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 Safety Manual
The Institute for Materials Research
Tohoku University
English version 0.1 (June 9, 2014)
Office of Safety and Health, IMR
Safety Manual (English version 0.1)
Chapter 1 Introduction
1.1 G eneral rem arks
All the staff members working or planning to work in The Institute for Materials Research
(IMR), regardless of his/her affiliation, are required to take safety instruction/training in
accordance with the Health and Safety Management Guidelines (JAPANESE) of the
university, as described in this manual.
It is one of the responsibilities of the head of research group, i.e., professors, project leaders,
etc. in IMR, to carry out necessary safety instruction/training to all the members in the group,
including students, despite the fact that the laws regarding occupational hazards, such as
The Occupational Health and Safety Act, do not legally apply to them.
1.2 Safety First
During research activities, the highest priority must be given to the safety. An accident not
only cause a possible injury or even death to those who are directly involved, but in many
cases, also give rise to hazards to others and the surroundings. In a worst case, single
accident could terminate entire research/education activities in the laboratory.
1.3 R eport im m ediately
In the event of an accident, one must report it to his/her supervisor as soon as practically
possible. It is, in return, the responsibility of the supervisor to inform the accident to the
safety office in IMR, regardless of its seriousness. This is the rule, not an option. The safety
office will undertake necessary investigations as to the cause of the accident. The information
will then serve as precautions/countermeasures against possible future accidents of similar
kinds.
1.4 G eneral aim s of safety instructions and training
All members of IMR, including students, are required to receive safety instructions/trainings
not only specific to their research, but also in general, before the commencement of research
activities. Their aims are:
(1) To protect themselves and those involved from possible injury and danger.
(2) To avoid any damage to the surroundings
(3) To give general ideas and fundamental rules concerning safety issues
1.5 A bout this m anual
1.5.1 O bjective
The purpose of this manual is to provide those who are involved in everyday research
activities in IMR with basic knowledge on potentially dangerous/hazardous materials, such
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IMR, Tohoku University
as chemical substances, gases, radioactivities, etc., so that they become capable of foreseeing
possible danger associated with their research. To that end, this manual includes not only
detailed descriptions of the materials themselves but also precautions and considerations
that should be understood and hence followed when handling them. In addition to these
preventive measures, the immediate actions that should be taken on the part of researchers
in the unfortunate event of an accident are also described to minimize the damage.
1.5.2. Scope and lim itations
It must be emphasized, however, that no single book can cover all the materials in the
laboratories, nor can it give a complete instruction to avoid even a tiny accident. Thus, this
manual should be regarded as a list of selected illustrations of safety practices, and should
not be taken as exhaustive. There are a number of materials and practices that are
potentially dangerous depending on how they are handled. It is worth pointing out that a
large number of accidents are caused by a lack of knowledge, and that the situations are often
worsened owing to poor judgment and mishandling of the immediate action after an
accidental event. Other factors that potentially increase the risk include narrow workspace,
unfit working environments, physical/mental conditions of experimentalists. In other words,
no perfect measure exists that can prevent an accident in laboratories, and thus, each and
every safety precautions are essential in daily research activities.
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Safety Manual (English version 0.1)
Chapter 2 Classified Dangerous Materials
2.1
Introduction
Many kinds of materials and chemicals are being used in laboratories in R&D activities in
the university. They possess potential risks, and they become a cause of an accident when
they are used improperly. This chapter describes basic rules for handling dangerous
materials, especially those classified as 'dangerous' by the law, having potential risks of fire
or explosions.
General cautions before starting an experiment are:
(1) When using materials you are not accustomed to handling, be sure to carefully check their
dangerous and toxic natures, such as ignition point, flash point, explosion range,
extinguishing method (especially for substances that react violently with water), etc., by
using the Material Safety Data Sheets (MSDS), data books, handbooks (see references listed
at the end of the chapter) and other sources of information.
(2) Learn and review appropriate actions against potential dangerous situations, and prepare
for various types of accidents that may occur.
(3) Make standard experimental procedures, in such a way so that you can forestall potential
dangers. For example, assess the heat of a reaction and a heat generated from mixing in
advance. Simulate what will happen.
(4) Share your knowledge with others in the laboratory and standardize the procedures
and/or handling on the dangerous or toxic nature of substances.
(5) You are fully responsible for all the handling of the substances, i.e., the procurement,
registration, storage, usage, and the disposal.
2.2
D angerous substances
2.2.1
G eneral rem arks
The Fire Prevention Law classifies legally designated dangerous substances into six groups
according to their characteristics as listed in Table 2-1, where the maximum quantities that
can be stored in a laboratory is also stipulated. The law also states that dangerous substances
beyond the limitations have to be stored in a designated storeroom. If you have an amount
above 20% of the specified limitation for a dangerous material, or an amount above the
specified limitation for a flammable solid, or if you keep statutorily stipulated dangerous
substances, the fire department needs to be informed of the details (refer to the Sendai City
regulation for fire prevention). For your own safety, you should not keep quantities of these
materials in excess of the limitations. Some general cautions and practices to be observed for
dangerous chemicals when handling them in the laboratory are described below.
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Table 2-1 Classification of dangerous substances under the Fire Laws.
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Safety Manual (English version 0.1)
2.2.2 O xidizers (G roups 1 and 6)
Oxidizers can react violently when they come into contact with flammable chemicals,
reducing agents, or metal powder.
Oxidizing solids:
Oxidizing liquids:
Oxidizing gases:
chlorates, perchlorates, permanganates, inorganic peroxides, etc.
hydrogen peroxide, perchloric acid, fuming nitric acid, etc.
ozone, fluorine, chlorine, etc.
Handling
(1) Avoid exposure to direct sunlight, heating and all forms of impact.
(2) Avoid mixing oxidizing agents with other chemicals. Be especially careful with organic
compounds and strong acid agents.
(3) Oxidizers can react violently when they come into contact with water and will readily
release oxygen and heat. Therefore, carefully plan all procedures that involve working with
oxidizing agents.
Extinguishing a fire
Water is generally used to extinguish fires involving oxidizers. The principle is that large
amounts of water are required to cool down the reaction. Dry sand should be used in case of
inorganic peroxides such as potassium peroxide and calcium peroxide.
2.2.3
Flam m able solids (G roup 2)
Flammable solids are materials that ignite easily at low temperatures and are then oxidized.
They are dangerous as they may explode when mixed with oxides or when they are subjected
to impact. Examples include phosphorus sulfide, red phosphorus, sulfur, iron powder,
aluminum powder, and magnesium. Some of them are also substances that release toxic gas
as a side product when burning or upon reaction with water. There are also substances that
self-ignite on exposure to air and some finely powdered substances that cause dust
explosions.
Handling
(1) Avoid igniting, heating or contact with any oxidant.
(2) Generally, close containers whilst being careful to prevent exposure to moisture and store
in a cold place.
(3) Avoid bringing iron powder, metallic powder, magnesium, and materials containing these
substances in contact with water or acid.
Extinguishing a Fire
If contact with water is dangerous, smother any fires using dry sand. Otherwise, use water or
a water digestive. Smother combustible solid fires using foam or powder digestives.
2.2.4
Pyrophoric substances (G roup 3)
White phosphorus, organolithium, organoaluminium, reduction metal catalysts (Pt, Pd, Ni)
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and silanes are examples of substances that spontaneously ignite upon contact with air.
Many substances of this type also ignite when in contact with water.
Handling
Use in a dry box purged using an inert gas (such as nitrogen and argon) to prevent contact
with air and moisture. Although caution whilst handling is indicated on the container for
special active compounds (such as raney nickel, reduced palladium), use them under the
guidance of a member of staff/faculty who is accustomed to handling them.
Extinguishing a fire
Use dry sand or a powder fire extinguisher.
2.2.5
W ater-prohibiting substances (G roup 3)
When water-prohibiting materials come into contact with water, they ignite and combustible
or noxious gas is generated. Metallic sodium, potassium, calcium carbide, calcium phosphide
(poisonous gas generation), organolithium and metal hydride compounds are included in this
group.
Handling
Care should be taken to ensure these compounds do not come into direct contact with water
or skin. In addition, the humidity level in the inventory location needs to be noted.
Extinguishing a fire
Cover with dry sand or use a powder fire extinguisher. Never use water. Also, be careful not
to use a carbon dioxide fire extinguisher, which is an aqueous based extinguishing agent that
forms bubbles.
2.2.6
Flam m able liquids (G roup 4)
Many organic solvents are dangerous substances because they are highly flammable. They
are categorized according to their flammability as follows:
Table 2-2 Classification of flammable liquids.
Special flammable materials
Diethyl ether, carbon disulfide and other liquids with an
ignition
point
of
≤100°C
at
atmospheric
pressure.
Substances with a flash point of≤–20°C or lower and a
boiling point of ≤40°C at atmospheric pressure.
First-class oils
Acetone, gasoline and other liquids with a flash point of
≤21°C at atmospheric pressure.
Alcohols
Saturated
monohydric
alcohol
(denatured
alcohol
is
included) with one to three carbon atoms. Composition is
taken into consideration, and some compounds are defined
by the statute to be excluded.
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Safety Manual (English version 0.1)
Second-class oils
Kerosene, diesel oil and other liquids with a flash point of ≥
21°C and ≤70°C at atmospheric pressure. Composition is
taken into consideration and some compounds are defined
by the statute to be excluded.
Third-class oils
Heavy oil, creosote oil and other liquids with a flash point
of ≥70°C and ≤200°C at atmospheric pressure. Composition
is taken into consideration and some are defined by the
statute to be excluded.
Fourth-class oils
Gear oil, cylinder oil and other liquids with a flash point of
≥200°C and ≤250°C at atmospheric pressure. Composition
is taken into consideration and some compounds are
defined by the statute to be excluded.
Animal and vegetable oils
Oils extracted from the fat or meat of an animal, the seed
or flesh of vegetables with a flash point of≤250°C at
atmospheric pressure.
Handling
(1) Special flammable materials such as ether (Flash point = –45 °C) and carbon disulfide
(CS2; Flash point = –30 °C) ignite in the presence of a pilot light or electrical spark even at a
distance. Therefore, the use of fire is strictly prohibited. Hexane, acetone, and benzene are
first-class oils. When heating and distilling them, careful attention must be paid to prevent
them from igniting. Although alcohol can be usually handled safely, in the absence of a naked
flame, please pay attention when heating and distilling alcohol.
(2) In general, you should handle as little liquid as possible and try not to bring more liquid
into the room than what is necessary. Make sure the laboratory is well ventilated. Most
organic solvents that possess a low boiling point have a low flash point too. Please check the
boiling point and the flash point of the solvent being handled.
Protect yourself
When using large amounts of flammable liquid, wear a protective mask and gloves made of
cotton.
Extinguishing a fire
In the event of a small fire, do not panic. Use a carbon dioxide or powder fire extinguisher to
put it out. If the fire keeps growing, it is advisable that you drench the fire with a large
amount of water.
2.2.7
Self-reactive substances (G roup 5, explosives)
Substances that explode or ignite by heat, impact, friction, or light irradiation. Examples of
self-reactive substances are benzoyl peroxides, nitrate esters, nitro and nitroso compounds,
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azo and diazo compounds, hydrazine derivatives, and metal azides. Substances such as
perchloric compounds that have many oxygen atoms in their molecular structures are
especially dangerous, though they are not classified into Group 5. Heavy metal perchlorates
such as silver perchlorate are extremely sensitive explosives. Even a small amount of silver
perchlorate can explode violently.
Handling
(1) Minimize the use of self-reactive substances.
(2) Keep away from naked flames, sparks, fire, and heat. Store in a cool area. Protect from
heat and impact.
(3) Do not use metal spatulas or spoons. Do not use glass stoppers to cap containers.
(4) Avoid storing peroxide-forming chemicals in oxidizing conditions or mixing them with
strong acids (i.e. nitric acid) for long periods. It is dangerous to store a mixture of alcohol and
hydrogen peroxide, especially at high concentrations (This mixture is often used for washing
experimental apparatus).
Extinguishing a fire
When a small amount of self-reactive substance catches fire, it can usually be extinguished
fairly easily. However, it might be impossible if there is a large amount of chemicals present.
Extinguish the fire with a large amount of water or foam fire extinguisher. Evacuate the area
as soon as possible if you feel there is an explosion hazard. Individual safety is the most
important consideration to take in account in such a scenario.
Table 2-3 Chemical bonds which lead may to facile explosion.
N-O Bonds
N-M Bonds
-O-NO2
nitrate esters
N-M3metallic nitrides
-NO2
nitro compounds
M-NH
metal-imidos
M-NH2
metal-amides
-N-NO2nitramines
-N-HNO3
amine nitrates
O-O Bonds
-NO
nitroso compounds
-OO-H
hydroperoxide
-ONC
fulminates
-OO-
peroxide
N-N Bonds
-CO-OO-H
peroxyacid
[-N三N]+diazonium salts
-O3ozonides
-N=N-C三Ndiazocyanides o-x
O-X Bonds
(-N=N2-S
-N-HClO4amine perchlorates
-N3azides
diazosulfides
-OCIO3perchlorate esters
-N-HClO
chloric acid amides
-C-OClO2chloric acid esters
-ClO2chlorites
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Safety Manual (English version 0.1)
2.2.8
Incom patible com binations of chem icals
When some chemicals are combined, there is a risk of fire, explosions, or the production of
poisonous gas. A great number of combinations are known have a potential risk of various
hazards.
In general, the following combinations are highly dangerous:
(1) Mixtures of oxidizers and reducers:
- Typical oxidizers: nitric acid, concentrated sulfuric acid, perchlorates, hypochlorites,
permanganates, bichromates, oxygen, and chlorine.
- Typical reducers: amine derivatives, various alcohols, sulfur, phosphorous, hydrocarbons
(organic chemicals), and metal powders.
(2) Mixtures of oxidizing salts and strong acids:
-Combinations of strong acids (nitric or sulfuric acid) and perchlorates, chlorates or
permanganates
(3) Mixtures producing unstable chemicals:
- Combinations of ammonia and iodine,ammonia and silver nitrate, metallic sodium and
chloroform (and carbon tetrachloride), and silver or copper salts and acetylene. The above
does not cover all dangerous combinations.
There are many other incompatible chemicals.
Handling
(1) Reference 4, "Handbook of Incompatible Chemicals" shown at the end of this chapter
describes the cautions required in regard to mixing and contact between various compounds.
Typical reactions involving large amounts of heat of reaction, fire and explosive hazards are
discussed in detail. Please refer to this handbook before carrying out an experimental
procedure with a potential risk of an accident when trying to dissolve or mix unfamiliar
chemicals together.
(2) It is essential that you observe the exothermic heat of mixing with a small amount of
chemicals prior to conducting the reaction. Once you have made sure your procedure is safe,
the amounts can be gradually increased.
(3) Be aware that general neutralization and dissolution can generate a relatively large
amount of heat beyond what you might expect.
(4) Be especially careful of the hazards when you use chemicals that you do not use often.
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Table 2-4 Inorganic compounds which are dangerous when mixed.
Main component
Sub component
Oxygen
Combustibles (especially H2, oil)
Ammonia
Ag, halogens, Ca(ClO)2
Halogen
NH3, alkynes, olefins, petroleum gas, turpentine oil,C6H6,
metal powder
Inorganic oxidizers
Reducing materials (ammonium salts, acid, metal powder,
combustible organic matter, S, Bi(including its alloys)
Alkaline and
H2O, CO, CO2, CCl4, hydrocarbon halide, heavy metalchlorides
Alkalineearth metals
Metals (Cu, Ag, Hg))
Alkynes, oxalic acid, tartaric acid, fumaric acid,ammonium
compounds, H202, fulminic acid
Ammonium nitrate
ROH, RCORl, HCN, CS2, combustibles
Table 2-5 Organic compounds which are dangerous when mixed.
Main component
Sub component
Acetylene
Cl2, Br2, F3, Ag, Cu, Hg
Acetone
Mixed acids (HNO3 +H2SO4)
Aniline
HNO3,H2O2
Acetic acid
HNO3, chromic acid, permanganate, peroxide
Oxalic acid
Ag,Hg
Hydrocarbon
Halogen, chromic acid, peroxide
Nitroparaffin
Chlorine, amine
Nitrobenzene
KOH
Hydrazine
H2O2,NHO3,oxidizers
Acetic anhydride
Alcohols (e.g. ethylene glycol), perchloric acid, bromine
Organic peroxide
Organic acids, inorganic acids, amines
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Safety Manual (English version 0.1)
Chapter 3 Hazardous Substances
3.1
G eneral
All substances used in experiments are considered hazardous to some extent. In most cases,
the amounts used are too small to pose any risk or hazard unless they are taken internally.
However, you must be very careful when handling toxic substances and highly volatile
poisonous substances. It is of the utmost importance that you take the time to collect
information on the toxicity of the substances you intend to use before using them.
3.2
Toxic substances
3.2.1
Poisonous substances and deleterious substances
Poisonous and deleterious substances are defined as having an LD50, a lethal dose per kg to
kill half of the tested population (Table 3-1). As defined in the "Poisonous and Deleterious
Substances Control Law" Article 2; chemical substances with a LD50 of ≤1.8 g are considered
poisonous substances and those with a LD50 of ≤18 g are considered deleterious substances for
adults (with an average weight of 60 kg)(Table 3-2).
Table 3-1
Poisonous
substances
Deleterious
substances
Table 3-2
Criteria for poisonous and deleterious substances.
Inhalation LC50
Oral
Transderma
LD50
LD50
Gas
≦30mg/kg
≦100 mg/kg
≦500ppm (4h)
30 mg/kg<
100mg/kg<
and
and
≦300mg/kg
Vapor
≦2.0 mg/L (4h) ≦0.5 mg/L (4h)
2.0mgl/(4h)<
500ppm(4h)< and
≦1,000 mg/kg
≦2,500ppm(4h)
Dust, mist
0.5mg/L(4h)<
and
and
≦ 10mg/L(4h) ≦1.0 mg/L (4h)
Designated substances by the Poisonous and Deleterious Substances Control Law
Definition
No
Classification
(Poisonous and Deleterious
Substances
Control
Law
noted
in
Main designated substances
Article 2)
Substances
1
Poisonous
substances
Attached Table 1 except
Hydrogen cyanide, sodium cyanide, mercury,
drugs
selenium,
and
drugs;
items1-28.
12
unregulated
designated
by
fluoride, etc.
nicotine,
arsenic,
hydrogen
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Substances
2
noted
in
Attached Table 2 except
Deleterious
drugs
substances
and
unregulated
drugs; designated by items
1–94.
3
Ammonia,
hydrogen
hydrogenperoxide,
sodium
potassium,
chloroform,
cresol,
peroxide,
carbon
tetrachloride, dichromic, acid, oxalic acid,
nitric acid, sodium hydroxide, picric acid,
phenol, methanol, sulfuric acid, etc.
Specified
Poisonous substances noted
Octamethylpyrophosphoramide,
poisonous
in
tetraalkyllead, etc.
substances
designated by items 1–10.
Attached
chloride,
Table
3;
Table 3-3 describes the classification of toxic and deleterious substances according to their
effects.
Table 3-3Classification of toxic and deleterious substances according to their effects.
Effect
Typical examples
Skin cornification: arsenic, cobalt, dilute alkali solutions, etc.
Skin coloration: picric acid, silver nitrate, iodine, etc.
Pigment anomaly: tar, pitch, arsenic, etc.
Acute dermatitis and rash: acid, alkali, chloro dinitrobenzene, formalin, tar,
Dermal lesions
pitch, etc.
Ulcers: chromium, nickel, acid, alkali, etc.
Lesions of hair and the sebaceous gland: mineral oil, tar, chloro naphthalene,
etc.
Hair lesions: thallium, manganese, etc.
Lesion of the nail and surrounding skin: selenium, thallium, fluorine, etc.
Mainly affecting the upper respiratory tract: aldehyde, alkalinity dust and
mist,ammonia, chromic acid, ethylene oxide, hydrogen chloride, hydrogen
fluoride,sulfur dioxide gas, sulfuric anhydride, etc.
Mucosadefects
Affecting the upper respiratory tract and pulmonary tissue: bromine,
chlorine,chlorine oxide, cyanogen bromide, dimethyl sulfate, fluorine, iodine,
etc.
Affecting peripheral airways, lower thoracic and pulmonaryalveoli:arsenic
trichloride, nitrogen peroxide, phosgene, etc.
Simple asphyxiation:
carbon dioxide, ethane, helium, hydrogen, nitrogen,
nitrous
Asphyxiation
oxide.
Chemical asphyxiation:
carbon monoxide, cyanide, hydrogen cyanide, nitrile,
aromatic nitro compounds (nitrobenzene, dinitrobenzene, etc.), aromatic
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Safety Manual (English version 0.1)
amines
(aniline, methylaniline, etc.), hydrogen sulfide
Anesthesia
Nervous
System
lesions
Liver and lesions
Blood lesions
Hard tissue
lesions
Most
organic
solvents
and
lipid
soluble
solids
have
a
variety
of
aesthesiaaffects.
Carbon disulfide, halogenated hydrocarbon, methanol, thiophene, tetraethyl
lead,manganese, mercury, etc.
Carbon
tetrachloride,
tetrachloroethane,
hexachloronaphthalene,
trinitrotoluene,dioxane (especially the kidney),uranium, cadmium, etc.
Benzene, lead, radiation, phosphine, arsine, etc.
Acid mist, yellow phosphorus, fluorine, etc.
Alveolus stimulant substances (lung edema, pneumonia), hardly soluble dust
(pneumoconiosis),
Lung lesions
talc(talcosis),
free
silicic
acid
agalmatolite
(silicosis
),
asbestos
(asbestosis),
(pyrophyllitosis),
aluminum
(aluminosispulmonum), coalpowder (coal miner's lung),graphite (graphitosis),
welding dust (welder's lung),beryllium (pulmonary berylliosis), etc.
Others
Allergy:
metallic oxide and fume, etc.
Circulatory function defects: nitro glycol, nitroglycerine, etc.
Cautions regarding storing and handling toxic and deleterious substances:
(1) Poisonous and deleterious substances must be exclusively stored in sealed containers and
placed in a locked cabinet for their exclusive storage. When purchasing or using these
substances, keep a strict record in the logbook. In addition, every time you purchase or use
them, make an entry into the management system for laboratory chemicals.
(2) Collect information on the degree of carcinogenicity and toxicity from reference
data(MSDS).
(3) Handle substances inside a fume cupboard equipped with a hazardous substances
removal unit.
(4) Wear the appropriate personal protection such as protective safety glasses, gas mask,
gloves, and other basic protective clothing.
(5) Be prepared to take the appropriate countermeasures in case of spillage or any other type
of accident.
(6) Never dispose of poisonous and deleterious substances in the ground or water supply and
never burn them.
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3.2
Specified chem ical substances
The Industrial Health and Safety Law and the Ordinance on the Prevention of Hazards due
to Specified Chemical Substances describes the responsibility of an organization to protect
their employees from cancer, dermatitis, nervous system diseases and other health damage
due to chemical substances. Employers are required to check the toxicity of substances,
possible replacements, work procedures, the maintenance and improvement of facilities and
ensure thorough health management and various other safety measures. Table 3-4 shows the
chemical substances that are designated by the Industrial Health and Safety Law. When
handling these substances, it is required to have local ventilation equipment, dust collectors,
an exhaust gas treatment system, a discharged liquid treatment system, and a system to
treat the residuals from experiments. In addition, installing of two or more doorways,
designating restricted areas, performing voluntary periodical inspection of machines, work
environment measurement, prohibiting eating, drinking and smoking, medical examinations,
wearing of safety gear, etc. must be adhered to.
Table 3-4 Specified chemical substances.
1. Group 1.
1 Dichlorobenzidine or its salts
2 α - naphthylamine or its salts
3 Chlorinated biphenyls(otherwise called
PCB)
4 O-tolidine or its salts
5 Dianisidine or its salts
6 Beryllium or its compounds
7 Benzotrichloride
8
Formulation
and
other
substances
containing more than 1% of its weight of
substances from 1 through 6, or more than
0.5% of its weight of 7 (in terms of alloy,
containing 3% of its weight of beryllium)
2. Group 2.
1 AcryIamide
20 Methyl bromide
2 Acrylonitrile
21 Dichromic acid or its salts
3Alkylmercurycompounds (only substances
22 Mercury or its inorganic compounds
in which alkyl group is methyl or ethyl
(exclusive of mercury sulfide)
group)
23 Trilene-diisocyanate
4 Ethyleneimine
24 Nickel carbonyl
5 Ethylene oxide
25 Nitroglycol
6 Chloroethylene
26 Para -dimethylaminoazobenzene
7 Chlorine
27 Para -nitrochlorobenzene
8 Auramine
28 Hydrogen fluoride
9 Ortho-phthalodinitrile
29 {3 -propiolactone
10 Cadmium or its compounds
30 Benzene
11 Chromic acid or its salts
31 Pentachlorophenol (PCP) or its sodium
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Safety Manual (English version 0.1)
12 Chloromethyl methyl ether
salts
13 Vanadium pentoxide
32 Magenta
14 Coal tar
33 Manganese or its compounds (exclusive
15 Arsenic trioxide
of basic manganese oxides)
16 Potassium cyanide
34 Methyl iodide
17 Hydrogen cyanide
35 Hydrogen sulfide
18 Sodium cyanide
36 Dimethyl sulfide
19 3.3'-dichloro-4.4'-diaminodiphenylmethane
37
Formulations
or
other
substances
containing substances from 1–36 shown
above,designated by Ministry of Health,
Labor and Welfare Ordinance
3. Group 3 (not subjected to work environment measures).
1 Ammonia
7 Phosgene
2 Carbon monoxide e
8 Formaldehyde
3 Hydrogen chloride
9 Sulfuric acid
4 Nitric acid
10 Formulations and other substances
5 Sulfur dioxide
containing substances from 1 through 9
6 Phenol
shown above, designated by Ministry of
Health,Labour and Welfare Ordinance.
* Asbestos, which formerly belonged to Group 3, was removed from the ''Designated Chemical
Substances" list in February 2005 and is now under the strict control of the new "Asbestos
Damage Prevention Regulations."
3.3
O rganic solvents
3.3.1
H azardous organic solvents
Under the Organic Solvent Toxication Prevention Regulations of the Industrial Health and
Safety Law, 55 types of organic solvents listed below are designated detailed rules to be
followed to prevent health damage (the solvents are classified into three groups depending on
the level of danger and hazard associated with their use). These rules specifically refer to the
equipment, ventilation system, work environment measurement, sign posting, indication,
evacuation procedure, storage, personal protection, health checkups, etc. Failure to
appropriately handle these organic solvents can cause health damage. Students are also
required to adhere to these rules.
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Table 3-5
Organic solvents.
Group 1.
Chloroform
Tertachlorocarbon
Trichloroethylene
1,2-Dichloroethane
1,2-Dichloroethylene
1,1,2,2-Tetrachloroethane
(dichloroethylene)
(dichloroacetylene)
(tetrachloroacetylene)
Acetone
Isobutylalcohol
Isopropylalcohol
Isoperitylalcohol
Ethylether
Ethylene
Carbon disulfide
Group 2.
(isoamylalcohol)
glycol
monoethylether (cellosolve)
Ethylene
glycol
monoethylether
acetate
Ethylene
glycol
n-butylether
mono
Ethylene glycol monomethyl
(butyl
ether (methyl cellosolve)
(cellosolve acetate)
cellosolve)
ortho-dichlorobenzene
Xylene
Cresol
Chlorobenzene
Isobutyl acetate
Isopropyl acetate
Ethyl acetate
n-butyl acetate
Isopentyl
acetate
(isoamyl
acetate)
Normal propyl acetate
Normal
pentyl
acetate
Methyl acetate
(normal amyl acetate)
Cyclohexanol
Cyclohexane
1,4-Dioxane
Dichloromethane
N,N-Dimethylformamide
Styrene
(dichloromethylene)
(DMF)
Tetrachloroethylene
Tetrahydrofuran (THF)
1,1,1-Trichloroethane
Toluene
n-hexane
1-Butanol
2-Butanol
Methanol
Methyl isobutyl ketone
Methyl ethyl ketone
Methyl cyclohexanol
Methyl cyclohexane
(perchloroethylene)
Methyl n-butyl ketone
Group 3.
Gasoline
Coal tar naphtha (including Petroleum ether
solvent naphtha)
Petroleum naphtha
Petroleum, benzene
Turpentine oil
Mineral spirit (including mineral thinner, petroleum spirit,
Mixtures
of
the
white spirit, andmineral turpentine)
listed above (1–54)
materials
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Safety Manual (English version 0.1)
3.4
M anufacturing prohibited and restricted substances
When using substances whose manufacturing is forbidden or restricted, you must comply
fully with the procedure required by the Industrial Health and Safety Law, Articles 55 and 56.
Before using those substances, permission must be granted from the Chief of the Miyagi
Labor Standards Inspection Office for the manufacture of prohibited substances and from the
Minister for Health, Welfare and Labor for the use and manufacture of restricted substances.
When falling under this case, contact the Health and Safety Management Office in advance.
3.4.1
Substances prohibited to be m anufactured
The manufacture of the following substances is strictly forbidden.
(1) Yellow phosphorus matches.
(2) Benzidine and its salts.
(3) 4-aminodiphenyl and its salts.
(4) Amosite.
(5) Crocidolite.
(6) 4-nitrodiphenyl and its salts.
(7) Bis(chloromethyI)ether.
(8) β-naphthylamine and its salts.
(9) Products that contain asbestos [exclusive of (4) and (5)] with >1 wt % asbestos content
(10) Gum, glue that contains > 5% benzene (of the total solvent, including the diluent).
(11) Formulations and other substances containing > 1 wt % of the substances described in (2)
through (8).
3.4.2 R estricted substances
The manufacture of the following substances requires a license.
(1) Dichlorobenzidine and its salts.
(2) α-naphthylamine and its salts.
(3) Polychlorinated biphenyl(PCB).
(4) ortho-Tolidineand its salts.
(5) Dianisidine and its salts.
(6) Beryllium and its compounds.
(7) Benzotrichloride.
(8) Formulations and other substances containing > 1wt% of the substances described in
(1)–(6), or formulations and other substances containing > 0.5wt% of substances described in
(1)–(6), and> 0.5wt% of substances described in (7). (Alloys containing > 3wt% of beryllium).
18
IMR, Tohoku University
3.5
Carcinogenic substances
The Japan Society for Occupational Health has accepted the classification of carcinogenic
substances by the International Agency for Research on Cancer (lARC) and has added extra
information in the table of carcinogenic substances to provide more information about
industrial chemicals and related substances. Group 1 includes substances carcinogenic to
humans. Group 2 includes substances deemed to be carcinogenic to humans. This group is
divided into two sub groups: Group 2-A includes agents, mixtures and circumstances that are
probably carcinogenic to humans and Group 2-B includes agents, mixtures and
circumstances that are possibly carcinogenic to humans. Table 5-4 shows the main
carcinogenic substances.
Table 3-6
The main carcinogenic substances.
Group 1.
Aflatoxin
Ethylene oxide
4-aminobiphenyl
Gamma ray irradiation
Arsenic and arsenic compounds
Formaldehyde
Asbestos
2-naphthylamine
Benzene
Neutron ray
Benzidine
Nickel compounds
Beryllium and beryllium compounds
Radionuclide that emit alpha ray radiation
Bis(chloromethyl) ether and chloromethyl ether
Radionuclide that emit beta ray radiation
Cadmium and cadmium compounds
Talc (containing asbestiform fibers)
Hexavalent chromium compounds
Vinyl chloride monomer
Erionite
X-ray irradiation
Group 2-A.
Acrylic amide
Indium phosphide
Butadiene acrylonitrile
Inorganic lead compounds
Diethyl sulfate
Methyl methanesulfonate
1,2-dimethylhydrazine
Tetrachloroethylene
Dimethyl sulfate
Trichloroethylene
Epichlorohydrin
Vinyl bromide
Ethylene dibromide
Vinyl fluoride
Group 2-B.
Acetaldehyde
Dioxane
Acrylonitrile
Lead
Carbon tetrachloride
Magenta
Catechol
Metal nickel
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Safety Manual (English version 0.1)
Chloroform
Nitrobenzene
Cobalt
Phenobarbital
Cobalt sulfate
Styrene
Dichloromethane
Vanadium·pentoxide
Gasoline
3.6
Sarin and other specific chem icals
The "Law on the Prohibition of Chemical Weapons and the Regulation of Specific
Chemicals" was enforced on the5thMay 1995. Table 5-6 shows the substances that are
subject to this law (Besides the substances listed, organochemical and specific
organochemical substances are also subject to this law). You must receive permission
from the Minister of Economics, Trade and Industry before manufacturing or using these
specific substances. The possession and transport of these specified substances without
permission are prohibited by the law. It is mandatory to obey the law and to ensure that
appropriate procedures are taken in account in the laboratory when researchers are
handling these chemicals. It is important to note that if you synthesize any of these
substances or their precursors without being aware of the relevant laws, you are still
liable under the law and will be punished accordingly.
In terms of manufacturing, use, and import/export of the specific materials, organic
chemicals and specific organic chemicals, application to the Minister of the Economics,
Trade and Industry is required depending on the group and amount of the substance
involved. When falling under this case, contact the Health and Safety Management
Office in advance.
Table 3-7
Substances subjected to the “Law on the Prohibition of Chemical Weapons
and the Regulation of Specific Chemicals.”
Toxic chemicals
Precursors
Reagent lA
Reagent 1B
See text
See text
Reagent 2A
< Reagent 2B >
Designated
(1) (O,O-diethyl-S-[2-(diethylamino)ethyl]
(1) Compounds (except following
substances
phosphorothioate(amiton), itsalkyl
substances) with a phosphorus
andprotonated salts
atom that is not bonded with a
(2)
carbon atom, except for those
1,1,3,3.,3-pentafluoro-2-(trifluoromethyl)-l
bonded to an alkyl group which is
-propene(PFIB)
designated
1 Group 1
Specified
substances
2 Group 1
20
in
the
specified
IMR, Tohoku University
(3) 3-quinuclidinylbenzylate(BZ)
substances and which has three or
less carbon atoms.
a) Substances described in 1 –4 of
column 3 and column 4 in the
specifiedsubstances shown above.
b)
O-Ethyl-S-phenylethylphosphonod
ithionate (fonofos)
(2) N,N-dialkyl(Me, Et, n-Pr or
i-Pr)phospholamidicdihalides
(3) N,N-dialkyl(Me, Et, n-Pr or
i-Pr)phosphoramidates
(4) Arsenic trichloride
(5)2,2-diphenyl-2-hydroxyacetic
acid
(6) Quinuclidine-3-01
(7) N,N-dialkyl(Me, Et, n-Pr or
iPr)aminoethyl-2-chlorides
and
their protonated salts
(8) N,N-dialkyl(Me, Et, n-Pr
ori-Pr)aminoethane-2- ols
(exemptions:
N,N-dimethylaminoethanol and
N,N-diethylaminoethanol and
their protonated salts
(9) N,N-dialkyl(Me, Et, n-Pr or
i-Pr)aminoethane-2-thiol and their
protonated salts
(10)
Bis(2-hydroxyethyl)
sulfide
(thiodiglycol)
(11)
3,3-dimethyl-2-butanol(pinacolyl
alcohol)
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Safety Manual (English version 0.1)
3 Group
2
Reagent 3A
Reagent 3B
Specified
(1) Carbonyl dichloride(phosgene)
(1) Phosphoryl chloride
substances
(2) Cyanogen chloride
(2) Phosphorus trichloride
(3) Hydrogen cyanide
(3) Phosphorous pentachloride
(4) Trichloronitromethane(chloropicrin)
(4) Trimethylphosphite
(5) Triethylphosphite
(6)Dimethylphosphite
(7) Diethyl phosphite
(8) Sulfur monochloride
(9) Sulfur dichloride
(10) Thionyl chloride
(11) Ethyldiethanolamine
(12) Methyldiethanolamine.
(13) Triethanolamine
The chemical structure of sarin and other specific substances (Reagent lA) and their
precursors (Reagent 1B).have the following names:
(1)Sarin, soman, and their derivatives.
(2)Tabun derivatives.
(3) and (4) VX.
(5)–(13)Sulfur mustards.
(14)–(16)Lewisite.
(17)–(19)Nitrogen mustards.
(20)Saxitoxin.
(21)Ricin.
Sarin
m.p. –57°C; b.p. 147°C
Lethal dose:
0.01 mg/kg
(Potassium cyanide:
10 mg/kg)
(i.e. 0.6 mg for 60 kg weight)
3.6.1
Specific substances
Toxic chemicals (Reagent lA)
(1) O-Alkyl(≤ClO, incl. cycloalkyl.) alkyl(Me, Et, n-Pr or i-Pr) phosphonofluoridates
R1OPO(R2)F.
e.g.
Sarin: O-Isopropyl methylphosphonofluoridate.
22
IMR, Tohoku University
Soman: O-Pinacolylmethylphosphonofluoridate.
(2)
O-Alkyl(~ClO,
incl.
cycloalkyl)N,N-dialkyl
(Me,
Et,
n-Pr
or
or
i-Pr)
i-Pr)phosphonylamidecyanidates R1OPO(CN)NR2R3.
e.g.
Tabun: O-Ethyl-N,N-dimethyl phosphoramidocyanidate
(3)
O-Alkyl
(≤H
or
≤C10,
incl.
cycloalkyl)S-2-dialkyl(Me,
Et,
n-Pr
aminoethyl=alkyl (Me, Et,n-Pr or i-Pr) phosphonothiolates and their corresponding alkyl
and protonated salts, R1OPO(SCH2CHNR2R3)R4.
e.g.
VX: O-Ethyl S-2-diisopropylaminoethyl methylphosphonothiolate.
(4) S-2-Dialkyl(Me, Et, n-Pr or i-Pr) aminoethyl, hydrogen, alkyl(Me, Et, n-Pr or
i-Pr)phosphonothiolates
and
their
corresponding
alkyl
or
protonated
salts,
(R1R2NCHCH2S)PO(OIDR3
(5) 2-Chloroethyl chloromethyl sulfide, ClCH2-S-CH2CH2Cl
(6) Bis(2-chloroethyl) sulfide (mustard gas), S(CH2CH2Cl)2
(7) Bis(2-chloroethylthio)methane, CH2(SCH2CH2Cl)2
(8)1,2-Bis (2- chloroethylthio) ethane (sesquimustard), ClCH2CH2S-(CH2)2- SCH2CH2Cl
(9)1,3-Bis(2-chloroethylthio)-n-propane, ClCH2CH2S-( CH2)2- SCH2CH2Cl
(10)1,4-Bis(2- chloroethylthio)-n-butane, ClCH2CH2S-(CH2)4- SCH2CH2Cl
(11)1,5-bis (2- chloroethylthio)-n-pentane, ClCH2CH2S-( CH2)3- SCH2CH2Cl
(12) Bis(2- chloroethylthiomethyD ether, O(CH2SCH2CH2CD2
(13)Bis(2- chloroethylthioethyl ether (o-mustard), O(CH2CH2SCH2CH2Cl)2
(14) 2-Chlorovinyldichloroarsine (lewisite 1), Cl2AsCH=CH2Cl
(15) Bis(2-chlorovinyl) dichloroarsine(lewisite 2), ClAs(CH=CHCl2
(16) Tris(2-chlorovinyl) arsine (lewisite 3), As(CH=CHCl)3
(17) Bis(2-chloroethyl) ethylamine (HN1), CHsCH2N(CH2CH2Cl)2
(18) Bis(2-chloroethyl) methylamine (HN2), CHsN(CH2CH2Cl)2
(19) Tris (2-chloroethyl)amine (HN3), N(CH2CH2Cl)3
(20) Saxitoxin
(21) Ricin, a kind of albumin contained in castor-oil plant seeds (protein).
Precursors (Reagent 1B)
(1) Alkyl(Me, Et, n-Pr or i-Pr)phosphonyldifluoride, R1POF2
(2)O-Alkyl (H or ≤C10, incl. cycloalkyl) O-2-dialkyl(Me, Et, n-Pror i-Pr)aminoethyl,
23
Safety Manual (English version 0.1)
alkyl(Me, Et,n-Pr or i-Pr)phosphonites and their corresponding alkyl and protonated
salts, R1OPO(OCH2CHNR2R3)R4
(3) O-2-Dialkyl (Me, Et, n-Pr or i-Pr)aminoethyl, hydrogen, alkyl(Me, Et, n-Pr or
i-Pr)phosphonites
and
their
corresponding
alkyl
and
protonated
(R1R2NCHCH2O)PO(OH)R3
(4) O-Isopropyl, methylphosphonochloridate (chlorosarin), (CH3)2CHOPO(CH3)Cl
(5) O-Pinacolyl, methylphosphonochloridate, (CH3)3C(CH3)CHOPO(CH3)Cl
24
salts,
IMR, Tohoku University
Chapter 4 Radiation (radioisotopes) and X-rays
4.1
Effects of radiation
Radiation damage induces a variety of symptoms (such as skin erythema or a reduced white
blood cell count) that appear only when the radiation dose exceeds certain thresholds
(deterministic effect) and that yields cancer or genetic consequences at a certain probability
without the threshold (probabilistic effect).
Current laws and ordinances were established based on the 1990 recommendation of the
International Commission on Radiological Protection (ICRP). The basic concept was to
prevent deterministic effects and regulate probabilistic effects to an acceptable level.
The absorbed dose shows the amount of energy of the radiation transferred to a given
material. A unit of 1 Gy (gray) is assigned to an absorption of energy of 1 J/kg. Even at the
same absorbed dose, the effect on living systems differs depending on the type of radiation,
and on the type of tissue or organ absorbing the radiation. In order to include these factors,
the effective dose with the unit, Sv (sievert), is defined. People engaged in handling radiation
must not be exposed to ≥ 100 mSv over a five year period (the effective dose limit).
Incidentally, people is exposed to ~ 0.05 mSv during an X-ray photofluorography and ~ 0.6
mSv during an X-ray examination of the stomach. According to the United Nations Scientific
Committee we are exposed to a yearly average of 2.4 mSv of naturally occurring radiation,
including radiation from within the body.
The deterministic effect that occurs in one incident of exposure at the lowest threshold is the
reduction of the number of lymph corpuscles, at 250 mSv.
4.2 R adiation regulations
Substances/items that can generate radiation are classified into three categories:(1) nuclear
fuel material, (2) radioisotopes (RI)/radiation generators and (3) radioactive medicine. The
radioactive medicine is not the object of our researches in the IMR so that they will not be
covered in this document. Nuclear fuel material is regulated by the "Act for the Control of
Nuclear Materials, Nuclear Fuel Materials and Atomic Reactors" (Reactor Regulation Act),
whilst radioisotopes/radiation generators are regulated by the "Law Concerning Prevention
from Radiation Hazards due to Radio‐Isotopes, etc." (Radiation Hazard Prevention Law).
While electron beams with a voltage of less than one million electrons and X-ray generators
are not covered by the Radiation Hazard Prevention Law, they are regulated by the "Ordinance on
Prevention of Ionizing Radiation Hazards" (Ionization Ordinance) of the Industrial Health and
25
Safety Manual (English version 0.1)
Safety Act. However, while basics are established with laws, more specific concerns are defined in
enforcement ordinances, enforcement regulations, announcements, etc. These are collectively
referred as laws and ordinances.
4.2.1 A dm inistrative structure in the institute for m aterials research
The IMR has established the "Institute for Materials Research, Tohoku University, Radiation
Hazard Prevention Regulations" based on the Radiation Hazard Prevention Law. The
regulations establish a Radiation Hazard Prevention Committee within the IMR which
regulates radioisotopes and X-ray generators, post a Radiation Protection Chief, who in
charge of registration of those who will use radiation or X-rays as well as in charge of making
them complete the necessary training and health examinations, and establish rules related to
maintaining and managing a radiation facility. The use of nuclear fuel materials etc. is
regulated by following to these regulations. Figure 4-1 shows the organization chart related
to safety administration of handling radiation.
Nuclear fuel material is regulated by the "Ordinance on Use of Internationally Regulated
Materials" since it is an internationally regulated material. The "Institute for Materials
Research, Tohoku University Measuring Control Regulations" was established in order to
carry out appropriate measuring control of nuclear material. Classification changes of
nuclear fuel materials due to receipt, disposition, or usage is performed under the
responsibility of the Measuring Control Administrator. The classification changes are
reported
monthly
to
the
Ministry
of
Education,
Culture,
Sports,
Science
and
Technology/Safeguard Office and the International Atomic Energy Agency (IAEA) via the
Nuclear Material Control Center.
26
IMR, Tohoku University
Figure 4-1.
Radiation safety administration organization chart.
Faculty Council
Radiation
Hazard
Prevention
Laboratory Head
Radiation Protection Chief
Committee
X-ray
Radiation
Radiation
Radiation Facility
Equipment
Protection
Protection
Safety
Supervisor
Management
Inspector
Chief Assistant
Supervisor
Radiation
Control Office
Radiation
Operator
Controlled
Access
Location Supervisor
4.2.2
Radiation operator registration
Radiation operators in the university are classified as:
(1) Those who use non-sealed radioisotopes (RI)/accelerators.
(2) Those who do not use non-sealed radioisotopes (RI)/accelerators but enter controlled
access locations.
(3) Those who handle X-ray equipment.
As a general rule regardless of the category of work, those who will use radiation must first
complete the courses (so-called the general course of the university) held by the Cyclotron and
Radioisotope Center in May and November. It is also necessary to undergo a health
examination for radiation operators administered by the university, before using radiation.
According to the Radiation Hazard Prevention Law, operators classified as (1) or (2) are
referred to as "radiation workers." Those classified as (2) and will conduct experiments on
sites such as SPring-8 are exempt from the practical training in this course that uses
non-sealed radioactive material.
To be registered as a radiation operator, first submit an designated registration application
to the Laboratory Head (general affairs section) via the laboratory/center/etc. you are
assigned to. Submitted applications are investigated by the Radiation Hazard Prevention
27
Safety Manual (English version 0.1)
Committee. To those who are registered the booklet for radiation operations is delivered.
Those classified as (1) and (2) are given a red booklet. The booklets given to those classified as
(2) are printed as SOR [synchrotron–orbital–radiation] on their covers: the holder of the
booklet are prohibited from the operation of using radioisotopes etc. Those classified as (3)
are given a blue booklet.
4.2.3 U se of other facilities
In order to carry out radiological work in other facilities (e.g. at another university etc.), it is
necessary to submit an designated application for the relevant facility. There are also cases
where the radiation operator will need to complete courses at the relevant facility. It is
especially important to note that if someone is willing to enter controlled access locations
such as SPring-8, he or she is needed to be an registered radiation worker in IMR after the
completion of the general course prior to the entrance.
4.3 R adiation use precautions
4.3.1 R adiation operator duties
Duties when performing radiological work include carrying a glass badge dosimeter and
having a health examination (including two interviews) twice per year. Furthermore,
radiation workers classified as (1) and (2) (i.e. those with the red booklet) must attend
complete the education and training course (i.e. the retraining) once per year. Additionally,
the amount of radiation exposure and results of the health examination must be recorded in
the booklet.
Glass badge dosimeters
The following types of glass badge dosimeters are used:
(1) For X-rays (FX): a X-ray monitor (for those who uses only X-ray equipment).
(2) Wide Range (FS): a X-ray, gamma ray, and beta ray monitor (for those who use
RI/accelerators).
(3) Neutron Wide Range (NS): a X-ray, gamma ray, beta ray and neutron ray monitor (for
those who use RI/accelerators/nuclear reactors and have a risk to be exposed to neutrons).
Glass rings are available for those whose hands, feet, etc. have a risk to be exposed to
radiation.
28
IMR, Tohoku University
4.3.2 R I usage precautions
The three principles for the protection from external exposures when using non-sealed RI are:
(1) time, (2) distance and (3) shielding. In other words, we practice cold runs in order to
reduce time for working with radioactive material. Do not touch radiation sources or
irradiated samples directly. Instead, use tools such as tweezers or tongs to keep the distance
from the sources or samples. Finally, in order to perform shielding, use lead blocks or lead
glass.
When using non-sealed RI, place a survey meter near the working location whose dosage rate
is relatively low so that you can check your body etc. for contamination as required. If
contamination could be found, do not move around but stay there. In order to prevent
spreading the contamination, be sure to call someone else and make him/her report to the
administrative office. Also, be sure to work with other person when you use RI and there is a
risk of contamination. Avoid working on days off and at night when no one is around.
4.3.3 X-ray equipm ent usage precautions
X-ray equipment normally must be placed in a radiation equipment room with safeguards as
a controlled access location. It is not necessary to be placed in a radiation equipment room if
the condition of "controlled access location is limited to within the box" is satisfied.
Most of the X-ray equipment located in IMR corresponds to this "controlled access location
limited to within the box only" category."Radiation Equipment Room Installation Standards"
and "Conditions When Controlled Access Location is in the Box Only" regulated by the
Ionization Ordinance are as follows:
(1) Radiation Equipment Room Installation Standards(Ionization Ordinance, 15.1).
- The dose equivalent to a rate of one centimeter by external radiation >20 µSv/h. Therefore,
it is not necessary to establish a radiation equipment room if the threshold of 20µSv/h is not
exceeded.
(2) Conditions When Controlled Access Location is limited to within the Box (Ionization
Ordinance, 13.1.1).
- The effective dose of external radiation + effective dose of radioactive material in the air is
1.3 mSv over three months.
Explanation
- Radioisotopes are not used in X-ray rooms, thus only the effective dose due to the external
radiation needs to be considered.
- We can assume that there are 13 weeks in three months, thus 1.3 mSv/three months is 0.1
mSv/week. By assuming a 40-hour working week, this means the effective dose ≤2.5
29
Safety Manual (English version 0.1)
µSv/h(The effective dose can be taken as a one-centimeter dosage rate).
- The worker must not place his or her body in whole or in part into the box.
- It must be structured with an interlock so that anything not enclosed in the box is exposed
to X-rays.
- The worker must not be able to easily unlock the interlock.
An X-ray equipment inspector is posted in each laboratory at the IMR. Whilst the laws and
ordinances do not require that an authorized chief X-ray inspection engineer to be posted for
each piece of "controlled access location is limited to within the box" equipment, all the X-ray
equipment inspectors are preferred to be the authorized chief X-ray inspection engineer (i.e.
license holders). The official duties of X-ray equipment inspectors include X-ray equipment
maintenance, compliance with instructions by the radiation protection chief in order to
prevent radiation hazards, and measurement of the working environment every six months
(at a one centimeter dosage rate).
(2) Conditions When Controlled Access Location is limited to within the Box (Ionization
Ordinance, 13.1.1).
- The effective dose of external radiation + effective dose of radioactive material in the air is
1.3 mSv over three months.
Explanation
- Radioisotopes are not used in X-ray rooms, thus only the effective dose due to the external
radiation needs to be considered.
- We can assume that there are 13 weeks in three months, thus 1.3 mSv/three months is 0.1
mSv/week. By assuming a 40-hour working week, this means the effective dose ≤2.5 µSv/h
(The effective dose can be taken as a one-centimeter dosage rate).
- The worker must not place his or her body in whole or in part into the box.
- It must be structured with an interlock so that anything not enclosed in the box is exposed
to X-rays.
- The worker must not be able to easily unlock the interlock.
An X-ray equipment inspector is posted in each laboratory at the IMR. Whilst the laws and
ordinances do not require that an authorized chief X-ray inspection engineer to be posted for
each piece of "controlled access location is limited to within the box" equipment, all the X-ray
equipment inspectors are preferred to be the authorized chief X-ray inspection engineer (i.e.
license holders). The official duties of X-ray equipment inspectors include X-ray equipment
maintenance, compliance with instructions by the radiation protection chief in order to
prevent radiation hazards, and measurement of the working environment every six months
(at a one centimeter dosage rate).
30
IMR, Tohoku University
It is necessary to display the "controlled access location (Figure 4-2), precautions, and name
and contact information of the X-ray inspector" on the surface of the equipment.
Notification must be sent to the Labor Standards Supervision Office, 30 days before installing
equipment that generate X-rays.
Figure 4-2. Radiation control area
marking.
31
Safety Manual (English version 0.1)
Chapter5
5.1
Laser appliances
G eneral caution
The potential risks to the human body posed by laser beams must be carefully controlled
and avoided. Laser damage to the eyes and the skin is particularly hazardous.
Ultraviolet laser beam burns to the retina can cause irreversible damage to vision.
Continued skin exposure to a laser may cause skin cancer. Laser beams, depending on
their intensity and the risks they present with regard to eye damage, are classified into
four categories, from Class 1 (negligible risk) to Class 4(extremely hazardous). It is
important to know which class of laser you are going to work with prior to starting
experimental work and to take all the necessary safety precautions required. All
procedures must be carried out safely and correctly at all times.
The following precautions for safety only refer to open-type laser beams, which are
emitted outside the equipment casing. It is also important to be careful with closed-type
equipment especially when the protective shields are removed during routine inspection
and maintenance.
(1) Indicate "DANGER" when using a laser beam (especially for Class 3 or higher lasers)
on the door of the room where it is being used. Make sure that no one inexperienced
comes into the room while the laser beam is in use.
(2) Attention must be paid to handling the high voltage power supply, since laser
equipment is typically powered by high energy capacitors. When replacing the laser
excitation lamp, make sure the power supply breaker is switched off. Whilst working,
never let others operate the power supply.
(3) When using an ultraviolet laser, be aware if ozone and other toxic gases are being
generated. In particular, when using the eximer laser, make sure the room is well
ventilated.
(4) Do not directly expose any part of your body to high power laser beams (especially for
Class 3 or higher lasers). As well as the risk of skin burns, disorders that may result in
tissue degeneration and skin cancer, there is a risk that your clothing may catch fire.
Users are advised to wear fire-resistant work wear.
(5) Only a qualified controller with sufficient knowledge and training or an entrusted
delegate of the qualified controller are allowed to operate hazardous laser equipment
(Class 3 or higher lasers).
5.2
Precautions to protect eyesight
Laser beams can penetrate the eyeball, concentrating energy, which burns the retina of
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the eye. The duration of emissions from a pulsed laser flash is very short and the laser
light enters the eye directly. It should be noted that only visible light provokes a
protection response in humans by closing their eyelids. Extreme care must be taken at all
times when using high-powered lasers.
(1) To avoid laser beams from unexpectedly penetrating the eye, never mount the laser
equipment at eyelevel.
(2) To minimize the potential risk of eye damage, ensure that the workroom is well lit so
that the eye pupils remain small.
(3) Never reflect the beam off a highly reflective object. Remove your wristwatch when
calibrating the equipment.
(4) When using invisible-band lasers such as infra-red or ultraviolet lasers, anticipate the
paths of the beam and confirm where the light is reflected or scattered using for example,
an infrared viewer or fluorescent plate prior to laser use. Pay attention to what
co-workers in the vicinity of the laser are doing and alert them to what is going on.
(5) Never look into any of the following:
the laser source, scattered rays or
glass-reflected rays, even from a low-energy (low class) laser sources. Stay alert and take
care of your eye position while calibrating the axis since it is possible that the laser can
suddenly resonate and start emitting.
(6) Wear eye protection when using highly dangerous lasers (Class 3B or higher lasers).
The eye protection must adequately correspond to the laser wavelength in use. Do not
remove your eye protection without being absolutely sure that it is completely safe to do
so and do not stand in the direct path of a laser beam. Do not look directly into the laser
beam since protective glasses cannot completely kill the laser beam. Please note that eye
protection are for back-up purposes only and are only to be considered as an added safety
precaution after learning and completing the necessary laser safety training,
management and operating procedures.
(7) In the case of a pulsed YAG laser, there is subsidiary beam radiation that is emitted
in directions with a ~ 1% variation from the main beam, which is killed using the
absorbent. Be sure to place a protective shield behind the absorbent to prevent the
subsidiary beam being directed at the user because the absorbent is moved when
measuring the intensity of the main beam.
(8) Wear eye protection when changing the operating conditions of the laser equipment.
When making a change to the laser path, confirm the beams direction and where and
how the beam is scattered using an infrared viewer.
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Chapter 6 High pressure gas and liquefied Gases
6.1
Introduction
There are many gases stored and used in the IMR. Amongst these, there are many explosive
and highly poisonous gases. So it is important to use caution when handling them. Even inert
gases that are not explosive or poisonous and appear safe have possibilities to cause the
oxygen deficiency and the explosion originating from the low-temperature embrittlement and
the sealing when they are at high pressure/low temperature state.
6.2
Types of dangerous gases
6.2.1
Types of gases
Combustible Gases: H2, CO, NH3, H2S, methane, propane, city gas etc.
Combustion Enhancing Gases: Air, oxygen, ozone, chlorine, NO, NO2 etc.
Explosive Gases: Mixure of combustible and combustion enhancing gases and the gases such
as silane, alkylamine, metallic hydride and organometallic compounds. These gases will
explode when they are mixed with air.
Inert Gases: Nitrogen, carbon dioxide, helium, argon, etc. These gases are not harmful alone,
but may cause oxygen deficiency state.
Liquefied Gases: Liquid nitrogen, liquid helium, dry ice etc. Use caution when handling these
gases as frostbite, oxygen deficiency or explosion in a sealed environment may occur.
Poisonous Gases: Chlorine, fluorine, hydrogen chloride, hydrogen sulfide, hydrogen cyanide,
arsine (AsH3), phosgene, silane, ozone, etc.
Corrosive Gases: Chlorine, hydrogen chloride and ozone. These gases corrode metal, rubber,
plastic and other materials.
6.2.2
H andling explosive gases
(1) When combustible gases and combustion enhancing gases are mixed at a certain ratio,
they are treated as explosive gases. They are generally mixed with air and their explosive
limits are summarized in Table 6-1. When using mixed gases, be sure to check the mixed
explosive limit for each gas.
(2) Use caution as the ignition sources for mixed gases include not only naked flames, but also
heat, static electricity sparks, shocks and fine metallic powders.
(3) Pay attention to the ventilation in the room and be careful that you do not approach the
explosive limit even when a gas has leaked.
(4) When handling special gases, look up the properties of the gases, ask for an experienced
person to direct you and follow all the safety rules.
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Table 6-1
Explosion limit of common gases in air (at 1 atm and ambient temperature)
(Digits represent the volume fraction in percentage of combustible gases)
Lower
Gases
Limit
Upper
Gases
Limit
Acetylene
2.5
100.0
Benzene
1.3
Toluene
Lower
Upper
Limit
Limit
Hydrogen sulfide
4.0
44.0
7.9
Hydrogen
4.0
75.0
1.2
7.1
Carbon monoxide
12.5
74.0
Cyclopropane
2.4
10.0
Methane
5.0
15.0
Cyclohexane
1.3
8.0
Ethane
3.0
12.5
Methanol
6.0
36.0
Propane
2.1
9.5
Ethanol
3.3
19.0
n-Butane
1.8
8.4
Isopropyl alcohol
2.0
12.7
Pentane
1.4
8.3
Acetaldehyde
4.0
60.0
n-hexane
1.1
7.5
Ether
1.9
48.0
Ethylene
2.7
36.0
Acetone
2.5
13.0
Propylene
2.0
11.0
Ethylene oxide
3.0
100.0
1-Butene
1.6
10.0
Propylene oxide
2.0
22.0
Isobutylene
1.7
9.6
Vinyl chloride
3.6
33.0
1,3-Butadiene
2.0
12.0
Ammonia
15.0
28.0
Ethylene tetrafluoride
10.0
50.0
Carbon Disulfide
1.2
44.0
6.2.3
H andling poisonous gases
Even a small amount of poisonous gas can cause a serious accident. So the utmost of care and
knowledge is required in their use. Be absolutely sure to investigate the gases you will use in
advance, provide neutralizers and install leak sensors/security alarms. Also, be sure to
investigate antidotes and emergency measures, and make them available in case of an
accident.
.
Table 6.2 shows the allowable concentration of toxic substances (TLV-TWA) published by the
American Conference of Governmental Industrial Hygienists (ACGIH). The allowable
concentration indicates the time-weighted average concentration of a poisonous gas in a
working environment, where daily exposure during an eight hour working day does not have
an effect on the health of an otherwise healthy person.
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Safety Manual (English version 0.1)
Table 6.2
Threshold limit values (TLV) of toxic gases.
Gas
TLV
Gas
（ ppm
TLV
（ppm）
）
Ammonia
25
Acetone
500
Carbon monoxide
25
Benzene
0.5
5,000
Methanol
200
Carbon dioxide
Chlorine
0.5
Fluorine
1
Bromine
0.1
Ethanol
1,000
Diethylamine
5
Acetic acid
10
Ethylene oxide
1
Ethyl acetate
400
1,3-Butadiene
2
Butyl acetate
150
Nitrogen monoxide
25
Vinyl chloride
5
Hydrogen sulfide
10
Toluene
50
Hydrogen cyanide
10＊
Normal hexane
50
Hydrogen chloride
2＊
Acrylonitrile
2
Phosgene
0.1
Methyl bromide
1
Sulfur dioxide
2
* This is a gas that causes acute poisoning. This value indicates the uppermost value of the
concentration that must not be exceeded even for a short time.
6.3
H igh pressure gases (gas cylinders)
Many kinds of gases are currently used in high-pressure gas containers (cylinders). Whilst
gases tend to be handled with ease since they can be obtained upon opening and closing a
valve, misuse can result in a major accident depending on the properties of the gas involved.
Therefore, the following basic knowledge and precautions are necessary in order to prevent
accidents related to the use of compressed gases.
(1) A caved seal located on the shoulder of the high pressure gas container (cylinder) shows:
the name of the gas contained, container number/serial number, capacity (symbol: V, unit:
liter), container weight (weight without the valve or cap, symbol: W, unit: kg), pressure test
data, pressure test pressure (symbol: TP, unit: kg/cm2) and maximum fill pressure (symbol:
FP, unit: kg/cm2).
(2) The maximum fill pressure for compressed gases is the value at 35 °C (15 °C for
acetylene).
(3) High pressure containers (cylinders) are colored according to the gas they contain, as
shown in Chart 6-3.
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Table 6-3
Colors of high pressure gas cylinders.
Gases
Oxygen
Hydrogen
Cylinder
Gases
color
Black
Argon
Cylinder
color
Grey
Red
Nitrogen
Grey
Carbon dioxide
Green
Methane
Grey
Ammonia
White
LP-gas
Grey
Chlorine
Yellow
Carbon monoxide
Grey
Acetylene
Brown
Ethylene
Grey
(4) When moving and transporting high pressure gas containers (cylinders), release the
decompression valve (adjuster), attach the valve protection cap and use the push cart made
specifically for the container.
(5) In principle, the gas filling port screw for combustible gases is the left screw, whilst those
for other gases are the right screws. However, the container for ammonia gas has the right
screw and that for helium gas, which is an inert gas, has the left screw out of habit. So be
careful.
(6) When the residual pressure of the container reaches zero, air may enter the container and
effects the purity of the gas. Do not use the gas until the residual pressure becomes the same
or lower than the external pressure (1 MPa).
(7) In addition to precautions (1)–(6), when handling high-pressure gas cylinders in the IMR,
manage them according to guidelines outlined in section 6.4 "High Pressure Gas Cylinder
Management."
(8) The handling of the high pressure gas is accompanied with the opening and closing of the
valve. Generally, when opening a valve, completely open and then close it slightly so that
lightly turning the valve is considered to be opening it. In contrast, when closing it, do so
until the valve it tight. However, tightening the valve too much could damage it and cause a
leak.
6.4
H igh pressure gas cylinder m anagem ent
6.4.1
Security training
Perform security training periodically in each laboratory, center or facility. Record the name,
details of the training, and implementation date, and then report this information to the
Safety and Health Management Office.
6.4.2
Register
Register high pressure gases in the management system for lab chemicals (IASO).
6.4.3
G as cylinders
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(1) As a general rule, use the cylinders borrowed from gas venders. They should not be owned.
In case of owning the cylinders which are not used, dispose of them after consulting with the
Procurement Management of Administrative Office (ext 2975).
(2) Only place the minimum amount of gas cylinders necessary in each laboratory. As a
general rule, do not use them for longer than one year. Return cylinders that have been used
for one year to the vendor. Report to the Safety and Health Management Office if you would
like to use a cylinder for more than one year.
(3) Store filled containers (unused containers) and containers with left-over gas (used or
empty containers) separately.
(4) Store combustible gases and oxygen separately.
(5) Place combustible gas and poisonous gas cylinders in a well-ventilated area, and store at a
temperature < 40 °C.
(6) Take measures to prevent tipping.
(6-1) Use two chains with no slack to secure a cylinder (do not use a single chain only).
(6-2) Install anti-tip measures that are suitable for the size of the gas cylinder in use (even
when using small cylinders).
(7) When installing a regulator or piping to a gas cylinder, use a leak detection agent to
confirm no leakage is occurring.
(8) When a gas cylinder is not in use, remove the regulator, store it with the dedicated lid
attached.
(9) Indicate the delivery date and type of gas on the gas cylinder. Also, attach an opening and
closing tag.
(10) Secure access to the gas cylinder so that its valve can be opened and closed in an
emergency.
(11) Implement a total fire ban within five meters of combustible gas cylinders (such as
hydrogen, acetylene, ethylene, methane, propane, etc.) and install a fire extinguisher.
6.4.4
Cylinder w arehouse
The cylinder warehouse is a temporary storage area used in the period from the time when
contracted vendors deliver filled cylinders to the time when they are taken by the laboratory
and in the period from the time when the laboratory returns empty cylinders or those with
left-over gas until the vendor takes them. It is not authorized to use the cylinder warehouse
as a storage place of spare cylinders.
Deliveries
(1) Do not leave cylinders in the cylinder warehouse. Quickly take cylinders that have arrived
to the laboratory.
(2) Do not remove the delivery date tag until the cylinder has been taken to the laboratory.
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Returns
(1) Return cylinders with caps attached.
(2) Separate incombustible gases, combustible gases and poisonous gases.
(3) Gas cylinders not borrowed from contracted vendors will not be automatically collected
even if you returned them to the cylinder warehouse. In that case, contact the corresponding
vendors directly and ask them to pick-up the cylinders.
6.4.5
Transportation
(1) Always be sure to transport high pressure gas cylinders and liquid refrigerants with two
people.
(2) When using an elevator, any people must not ride in the elevator.
6.4.6
O ther
(The Safety and Health Management Office [ext 2986] must be consulted with)
(1) Notification of consumption must be sent to Sendai city in advance if you will be using
special high pressure gases (such as silane, phosphine, arsine, diborane, hydrogen selenide,
monogermane, disilane).
(2) A manufacturing license from Sendai city or a notification to Sendai city, depending on the
capability, is required in advance when manufacturing high pressure gas.
6.5
Cryogens
In order to handle cryogens (low temperature refrigerants) it is necessary undertake
appropriate training via a course and e-learning with examination. Even if someone else with
experience accompanies you, it is necessary to study via e-learning and take an exam in order
to handle these materials in the IMR.
6.5.1
Liquid nitrogen and liquid helium
Liquid nitrogen and liquid helium are used as cryogens (low temperature refrigerants) and
are created through repeated gas compression and semi-adiabatic expansion (and in case of
liquid helium, Joule-Thomson expansion process is added). Liquefied helium and nitrogen
gases are kept at very low temperatures of 4.2 K and 77 K, respectively, and they are
normally used at the normal pressure (the pressure of the atmosphere). The material parts
that make up cryostat (low temperature refrigerant manufacturing equipment) are exposed
to extremely low temperatures, which may cause low-temperature embrittlement or breaches
with ease. So they must be handled with extreme care.
In order
to maintain thermal insulation, the cryogen containers consist of a double
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structure made from thin metal pipes,
which are mechanically weak. It is therefore
necessary to be careful not to cause breaches in containers when transporting them. It is
especially dangerous if a container tips over. When handling low temperature liquefied gases
or utensils that have been refrigerated at a low temperature, it is important to wear
protective leather gloves. Gloves that are made of materials that absorb and retain liquids,
such as cotton gloves, have a high chance of causing low temperature burns (frostbite) and
therefore must not be used.
(1) Cryogens (low temperature liquefied gases) may cause frostbite, so do not touch them with
your bare hands or fingers.
(2) Using cryogens - such as liquid nitrogen or liquid helium in a sealed room could cause
oxygen deficiency, so be sure there is sufficient ventilation.
(3) Install safety measures such as safety valves or rupture disk (protective boards) on
containers or experiment equipment to protect against explosions caused by sudden
evaporation.
(4) When heat is introduced from outside into the piping where the low-temperature liquefied
gas is confined with the valve closed, the liquefied gas is vaporized and its pressure increases.
The piping may rupture, causing an explosion. Do not keep the cryogen in a sealed structure.
6.5.2
H ow to use liquid nitrogen
At the IMR, researchers can fill liquid nitrogen into the container by themselves 24 hours a
day (self-service; not available during New Year and summer holidays periods) at the Helium
Provision Room in Building #1 (Room #109). For large containers (such as 100 L or 50 L),
liquid nitrogen is transferred directly from the large storage tank built outside (Cold
Evaporator [CE]) using the Automatic Provision System. It is necessary to register containers
beforehand at Center for Low Temperature Science (Low Temperature Science Division) and ,
obtain a card with two kind of barcodes issued for each container and each laboratory.
Transferring liquid nitrogen to an unregistered container or to one with the wrong barcode
could cause a severe accident and is prohibited. While pumping liquid nitrogen, do note stay
away from the provision room and monitor that the operation is being conducted normally.
For small containers such as 5 L, 10 L, and 20 L, transfer liquid nitrogen manually from the
100 L container (called “selfer”) located in the provision room. Information on how to transfer
liquid nitrogen and how to fill out forms is posted in the provision room.
6.5.3
H ow to use self-pressurized liqu id nitrogen containers (selfers)
(1) Selfers are liquid nitrogen containers with a self-pressurizing function.
Structure
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There are three valves (liquid ejection valve, gas release valve and pressure increase valve), a
liquid nitrogen refill inlet tube, a safety valve and a pressure gauge attached to the top
portion.
Principles
Opening the pressure increase valve vaporizes a portion of the liquid nitrogen in the selfer
and increases the internal pressure. This pressure is used to push liquid nitrogen out via the
liquid ejection valve.
Usage
i) After having inserted an inlet tube in a small container, close the release valve and open
the ejection valve. Gradually opening the pressure increase valve increases the internal
pressure and liquid nitrogen is pushed out via the ejection valve. The amount of internal
pressure depends on the low temperature container which the liquid nitrogen is pumped into.
A pressure of ~ 0.1–0.2 kgf/cm2 is sufficient for small containers or glass dewars. A pressure of
~ 0.4–0.5 kgf/cm2 may be required for larger containers. However, most of containers will
hardly ever require more pressure than these amounts.
ii) To stop transfer liquid nitrogen, close the pressure increase valve and ejection valve, then
open the release valve so that the internal pressure decreases (Leave the release valve open.)
(2) Warnings for refilling selfers with liquid nitrogen
When the refill port (screw-type) on the upper portion is opened to refill a selfer with liquid
nitrogen from the large storage tank in the Helium Provision Room, be sure to confirm
beforehand that the gas release valve is open and the internal pressure is reduced. If the
internal pressure is high, it is very dangerous to remove the screw-type stopper since it may
jumped out. There are also some containers that must be filled via the liquid ejection valve.
Since a dedicated connection tool is supposed to be used in this case, you must ask some staff
in Center for Low Temperature Science and obtain one for each laboratory.
(3) General precautions for opening and closing valves
There is no need to use excessive strength when opening and closing valves. In particular, if a
valve is turned all the way to open, it may get stuck. It is better to completely open it and
then close it slightly. Likewise, if the valve is closed too much tightly, the seal could be
damaged. Never use tools such as a spanner or plier to open and close valves.
6.5.4
H ow to use liquid helium
(1) Handling liquid helium.
In order to use liquid helium safely and efficiently, it is necessary to always make several
checks before and after use. Be sure to always "point and call" valve operation, pressure
confirmation and piping connections. Additionally, always be on the lookout for abnormal
sounds, abnormal frosting and the formation of ice during operation and during experiments
(e.g. the sound of gas leaking and abnormal frost formation on recovery piping). Helium gas is
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Safety Manual (English version 0.1)
similar to nitrogen gas in that it is a tasteless, odorless, and colorless gas. Abnormal sounds
may be related to a gas leak, while abnormal frosting may be caused by an abnormal increase
in the evaporation of liquid helium (via degeneration of the adiabatic vacuum layer of the low
temperature container or heat due to quenching of a superconductive magnet). So if there is
an abnormality it is necessary for an experienced person to handle the situation immediately.
If anything is unclear, do not attempt to handle the situation by yourself. Contact the
technical staff of Center for Low Temperature Science (ext 2807) and request advice. When
you are unsure of how to handle something, have someone from the center meet with you
immediately.
(2) Transferring liquid helium to equipment.
i) Adding liquid helium when liquid helium is already in equipment.
When the room temperature transfer tube (a dedicated shielded tube with a dual-tube
construction) is inserted into the vessel (the container for liquid helium) and makes direct
contact with liquid helium, a large amount of helium will naturally evaporate, resulting in an
increase in pressure. Therefore, insert the transfer tube slowly whilst watching the pressure
gauge. It is desired that the gauge pressure does not exceed 0.1 kgf/cm 2.
When inserting the transfer tube into the vessel, open the needle valve slightly (if it is
attached) and pass a small amount of helium gas through the tube (if there is no needle valve,
helium gas will naturally blow out from opposite side. So insert the tube slowly to control the
amount). It is not necessary to make so much gas flow that a loud hissing noise is created.
The air in the tube should be replaced by helium gas. If this is not done, the air inside the
tube may freeze and become stuck, so it is necessary to purge the air sufficiently. If it
becomes stuck, remove the tube from the vessel, warm up the entire tube using a hair drier or
similar tool whilst passing dry nitrogen gas (if available) through the tube. If any frost has
formed, remove the frost and start over from the beginning.
Once the gas in the tube has been replaced, insert the other side of the transfer tube into the
low temperature equipment (or the container of it). When adding liquid helium, you should
insert the tip of the tube above the position of liquid surface in filling up the container. In
case of assembled transfer tube, connect the parts completely. Consider the position of the
helium vessel and low temperature equipment, so that excessive force is not applied to the
transfer tube (as the tube is made from thin-walled pipe, it bends easily). Close the vessel's
collection valve. Make use of the pressure build up caused by natural evaporation in the
vessel for some time (several minutes) and slowly pass the evaporated gas through the tube
to cool it (the vessel pressure at this point depends on the recovery line pressure, a pressure
of 0.05–0.1 kgf/cm2 is typical). Once the gas within the tube freezes and it starts to become
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liquid, completely open the needle valve if there is one (1–2 turns is enough, if it is attached),
apply external pressure using helium gas as needed and begin transferring liquid helium. If
this is done too quickly, warm helium gas will pour swiftly into the liquid helium remaining in
the low temperature equipment, leading to quick evaporation. This will increase the amount
lost during transfer. A vessel gauge pressure of 0.1–0.15 kgf/cm2 is sufficient during transfer.
The pressure of the low temperature container or the amount of evaporation may increase
when transferring helium. This is often due to oscillating phenomena (pipe resonance
vibration) that occurs as a result of various parameters such as the internal structure of the
low temperature container, the height of the helium's liquid surface, the position of the
transfer tube or impressed pressure. However, it is often difficult to determine the reason for
the increase in pressure. Try decreasing or increasing the pressure slightly or changing the
height of the transfer tube. If the condition does not improve or seems dangerous, stop
pressurizing of the vessel, open the collection valve and stop transferring helium.
When the required amount of helium has been transferred to the low temperature container,
stop pressurizing the vessel (by closing the pressurization valve), then open the collection
valve. Once the pressure in the vessel has decreased, close the needle valve (if it exists) on the
transfer tube. If the tube is composed of multiple needle valves (in case of assembled transfer
tube), close only the one that is nearest to the vessel (if multiple valves are closed
simultaneously, liquid helium and cooled helium gas remaining in the piping will warm up
and expand, resulting in a serious accident where the transfer tube ruptures).
Remove the transfer tube from the equipment and remove the transfer tube from the vessel
(if the transfer tube is made of hard metal piping and therefore not flexible, remove both
sides simultaneously, so as to not bend it). As the tube is cold, do not touch it with your bare
hands. Instead, wear leather gloves. Do not use a cloth, handkerchief, cloth gloves or other
materials under any circumstances.
When finished, point and call as you check the open/close state of each valve, the container,
and the pressure of the vessel.
ii) Transferring liquid helium into the empty container (not cold equipment) .
Thoroughly remove air and water from the space where liquid helium is stored using a tool
such as a pump before precooling with liquid nitrogen. The method differs depending on the
container or the way the experiment will be conducted (for example, liquid nitrogen may be
inserted directly into the helium space or it may be inserted into the liquid nitrogen space
surrounding the helium space to cool it indirectly). In general, this involves lowering the
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temperature of the space where helium is stored to around the same temperature as the
liquid nitrogen, preventing air and water from mixing during precooling, and then making
sure no liquid nitrogen is left in the helium space and replacing the atmosphere with helium
gas immediately before transferring liquid helium.
Transfer the helium into a container that has been precooled. The transfer tube should be
inserted as close to the bottom of the container as possible, which is different manner from
the case of adding liquid helium. If necessary, attach an extension tube to the tip of the inlet
tube. This is because cooling is performed using a sufficient enthalpy of vaporized helium gas,
since the evaporative latent heat of liquid helium is low. Therefore, it is better to keep the
amount transferred as low as possible until the internal temperature of the container or the
temperature of the cooling equipment (such as magnets) is 4.2 K (i.e. until liquid helium
starts collecting). If so much is transferred that the collection piping turns white, the cooling
time will shorten but the amount of liquid helium expended will increase.
Once liquid helium begins to collect, apply pressure in the same manner as the case of adding
liquid helim.
(3) Returning helium vessels
Do not use all of the liquid helium in the vessel. Instead, leave ~ 15% or more. This is because,
if there is no more liquid helium left, the temperature of the vessel will rapidly increase and a
large amount of liquid helium will be required for cooling when the vessel is filled up next
time. After use, return vessels to the Helium Provision Room (Building #1, Room #109),
connect the vessel's recovery port to the gas recovery line in the room, and record any
necessary information on the white board.
6.6
Safety m easures for handling liquid gases and high pressure gases
When liquid nitrogen and liquid helium are vaporized their volume increases about 700 times.
If these liquids are sealed in an enclosed space they will act like explosives.
Be careful of frost or ice forming around the nitrogen fill port or the gas outlet on low
temperature containers (equipment) that have a liquid nitrogen space. These ports may close
up, causing the nitrogen space to become blocked. Additionally, air may solidify after
penetrating diffusively from the evaporation gas outlet, blocking up the nitrogen space. While
cylindrical containers used in low temperature equipment cannot be easily broken when
pressed from inside (by high internal pressure), they collapse easily when pressed from
outside (by high external pressure). It is very dangerous if the nitrogen tank is obstructed as
it may collapse inward. This leads to crushing the adiabatic vacuum layer.
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It is also extremely dangerous to leave the recovery ports of liquid helium containers exposed
to air without connecting them to the recovery line because liquid helium absorbs air (even
more quickly than liquid nitrogen), solidifies and creates a sealed structure.
Neither helium nor nitrogen is poisonous. However, when they are in the gas phase they are
tasteless, odorless and colorless. This means that their existence or concentration cannot be
detected by sight or smell. When handling these gases or liquids in a sealed room, it is
necessary to always consider the danger of suffocation due to oxygen deprivation. By the time
you realize you are suffocating you will be unable to move and it will be too late.
Oxygen deprivation does not occur after the oxygen in the air has been removed. It occurs
when the concentration of oxygen in the air (usually ~ 21%) is reduced by some percentage.
This means that in a laboratory of normal size, if at least 10 L of liquid nitrogen is vaporized
the concentration of nitrogen will reach a dangerous level. Nitrogen gas is also heavier than
air and accumulates lower to the ground. It is more dangerous on the floor, so never rest on
the laboratory floor.
Remember: At an oxygen concentration of 18%, you will feel uncomfortable.
At 15% your ability to respond will be significantly impaired.
At 10% you will lose consciousness, leading to death.
The vaporized gas is in low temperature state like a liquid. When removing the transfer tube
once helium transfer is complete, if pressure in the container (equipment) or vessel is not
decreased sufficiently, cold gas could shoot out, causing low temperature burns. Additionally,
the O-ring and other parts could freeze by the cold gas and the stopper could be unable to be
used due to the freezing. In this situation, wear a pair of leather gloves (through which gas
will not pass) and attach the stopper in the liquid helium filling port, wait a while until the
O-ring and other parts warm up (if gas is not passing through, it will be cooled further) or
warm the stopper with a hair drier.
Always transport high-pressure gas cylinders or cryogen containers with two people. When
using an elevator, any people must not ride in the elevator along with the gas cylinders or
cryogen containers.
6.7
First Aid w hen there is an accident or fire
(1) When an accident has occurred, notify the people in charge of the laboratory and the
Guard's Room (extension 2119), and request an ambulance (0+119) (do not delay if oxygen
deprivation or suffocation may have occurred).
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(2) When there has been a strong earthquake or when there is a power failure due to
lightning or other phenomena, quickly stop your work, move to a safe location and contact the
people in charge, the staffs of Center for Low Temperature Science and others. Be especially
careful of sudden evaporation of liquid helium due to quenching of superconductive magnets
during power failures.
(3) Prevent explosions resulting from sudden evaporation of liquefied gases by the fall of the
low temperature containers. Prevent suffocation accidents caused by evaporation gas.
(4) Helium gas recovery is automatically interrupted during power failures. It is
automatically restored when power is recovered. If there is an unusual phenomena, contact
the laboratories related to low temperature or Center for Low Temperature Science.
(5) It is forbidden to get on the elevator with a cryogen container, Nevertheless, when shut
with the container in an accident, use the emergency contact equipment in the elevator to
notify someone immediately. Be sure to mention that you are trapped with a container
containing liquefied gas and that there is a high probability of suffocation (in general, the
door should open at the nearest floor).
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Chapter 7 Actions and Contacts in Emergency
7.1 First m ove
In the case of an accident, LET OTHERS KNOW, e.g., by making a loud voice. Even if you
think it is not a serious accident, it is important to notify other people and make an decision
as a group. This will also help them to take an necessary action, including evacuation.
Making decisions and acting on your own may cause a secondary accident and/or increase the
danger of the current situation.
The general rule is to keep yourself from the danger and evacuate the area. If it is judged that
the scale of the accident is not large and personal safety has been confirmed, then one should
take a measure, such as extinguishing fire. After carrying out an initial action, and
confirming that you are safely removed from the accident site, contact first the Guard's Room
and then contact a person in charge of the laboratory, e.g., a professor or assistant professors,
(referred to as the "responsible faculty member"). When initial fire extinguishing is
impossible or when the accident is life-threatening and there is no time to contact the
responsible faculty member, the person who discovered the accident should contact directly
the fire department or other authorities (Fig.3-1). If someone is nearby, ask him/her to make
contact with authorities. Whilst the responsible faculty member and guard are coming, ask
any faculty members or students nearby for support and act as a group. Often, the person
involved with the accident and/or any witnesses are shocked or confused, so it is important to
consult with other people, make decisions as a group and handle the situation as a team.
7.2 Em ergency C ontacts
A sign for emergency contact network of responsible faculty members and regular members,
and the emergency contact numbers, such as shown in the table below, are posted in various
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locations in the office and experimental areas of every laboratory in IMR.
7.3 Standard actions in em ergency
7.3.1 A ccidents w ith injury, intoxication, etc.
· Give him/her first aid
· In a case of serious situations, do not hesitate to call ambulance. The emergency center
in the university hospital is always available for accidents occurred within IMR or other
areas in the university. Therefore, tell the rescue team that he/she needs to be taken to
the emergency center.
· At the same time, call the emergency center, give them necessary information.
· Meanwhile, notify the guard of IMR and those in charge of the laboratory about the
case.
· When it is judged that the accident does not require immediate call for ambulance, fire
station, etc., notify the accident to those in charge of the laboratory, while giving him/her
necessary care.
7.3.2 Fires, explosions, etc.
(1) When you find fire, explosion, etc., let people around you know the incident by making
a loud voice, using fire alarms, etc. Then, notify the fire department and the guard.
(2) Make sure that everyone around you is informed of the situation. Help those injured,
if any. Then, evacuate to the designated safe place.
(3) Countermeasure to the incident, such as extinguishing the fire, can be taken only if it
is safe to do so. Even under such case, never act on your own.
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(4) At the evacuation site, first thing you should do is to CONFIRM THAT EVERYONE
IS SAFE. Remain there until further instruction is given. Do not act independently.
(5) If someone is leaving the site for any reason, such as going to hospital, notify the
leader of the group at the evacuation site before doing so.
7.3.3
Pow er outages, w ater outages, w ater leaks, gas leaks, etc.
(1) Power failure and electrical distribution board malfunctions
i) When an unexpected power failure occurs, the No. 2 Facilities Section confirms
information such as the cause, expected restoration time and measures, in collaboration
with the No. 1 Facilities Department Facilities Administration Division Safety
Technology Section. If power restoration is expected to take a long time, information will
be given using the building broadcast system or by telephone.
ii) When it is judged that the power failure is limited to their own building (e.g., by
checking lights or other signs in other buildings.) or that the problem is with the
electrical distribution board, notify the No. 2 Facilities Section and wait for their
instructions.
(2) Water failure, water leaks, etc.
In the case of an unexpected water outage, water leak, etc., notify the No. 2 Facilities
Section, and must wait for their instructions.
(3) Gas leakage
In the event of combustible gas leakage (such as city gas in laboratories), let people know
and evacuate the area, use fire alarm if it is judged necessary. Notify the fire department
and the No. 2 Facilities Section.
7.3.4
Loss, theft, etc.
When loss or theft of valuables or belongings owned by faculty members, students, or
others in the laboratory has occurred, the site must be secured and a report must be
made quickly to the person in charge of the laboratory and the No. 2 Supplies Section.
The report must explain in detail when and where the loss or theft occurred, and provide
the information of the valuable or belonging in question and any other information
regarding to the loss or theft.
7.3.5
Typhoons
(1) When typhoon warning is announced or when you judge that commuting is difficult,
e.g. no transportation, heavy rain, wind, etc., do not risk yourself coming to the
laboratory.
(2) If a typhoon is approaching whilst you are in the laboratory, respond and act
according to the instructions of the head of the laboratory.
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7.3.6
E arthquakes
(1) Secure your own safety. Once shaking has subsided, turn off gasses, furnaces, etc.
(2) When judged necessary, evacuate to the designated safe site, with a helmet and other
appropriate items available. In case someone is injured or shocked, help them evacuate.
(3) At the site, confirm that no one is missing.
(4) Do not act on your own. Wait for further instructions.
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Chapter 8 Actions in the case of a wide-scale earthquake,
magnitude of greater than five
8.1 O w n safety, fire prevention, first aid and evacuation
Do not wait for a broadcast during a wide-scale disaster. Evacuate according to the Crisis
Management Manual.
(1) O w n safety and fire prevention
Secure your own safety. Protect your head with a helmet. Turn off gas, furnaces, etc.,
that might cause fire. Disconnect electrical power chords. Do not make other unnecessary
actions, such as restoration of the laboratory.
(2) E vacuation
Evacuate to the designated evacuation site. (The primary evacuation site is the area,
south of Building #2, the secondary evacuation site is west of Building #4 and the tertiary
evacuation site is the square to the south of the electron microscopy center.)
At the site, make sure that no one is missing.
(3) A id
If you find anyone who cannot move and needs assistance, inform the Command and
Control Group. Do not enter any location in which the safety cannot be confirmed.
Rescuing actions, e.g., moving out those trapped under an object, must be made as a team
and should be done only if it is judged safe to do so. Transport severely injured people to
the evacuation site or another location. Do not hesitate to apply AED or perform cardiac
massage if necessary.
(4) Fire response
When a fire has occurred, and if it is safe to take a initial countermeasure on site, act as a
group, e.g., by using a fine powder fire extinguisher. Notify the Guard's Room (2119) and
request assistance. Take a necessary actions until the self-defense fire-fighting group
arrives, to whom sufficient information must be given, e.g., the plausible cause of the fire,
potential danger in the laboratory as described in the hazard map, the availability of
discharge water, etc. The self-defense fire-fighting group can prepare a fire hydrant and
will attempt to extinguish the fire.
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8.2
Safety
confirm ation,
transportation
of
the
injured
and
situation
assessm ent in order to prevent the spread of dam age.
After evacuation, confirm everyone's safety, make sure that no one is missing and assess
the situation, such as damage.
(1) Prim ary safety confirm ation
The group leader of each laboratory must confirm the safety of the member, and report
the status to the Safety Confirmation Group. The Safety Confirmation Group will set up
standing boards for further instruction and will carry out a role call. Names of any
severely injured people must be reported immediately to the Safety Confirmation Group.
Confirm the safety of each person according to the list and record their conditions. In
addition, report missing visitors or others if any. If there are many people missing, notify
the Safety Confirmation Group with a rough estimate of the number of the people.
(2) Secondary safety confirm ation
It is the responsibility of the Safety Confirmation Group, based on the given information,
to judge whether or not people are left inside a building. This applies not only to the
member of IMR but also to visitors. Record the status of the people on the list. For
example, if someone is on a business trip, and thus not on the site, record this
information. The confirmation process needs to be carried out within ten minutes after
the earthquake.
(3) Transport of the injured
Carry out emergency measures in cooperation with rescue groups and request emergency
transport for people that are seriously ill or injured. If the transport is expected to take
some time, move the injured to a nearby emergency response hospital, such as the
University Hospital or the Sendai City Hospital. Before the transportation of the injured,
inform the Safety Confirmation Group of the destination, name of the person and any
accompanying people. The division head must also be notified their departure.
(4) Situation report in order to prevent the spread of dam age
After confirming everyone's safety, examine the extent of the damage, and fill out the
Initial Damage Report Form. Some action in order to limit/confine the damage can be
initiated at this stage. For the case that needs an immediate countermeasure, report it to
the head of the office. For other minor damages, record them, and report them to the
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person in charge of liaison and coordination in the Command and Control Group.
Possible cases that require a report:
Fire, presence of apparatuses left on that might initiate fire, e.g., soldering irons and
electric furnaces, spilled chemicals, fallen gas cylinders, fallen refrigerant, scattered
glasses, broken equipment, fallen bookcases, gas leaks, equipment that can be damaged
at the restoration of electricity, etc.
8.3 Initial D am age R eport Form
Record the room name, draw a circle in the appropriate field, and
record any items that need to be taken care of
Ext
1-312
Fire
Water leak
Electrical furnace
or iron left ON
Spilled drugs
Fallen Cylinders
Scattered glass
Broken equipment
Fallen bookcase
Gas leak
Fallen refrigerant
other
comments
and information
Enter other items that must be taken care of at the bottom of the table.
example of comment: In room 1-313, the fallen 10 L nitrogen container may contain full
of nitrogen, an oxygen check is required before entering the room
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8.4 R eturning hom e or m oving to a shelter
In the case of a wide-scale disaster, return home or evacuate according to the instructions
from the headquarter.
(1) R e-entering buildings
If you need to re-enter the building, e.g., in order to get personal belongings, you must
follow the instruction of headquarters. Re-entrance is limited to offices with minimum
damage, and entering places, where there is a chance of a secondary disaster, such as
laboratories, is prohibited. Make sure you have necessary safety equipment, such as a
helmet. Do not stay more than enough to pick up necessary items, do not attempt to
make any restoration of the office.
(2) R eturning hom e
When you leave the institute, make sure that your supervisor is aware that you are
leaving for the day. You will also be requested to fill in the paper provided by the Safety
Confirmation Group, where the destination must be specified. Normal transportation to
home might not be available, thus also consider alternative measures, such as
car-sharing. After leaving, report your situation and other information via email.
(3) Take shelter in the institute w hen it is not safe to go hom e
If returning home is difficult or judged dangerous, make a shelter for the night in the
institute. Evacuation Command Group will organize the shelter for those in need
in safe places, such as an auditorium or conference room. Evacuees must follow the
instruction. They will also be asked to help construct the shelter. Generally, the
makeshift shelter is capable of accommodating them for one night and two days only.
After that period, the evacuees will be advised to return home or move to a public shelter.
Follow the aforementioned instructions when returning home.
8.5 Investigation of the dam age and restoration activities
Investigation of the damaged facilities and the restoration must be carried out as a group
under the instruction of the headquarter.
(1) Initial inspection
The entry to each building is controlled by the headquarter, and must be authorized. That is,
the entrance is limited to a single designated gate, e.g., the front entrance to Building #2, the
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IMR, Tohoku University
entry will be approved for a group with more than three people, etc. The authorized groups
must carry the hazard map of the building, examine in a concerted manner, especially for
the places where there is a potential danger from chemicals, gases, etc. Their mission
include reporting the details of the damage and danger, and filling in the Initial Damage
Report Form. Take photographs during the inspection and note any items that require an
urgent action. Do not undertake individual restoration measures until the entire scope of
the damage is assessed.
(2) A ssessm ent of the overall situation
Reports from individual inspection groups must be given to the headquarter. It is one of
the missions of the headquarter to make the list of hazardous locations in the buildings,
close off rooms with potential danger where necessary, and plan and organize further
actions.
(3) R estoration
Carry out restoration work for individual laboratories once safety is confirmed by the
headquarter. Permission is required. Always act as a group with conceivable dangers in
mind, e.g., aftershocks. Utilities, such as water, electricity, and gases, will be
re-functioned only under the surveillance of the headquarter.
(4) R estoration w ork w hen dam age is light
If the headquarter has judged that the damage is light, start restoration work following
specified instructions. Act as a group, take photographs and notes on the damage
situation. Whenever it is felt not safe, leave the room immediately and report to the
headquarter. Close the room and post an "No Entry" sign on the doors of such a room.
8.6 Em ergency care m anual
For information on emergency care, refer to other resources such as the Sendai Rescue
Navigator and study methods in advance.
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Chapter 9 Accident compensation: Insurance
9.1Personal accident insurance for students
Even if you are being careful in preventing accidents during everyday laboratory activities,
unexpected accidents do happen. The Personal Accident Insurance for Students Pursuing
Education and Research (Gakusei Kyouiku Kenkyu Saigai Shougai Hoken) is a nationwide
insurance designed to cover accidents that occur during school activities. This applies to all
students (including international students) studying in universities and junior colleges in
Japan.
9.1.1
Accidents covered by insurance
Students are insured for physical injuries and/or damage in the following cases:
(1) During classes: accidents that occur during lectures, experiments, laboratory training and
related activities.
(2) During school events: accidents that occur during entrance ceremonies, orientation,
graduation ceremonies, and other school sponsored events.
(3) Inside the school facilities: accidents that occur whilst inside the facilities owned by the
school for educational purposes.
(4) During official field activities outside the school facilities: accidents that occur during
cultural activities or sports events under the control of an internal University student group,
which should be authorized by the university.
(5) While commuting: while commuting between a residence and school facilities.
(6) Transit between school facilities: accidents during transit between school facilities and
whilst
moving
between
places
to
attend
classes
off-campus,
school
events
and
extra-curricular activities.
Cases not eligible for insurance compensation
Insurance does not cover injuries/damage resulting from the following: fighting, crime, illness,
earthquake, volcanic eruption, tsunami, riots, radiation exposure, driving without a license
or under the influence of alcohol, and dangerous, extra-curricular sporting activities outside
of the schools facilities. Accidents that are not considered to have occurred suddenly,
haphazardly or caused by extrinsic reasons, such as acute alcoholism, are not covered by the
insurance either.
9.1.2
Exam ples of incidents covered by insurance
(1) During classes
- During a chemical experiment, a flask exploded and pieces of glass got into the students
right eye (200,000 yen paid by insurance).
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IMR, Tohoku University
- During a gym class, a student damaged a joint ligament in his left leg after taking off for a
long jump and sustained a partial fracture (insurance payout 320,000 yen).
- During a geological field study, a student fell off a 20 m high, rocky cliff. He cracked his
skull and died (20,000,000 yen).
(2) During school events
- Whilst cooking at a food stand during a school festival, a kettle on the stovetop fell and
burned a student's leg (242,000 yen).
(3) Inside school facilities
- A student fell down the stairs and damaged a ligament in his right leg during a break
(30,000 yen).
- During soccer team practice, a student collided with the goalkeeper and ruptured his spleen.
He required a splenectomy (5,100,000 yen).
(4) During official field activities outside of the school facilities
- Whilst on a ski camp, a student fell and broke his left wrist (insurance payout 50,000 yen).
- During a game of rugby at the opponent team's stadium, a student was paralyzed after
injuries sustained in a tackle (15,000,000 yen).
9.1.3
W ho should be insured ?
All students pursuing education and research in Tohoku University are required to join the
personal accident insurance plan, provided by the university. This is not an option but a must.
It is his/her responsibility to make sure he/she is covered by the plan, especially after an
leave of absence. It is also necessary to renew the contract when you enter graduate school.
Since any accident that occurs whilst participating in laboratory research or in
extra-curricula activities without insurance may cost the students tremendously, they must
make sure that they are insured. If students are involved in an accident and are not insured,
they face the possibility of having to pay for expensive hospital fees that would otherwise be
covered by insurance. Therefore, students must not study or do research without being
insured.
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9.1.4
Reim bursem ent process for accidents
Accident
↓
- Report to the Student Support Section at the Education and Student Support Department.
-Treatment at the Tohoku University hospital or emergency room (after hours).
↓
Treatm ent
↓
After treatm ent
- Claim (fill in the necessary insurance document).
- Get the required proof and fill in the insurance claim form.
- Doctor's certificate (or treatment status report).
↓
Processed by the insurance com pany
↓
Reim bursem ent (paym ent by the plan)
9.2 Staff m em ber accident com pensation
Accident compensation for faculty members is regulated by the Tohoku University
Employment Regulations. The employment regulations can be found on the Head Office
Organization HR website, on the University website.
Tohoku University Staff Member Extralegal Accident Compensation Regulations.
http://www.bureau.tohoku.ac.jp/kitei/reiki_honbun/au10104361.html
9.3 Facility Liability Insurance
If students suffer injury, light or lethal, during educational research or extracurricular
activities under the instruction of a faculty member or if a damage occurs to property such as
research equipment or buildings and the faculty member becomes liable for damages, the
"Facility Liability Insurance" system compensates for such damages, which the faculty
member is liable for, as stipulated by the law.
The IMR, along with the IMRAM/IDAC/IFS/RIEC/Center for Northeast Asian Studies,
participates in an insurance program that provides reimbursement up to three hundred
million yen per person and one billion yen per accident (a deducible of 1,000 yen per
accident).
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