Operational Safety Procedure

For Bruker DAVINCI

Location : room 2407

Emergency Response

In case of emergency

a) cease all operations that will put you at risk to exposure

b) de-energize instrumentation
c) call radiation safety 862-1111
d) contact : Joe Reibenspies 693-2175
N Bhuvanesh 690-8752
R. Carter : 693-4767
e) close enclosure doors, post warning signs and walk away.
f) in case of severe injury call 9-911 and seek medical help

Rev 1.0.0 1/12/2018

X-ray Diffraction Laboratory 1/12/2018
The operation and safety procedures outlined in this manual are to ensure compliance
with the rules and regulations of Texas A & M University and to provide information
concerning radiation safety. It is assumed that the users of this facility have attended
the required University Training and are familiar with general radiation safety issues.

Radiation Sources in the X-ray Diffraction Laboratory

There are presently nine (8) x-ray diffraction instruments located in rooms 2407 and
2409. These instruments produce 6KeV x-rays.

As Low As Reasonably Acceptable (ALARA)

The instrumentation in the X-ray Diffraction Laboratory is equipped with safety

interlocks in order to eliminate accidental exposure.

The goal of this facility is that one should receive zero radiation exposure during
routine operation and alignment of the instrumentation. To achieve this goal the
Laboratory will

• Periodically monitor radiation levels.

• Provide sufficient shielding and distance separation.
• Maintain adequate radiation safety records
• Provide in-depth training
• Provide laboratory security and limit access
Normal Operating Procedure

1.1 All radiation producing devices are equipped with safety interlocks in
order to minimize accidental radiation exposure.
1.2 All panels and doors must be in place and secured before operation of
the instrumentation.
1.3 Visual inspection of the X-ray tube housing, collimator, water tubes and
high voltage cables are required before operation of the instrument.
a) if any part has been displaced or damaged then close enclosure de-
energized instrumentation and seek help
1.4 Visual inspection of the X-ray generator is required before operation of
the instrument.
a) if abnormal situation is seen then close enclosure de-energized
instrument and seek help.
1.5 Start the “Defract.Measurement” program.
1.6 Close the enclosure doors and test the shutter operation
- a distinct click noise will be heard and the shutter LEDs will
change from green to red.
- If abnormal operation is seen then de-energize x-rays and seek
help
1.7 Be sure shutter is closed before opening the enclosure doors.
1.8 Visually inspect the enclosure safety switches.
- shutter will not open with doors open
1.9 Use survey equipment to test for stray radiation.
- if excessive radiation is detected then cease activity, close
enclosure, de-energize x-rays and seek help.
1.10 With the “Defract.Measurement” program initialize drives.
- visually inspect angles, if not a zero seek help.
1.11 Ensure the shutter is closed and mount the sample in the holder
- keep your hands well below the primary beam area.
1.12 Visually check the detector position and generator settings
1.13 Close enclosure door
1.14 Enter information in the operational log book.
- Enter the date, your name, your advisors name
- Enter your project name and title.
- Enter any unusual event or circumstance
- Enter detector distance, generator settings

2.0 Operation during data collection

2.1 do not open enclosure doors during data collection
2.2 do not remove any instrument panels during operation
2.3 avoid movement in or around the instrument during data collection
Shutter/Enclosure Safety features.

There is one X-ray shutter on the DAVINCI system. The safety shutter that is behind
the first slit apparatus attached to the x-ray tube (left hand side).

Normal operation :

• AMBER LED on light on the tube will be lit when X-rays are on.
• When the Safety shutter opens (loud click sound) and the red LED light will be
seen on the tube housing.

Front/side/rear panels.

Normal operation :
• Yellow light (radiation symbol) on front left panel will be on for normal
operation.
• The solid green light will be on below the yellow light .
• The green light with door symbol will be on when door is open
• A solid Red Light and/or white light in either position indicates fault.
• Safety shutter will not open if the yellow or green lights are not lit.

Power Connection and Disconnection

Depressing the RED button located on the wall next to the exit doors will disconnect the
power to all diffractometers. This switch should be used in case of emergencies.

Depressing the RED button on the left-hand or right-hand panel of the diffractometer will
disconnect the power to an individual unit.

Radiation Hazard and Work Areas

An area of 4.5 meters (15ft.) extending in all directions from the X-ray diffractometer is
designated as a HAZORDOUS OCCUPATION AREA. This area should only be
occupied for short durations and only for the purpose of starting and ending an
experiment.

Energizing X-rays
1) All panels on the diffractometer must be in place and closed. All safety lights must
be green.
2) Red safety button on generator panel (lower left) must be pulled out.
3) Depress the to switch on generator panel left button.
4) X-ray will come on and ramp to KV 20 MA 5.
5) Use program to ramp generator to KV 40 MA 25.
De-energizing X-rays

1) Depress yellow switch on left-hand panel.

2) Wait for yellow Light to change to green .

3.0 Radiation Safety Information

Radiation Units

a) Roentgen (R) : amount of radiation that produces one unit of ions/cm3.

(measure of X-rays) 1mR/hr is considered a low rate. 100mR/hr is considered
high.

b) Radiation Absorbed Dose (rad) [SI unit : gray (Gy) where 1Gy = 100 rad]:
Energy imparted to matter in volume (V) divided by the mass. 1 rad = 100
ergs/gram (measure of any radiation) 100 rad/sec = 1 Watt/kg

c) Radiation Equivalent Dose (rem) [SI unit sievert (Sv) where 1Sv=100 rem]:
Product of the absorbed dose and the relative biological effect (RBE) necessary
to express on a common scale. rad x (RBE) = rem for X-rays the RBE = 1.0
and for neutrons = 10.0 (measure of radiation effect on humans)

for X-rays :

I rad = 1 rem 1R
3.6 x 105 R/hr 1 Watt/kg

d) Maximum Permissible Dose:

(https://www.osha.gov/SLTC/radiationionizing/introtoionizing/ionizingattachmentsix.ht
ml)

Whole body 5rems/yr. (elbows up; knees up) 2.5mR/hr

Long-term (N-18)* 5rems
Skin 15 rems/yr.
Hands 75 rems/yr.
Forearms 30 rems/yr.
non-occupational 0.17 rem/yr.
minors 0.17 rem/yr 0.01 mR/hr
pregnant (declared) 0. 5 rem/9-month (must be declared in writing)
 e) Background Radiation

Highest (world) 5 rem/yr. Kerala, India

Highest (U. S.A) 0.2 rem/yr Leadville,
Colorado
Average(world) 0.09 rem/yr
Lowest(U.S.A) 0.07 rem/yr Atlantic/Gulf
coast
X-ray Source.

Primary Beam Dosimetry

Radiation Level
Inverse Rate Law
R/hr = 2432 * [(kV * mA)/cm2 ] * Z atomic number of the target
X-rays - 'Soft' radiation - easily attenuated but never attenuated to zero.
1/d2 decrease (standard temperature and pressure)

X-ray diffraction -

monochromatic - reduces the radiation level (~105)

Filtered - reduces the radiation level (~101)
collimated beams directional
separate user from the source
reduce the primary radiation area

Leakage Dosimetry

Normally very low for X-ray Diffractometers unless collimator and/or

monochromator misaligned. (labyrinth design, well fitting joints)

Almost negligible leakage from tube housing.

Stray X-ray beam directions tend to be at large angles away from the direction
of the primary beam.

Adventitious Radiation.

High voltage rectifiers. (an X-ray tube is a rectifier)

Radiation Safety
 Radiation Measurement

Personal Dosimetry

(not employed at this location)

a) types
-LiF Thremoluminescent dosimetry TLD Pocket and extremity badges. (lowest
detectable dose 2-3 mrad ; highest 105 rad) -Film badge
-Pocket ion chamber (pencil dosimeters; show immediate response)

- usage
-badges should be worn in such a way as to maximize the possibility of
exposure in case of accident. (line of sight)

- advantages
usually first sign that something has gone wrong. extremity dosimetry is the
most useful legal aspects

- disadvantages
-directionality of the primary beam and scattered radiation. monitoring devices
must sustain a direct hit a 1/ 10000 chance for pocket and 1 /100 chance for
extremity badges -nuisance (if too troublesome it won't be used) -expensive

- dosimetry exclusions
-workers who are likely not to exceed the max. yearly limits. -dosimeters will
be distributed on a rotating basis.

Accidental Exposure

Rate

1 accident per 100 machines per year in 1968 and

1 accident per 200 machines per year in 1974.

for 10 X-ray diffractometers 1 accident every 10 years. 75% of those accident

are with XRD instruments. Relative User Risk (increasing risk)
- routine users are the safest (lowest risk)
- advanced users (a little knowledge is dangerous)
- managers and service personal (highest risk)
Exposure of Radiation to Flesh (localized) : Symptoms (103 rad)

-fingers, arms, eyes etc.(finger/hand exposure is the highest risk) -depth of

exposure of 10-20 keV X-rays 1.3-4.3 mm (tl/2) -non-stochastic (skin reaction)

0-1 hr. tingling

1-7 days swelling, blistering, pain, erythema,
hair loss (epilation), skin loss (desquamation)
7-30 days ulcers (sores that will not heal), gangrene
30-300 days loss of digits.
300+ days: cataracts, skin grafts

As dose increases the time for symptoms to appear decreases

Other doses
500-1000 rad erythema and epilation
300-500 rad mild erythema, some epilation
300 rad lowest visible detection of skin damage
1-300 rad no visible skin damage
0.1-1 rad significant dose (over-exposure)

As beam area decreases the dose required to produce skin damage increases.

stochastic (radiation-induced mutation : cell damage : cancer)

- No known threshold dose!
- risk is roughly proportional to the dose2
- >100 rad is considered significant
- >3000 rad cause cell sterilization - highest risk is between 2500-3000 rad
- known case for exposure above 2000 rad
- most cancers take more than 1O years to manifest symptoms
- for workers exposed to 100rem/life show only a statistical decrease in life
expectancy of 1%. (70 days for 70 years life expectancy)
- statistically one day of life loss for each rem of exposure.
- exposure is accumulative (rem/life)

Accident Detection

- X-rays are invisible (no sight, sound or taste)

- X-rays do not generate heat in tissue. (no touch)
400 rad will raise the skin temperature by only 0. 001o C
- X-rays do not produce detectable amounts Of 03, NO etc. (no smell).
- Personal Dosimetry
- Biological/Health Effect
 Bibliography

"Procedures Manual for Use of Radioisotopes and Radiation Producing Devices",

Office of Radiological Safety, Texas A & M University

"A Guide to the Safe Use of X-ray Diffraction and Spectrometry Equipment", Martin,
E., Science Reviews Ltd., Ash Drive, Leeds, LS 17 8RA U.K.

"A Case History of Severe Radiation Bums from 50 kVC X-rays", Steidley, K.,
Stabile, R. & Santillippo, L. Health Physics (1981). 40 399-405.

"Analytical X-ray Hazards: A Continuing Problem" Lubenau, J., Davis, J., McDonald,
D. & Gerusky, T. Health Physics (1969). 16, 739-746.

"Occupational Hazards in X-ray Analytical Work" Lindel, B. Health Physics (1968).

15, 481-486.

"Incidence, Detection and Monitoring of Radiation from X-ray Analytical

Instrumentation" Jenkins, R. & Haas, D. X-ray Spectrom (1975). 4, 33-39.

"Protection Against Radiation Injury" Cook, J. & Oosterkamp, W. Intemational Tables

for Crystallography (1962). 333 -338.

"Characteristic X-ray Flux from Sealed Cr, Cu, Mo, Ag, W Tubes" Honkimski, V.,
Sleight, J. & Suortti, P. J Appl. Cryst. (1990). 23, 412-417.