Determining Vacuum Chamber Gaseous Environment Using A Cold Finger
Determining Vacuum Chamber Gaseous Environment Using A Cold Finger
Determining Vacuum Chamber Gaseous Environment Using A Cold Finger
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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4.6 Both the pretest and posttest samples are placed in
previously cleaned and weighed evaporating dishes. The dishes
containing the samples are placed on a steam bath and the
solvent is evaporated. The dishes containing the residue are
then weighed using an analytical balance. The samples of the
solvent are similarly handled and any residue weighed. The
differences of mass between the pretest residue and posttest
residue is then determined (corrected if necessary for any
significant residue found in the solvent); this difference in mass
is taken as the residue collected by the cold finger during its
exposure to the vacuum environment, CFR.
4.7 Analytical procedures such as infrared spectroscopy or
gas chromatography-mass spectrometry may be used to iden-
tify those species that constitute the residue.
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extended to form a lip or trap annulus approximately 10 mm 9.2.1 Pour approximately 100 mL of solvent over the cold
high with a diameter of 75 mm so that fluid poured over the top finger. (Do not splash alcohol on the chamber shroud.) Pour at
of the cylinder and running down the sides can be captured. A such a rate that the trap annulus is filled to overflowing. Catch
small drain is provided in this lip and the fluid can drain this fluid in a basin or similar container and discard it.
through this aperture into a receptacle. Two tubes enter the cold 9.2.2 Pour 50 mL of the solvent over the cold finger. Do not
finger through the base, one providing the inlet and the other overflow the trap annulus. Catch the solvent directly with a
the outlet for the coolant. Temperatures shall be monitored. The clean sample bottle. Label this bottle Pretest Sample.
coolant recommended in this practice is liquid nitrogen. The 9.2.3 Pour 50 mL of solvent (Note 2) into a clean sample
apparatus should be thoroughly cleaned after the manufacture. bottle directly from the same container used to pour it over the
6.2 Containers must not react with the solvents. Glass, cold finger. Label this bottle Pretest Stock.
austenitic stainless steels, or PTFE generally are acceptable. NOTE 2—If experience indicates the solvent to yield consistently less
than 0.2 mg of residue, the steps indicated in 9.2.3 and 9.4.2 need be done
7. Reagents only when a new container of solvent is used.
7.1 Spectroscopic grade isopropanol is isopropyl alcohol 9.3 Chamber Operations:
having a gas chromatograph (GC) purity level of at least 9.3.1 If any protective cover has been placed over the cold
99.9 % and <1 ppm residue after evaporation. It is the solvent finger, it should be removed immediately before the chamber
used for obtaining the sample from the cold finger and as the door is closed.
final rinse material in the cleaning procedures for the various 9.3.2 Coolant should be admitted to the cold finger when the
equipment that will come in contact with the sample during the chamber pressure decreases below 1 mPa (8 × 10−6 torr), and
execution of this practice. flow should be continued to maintain the cold finger at a stable
temperature until the chamber return to atmosphere is under-
8. Precautions way. The temperature of the cold finger should be monitored.
8.1 Equipment other than the cold finger that will come in 9.3.3 The coolant flow should be terminated when the
contact with samples should be cleaned in accordance with the chamber pressure rises above 80 kPa (600 torr) during the
annex to this practice. return to room ambient conditions using gaseous nitrogen. The
temperature of the cold finger should be kept above the dew
8.2 The cold finger should never be touched with bare hands point of water in the ambience during the return to atmosphere
after cleaning. and after the chamber door is opened.
9. Procedure 9.4 Taking the Posttest Cold Finger Sample:
9.4.1 As soon as possible after the chamber is open, pour 50
9.1 Cleaning the Cold Finger—The cold finger should be
mL of solvent over the cold finger. Catch the solvent directly
thoroughly cleaned when installed and after each test to ensure
with a clean sample bottle. Label this bottle Posttest Sample.
that contamination is not carried from test to test. The cleaning
9.4.2 Pour 50 mL of solvent (Note 2) from the same
procedure should be as follows:
container directly into a clean sample bottle. Label this bottle
9.1.1 Heat the cold finger with an electric torch or flexible
Posttest Stock. (This step may be omitted if the solvent is taken
heater to approximately 60°C.
from the same container as that in 9.3.2.)
9.1.2 Scrub the cold finger with a solution of laboratory
detergent3 and hot distilled water using an extracted, lint-free 9.5 Evaporating and Weighing—This section applies to
wiping pad. It should be cleaned on all surfaces, plus approxi- pretest and posttest cold finger and stock samples.
mately 50 mm of the coolant lines where they enter the cold 9.5.1 Weigh a cleaned porcelain evaporating dish (about 75
finger. mm in diameter) using an analytical balance having accuracy
9.1.3 Rinse the cold finger with hot, clean, distilled water. and a precision of at least 0.1 mg.
Particular attention should be given to the corners of the 9.5.2 Place the entire sample in the evaporating dish.
annulus and its drain hole as well as the welding relief groove 9.5.3 Place the evaporating dish containing the sample in a
on the top. steam bath and heat the dish until the solvent has been
9.1.4 Flood rinse all washed surfaces with solvent. The evaporated.
electric torch may be used to assist the drying action. 9.5.4 Weigh the evaporating dish containing any residue
9.1.5 Discard all used wash and rinse fluids. from the sample using a balance as in 9.5.1.
9.1.6 Cover the cold finger with a piece of cleaned alumi- 9.5.5 Warning—The evaporating dish should not be
num foil or lint-free cloth if the wash sample is not to be taken handled with bare hands so that skin oils or other contaminants
at once. are not transferred to the dish.
9.2 Taking the Pretest Cold Finger Sample: 9.5.6 Warning—Weighing should be done after the evapo-
rating dishes have reached room temperature.
9.6 Other Analysis—The residue that remains in the evapo-
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The sole source of supply of the laboratory detergent known to the committee rating dish may be subjected to chemical analysis such as
at this time is Alconox, 30 Glenn St., Suite 309, White Plains, NY 10603. If you are
infrared spectroscopy or gas chromatography-mass spectrom-
aware of alternative suppliers, please provide this information to ASTM Interna-
tional Headquarters. Your comments will receive careful consideration at a meeting etry so as to identify those species that constitute it; a relative
of the responsible technical committee,1 which you may attend. quantitazation among species is often helpful.
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10. Calculation 11.1.5 The dates and times over which the sample was
10.1 Calculate CFR as follows: obtained and the total number of hours the cold finger was
10.1.1 Determine the mass of the residue in stock samples being cooled.
by subtracting the mass of the empty evaporating dish from the 11.1.6 The temperature of the cold finger during the vacuum
mass of the evaporating dish after the stock sample has been exposure; the measurement technique and estimated accuracy.
evaporated. Designate the pretest stock residue as Si and the 11.1.7 The masses of the stock sample residues, Si and Sf
posttest residue as Sf, both expressed in milligrams. If either Si expressed in milligrams; if both Si and Sf are equal or less than
or Sf are found to be greater than 0.2 mg for a 50-mL sample, 0.2 mg, this should be noted and specific masses need not be
their effect should be considered; if not, they may be neglected provided.
from the calculations. 11.1.8 The masses of the cold-finger sample residues, Mi
10.1.2 Determine the mass of the residue in the cold finger and Mf, expressed in milligrams.
sample by subtracting the mass of the empty evaporating dish 11.1.9 The mass of the residue collected during the vacuum
from the mass of the dish after the cold finger sample has been exposure, CFR.
evaporated. Designate the pretest cold finger sample residue as 11.1.10 The results of any chemical analysis that may have
Mi and the posttest cold finger sample residue as Mf, both been conducted to characterize the residue further. The ana-
expressed in milligrams. lytical technique and the particular instrument used should be
10.1.3 The mass of the residue collected by the cold finger identified.
during its exposure to vacuum and remaining after processing 11.1.11 Any other pertinent information that the supplier
to this part, CFR, is expressed in milligrams: considers relevant.
CFR 5 ~ M f 2 S f ! 2 ~ M i 2 S i ! (1) 12. Precision and Bias
11. Report 12.1 Neither the precision nor the bias for this practice has
11.1 The report of the results of the cold finger procedure been determined.
should contain the following information: 12.2 The 50-mL samples should have a precision of 62 mL.
11.1.1 The name of the organization conducting the proce- 12.3 Weighings should be made to the nearest 0.1 mg.
dure.
11.1.2 The date of the weighing. 12.4 Results should be expressed to the nearest 1 mg.
11.1.3 The designation and short description of the facility
in which the cold finger sample was obtained. 13. Keywords
11.1.4 A short description of the purpose of the vacuum 13.1 cold finger; contamination monitoring; residual gas
exposure; one sentence will generally suffice. compositions; vacuum chamber
ANNEX
(Mandatory Information)
A1. CLEANING
A1.1 Equipment Required A1.2.3 Soak the aluminum dishes for a minimum of 1 h.
A1.1.1 Air furnace capable of achieving 550°C. Soak the glass and porcelain items for at least 2 h.
A1.1.2 Cotton gloves. A1.2.4 Allow the items to cool in the oven until less than
35°C.
A1.1.3 Plastic gloves (not vinyl or extractable plasticized
type). A1.2.5 Remove the weighing dishes from the furnace and
place them in aluminum foil until ready for use.
A1.2 Procedure
A1.2.6 Remove the bottles and stoppers from the furnace.
A1.2.1 Place transfer bottles, stoppers, porcelain weighing Insert a stopper into the bottle mouth and seal with a strip of
dishes, and aluminum weighing dishes in the furnace. clear tape over the stopper, making sure that the tape adhesive
A1.2.2 Heat the furnace to 550°C. does not adhere to the lip of the bottle.
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