP website at

http://www.enma.umd.edu/LAMP/lamp_msds.htm

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Wet chemical inventory

Chemical Supplier Volume MSDS

Acetone, 99.9+% Sigma Aldrich 2L Electronic

Copy

Ammonium cerium nitrate Aldrich 50g Electronic

Copy

AZ 300MIF developer Clariant 1L Electronic

Copy

AZ 400K Developer Clariant 1Ga Electronic

Copy

Bismuth acetate Alfa Aesar 50g Electronic

Copy

Butanol (1-) Aldrich Electronic

Copy

Ethyl alcohol, reagent Aldrich 1L Electronic

Copy

Gold Alfa Aesar 1g Electronic

Copy

Gold etch - iodine 500ml Electronic

Copy

Hydrochloric acid 50% Fisher chemical 500ml Electronic

Copy

Hydrofluoric acid (37%) 1l Electronic

Copy

Hydrofluoric acid 10% 1l Electronic

Copy

Hydrofluoric acid 5% 1l Electonic & hard copy

Hydrofluoric acid, ammonium fluoride 6:1 (Buffered Oxide Etch)

JT Baker 9lb Electronic

Copy

Hydrogen peroxide H2O2 30% Fisher Scientific 500ml Electronic

Copy

Lead Titanium Isopropoxide Alfa Aesar 100ml Electronic

Copy

Lead Zirconium ethylhexano isopropoxide, 10%W/V

Alfa Aesar 100ml Electronic

Copy

Methanol J.T.Baker 4L Electronic

Copy

Methoxy ethanol (2-), 99% Alfa Aesar 1L Electronic

Copy

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Methylsilsquioxane 35% in mix solvents

100ml Electronic

Copy

Microposit 452 Developer Shipley 1Ga Electronic

Copy

Nitric acid 70% JT Baker 2.5l Electronic

Copy

O-phosphoric Acid Fisher 500ml Electronic

Copy

Platinum Alfa Aesar 5g Electonic & hard copy

Potassium hydroxide, Potassium phosphate

1l Electronic

Copy

Propanol (1-) Fisher Scientific 500ml Electronic

Copy

Propanol (2-) Aldrich 4L Electronic

Copy

Sulfuric acid Fisher Scientific 2.5L Electronic

Copy

Tetrachloro ethane TCE 1,1,1 Alfa Aesar 4L Electronic

Copy

Tetramethyl ammonium hydroxyde Aldrich 1l Electronic

Copy

Titanium 2-ethyl hexoxide Alfa Aesar 500g Electronic

Copy

Toluene Fisher Scientific 4L Electronic

Copy

Trichloroethylene Fisher 2L Electronic

Copy

Xylene Fisher Scientific 1l Electronic

Copy

Zinc 2-Ethylhexanoate Alfa Aesar 100gm Electronic

Copy

Zinc neodecanoate Alfa Aesar 250g Electronic

Copy

Zirconium 2-ethylhexanoate Alfa Aesar 100gm Electronic

Copy

Gas inventory

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Tungsten hexafluoride – WF6 Air Products 15 lb Electronic

Copy

Ammonia (NH3) Air Products 50 lbs Electronic

Copy

Sulfur hexafluoride Air Products 7 lbs Electronic

Copy

Hydrogen Air Products 196 ft3 Electronic

Copy

Hydrogen Praxair 196 ft3 Electronic

Copy

Diluted silane (1% in 99% N2) Praxair 20 lbs Electronic

Copy

Nitrogen Praxair Electronic

Copy

Argon Praxair Electronic

Copy

Helium Praxair Electronic

Copy

Hafnium tetrakis dimethyl amide Aldrich 20 g Electronic

Copy

Hafnium tetrakis ethyl methyl amide Epichem 50 g Electronic

Copy

Titanium isopropoxide InorgTech 100g Electronic

Copy