ASTM E595_06 Standard Test Method for Total Mass Loss and Collected Volatile Condensable Materials f
Designation:E595–06
Standard Test Method for
Total Mass Loss and Collected Volatile Condensable Materials from Outgassing in a Vacuum Environment1
This standard is issued under the?xed designation E595;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.A superscript epsilon(e)indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1.Scope
1.1This test method covers a screening technique to deter-mine volatile content of materials when exposed to a vacuum environment.Two parameters are measured:total mass loss (TML)and collected volatile condensable materials(CVCM). An additional parameter,the amount of water vapor regained (WVR),can also be obtained after completion of exposures and measurements required for TML and CVCM.
1.2This test method describes the test apparatus and related operating procedures for evaluating the mass loss of materials being subjected to125°C at less than7310?3Pa(5310?5 torr)for24h.The overall mass loss can be classi?ed into noncondensables and condensables.The latter are character-ized herein as being capable of condensing on a collector at a temperature of25°C.
N OTE1—Unless otherwise noted,the tolerance on25and125°C is 61°C and on23°C is62°C.The tolerance on relative humidity is65%.
1.3Many types of organic,polymeric,and inorganic mate-rials can be tested.These include polymer potting compounds, foams,elastomers,?lms,tapes,insulations,shrink tubings, adhesives,coatings,fabrics,tie cords,and lubricants.The materials may be tested in the“as-received”condition or prepared for test by various curing speci?cations.
1.4This test method is primarily a screening technique for materials and is not necessarily valid for computing actual contamination on a system or component because of differ-ences in con?guration,temperatures,and material processing.
1.5The criteria used for the acceptance and rejection of materials shall be determined by the user and based upon speci?c component and system requirements.Historically, TML of1.00%and CVCM of0.10%have been used as screening levels for rejection of spacecraft materials.
1.6The use of materials that are deemed acceptable in accordance with this test method does not ensure that the system or component will remain uncontaminated.Therefore,subsequent functional,developmental,and quali?cation tests should be used,as necessary,to ensure that the material’s performance is satisfactory.
1.7This standard does not purport to address all of the safety concerns associated with its use.It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
2.Referenced Documents
2.1ASTM Standards:2
E177Practice for Use of the Terms Precision and Bias in ASTM Test Methods
2.2ASTM Adjuncts:
Micro VCM Detailed Drawings3
3.Terminology
3.1De?nitions:
3.1.1collected volatile condensable material,CVCM—the quantity of outgassed matter from a test specimen that con-denses on a collector maintained at a speci?c constant tem-perature for a speci?ed time.CVCM is expressed as a percentage of the initial specimen mass and is calculated from the condensate mass determined from the difference in mass of the collector plate before and after the test.
3.1.2total mass loss,TML—total mass of material out-gassed from a specimen that is maintained at a speci?ed constant temperature and operating pressure for a speci?ed time.TML is calculated from the mass of the specimen as measured before and after the test and is expressed as a percentage of the initial specimen mass.
3.1.3water vapor regained,WVR—the mass of the water vapor regained by the specimen after the optional recondition-ing step.WVR is calculated from the differences in the specimen mass determined after the test for TML and CVCM
1This test method is under the jurisdiction of ASTM Committee E21on Space Simulation and Applications of Space Technology and is the direct responsibility of Subcommittee E21.05on Contamination.
Current edition approved Nov.1,2006.Published December2006.Originally approved https://www.wendangku.net/doc/3012479230.html,st previous edition approved in2003as E595–93(2003)e2.
2For referenced ASTM standards,visit the ASTM website,https://www.wendangku.net/doc/3012479230.html,,or contact ASTM Customer Service at service@https://www.wendangku.net/doc/3012479230.html,.For Annual Book of ASTM Standards volume information,refer to the standard’s Document Summary page on the ASTM website.
3Available from ASTM International,100Barr Harbor Dr.,PO Box C700,West Conshohocken,PA19428–2959.Order Adjunct ADJE0595.
Copyright?ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959,United States.
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and again after exposure to a50%relative humidity atmo-sphere at23°C for24h.WVR is expressed as a percentage of the initial specimen mass.
4.Summary of Test Method
4.1This microvolatile condensable system4was developed from an earlier system for determination of macrovolatile condensables that required much larger samples and a longer test.
4.2The test specimen is exposed to23°C and50%relative humidity for24h in a preformed,degreased container(boat) that has been weighed.After this exposure,the boat and specimen are weighed and put in one of the specimen com-partments in a copper heating bar that is part of the test apparatus.The copper heating bar can accommodate a number of specimens for simultaneous testing.The vacuum chamber in which the heating bar and other parts of the test apparatus are placed is then sealed and evacuated to a vacuum of at least 7310?3Pa(5310?5torr).The heating bar is used to raise the specimen compartment temperature to125°C.This causes vapor from the heated specimen to stream from the hole in the specimen compartment.A portion of the vapor passes into a collector chamber in which some vapor condenses on a previously-weighed and independently temperature-controlled, chromium-plated collector plate that is maintained at25°C. Each specimen compartment has a corresponding collector chamber that is isolated from the others by a compartmented separator plate to prevent cross contamination.After24h,the test apparatus is cooled and the vacuum chamber is repressur-ized with a dry,inert gas.The specimen and the collector plates are weighed.From these results and the specimen mass determined before the vacuum exposure,the percentage TML and percentage CVCM are obtained.Normally,the reported values are an average of the percentages obtained from three samples of the same material.
N OTE2—It is also possible to conduct infrared and other analytical tests on the condensates in conjunction with mass-loss tests.Sodium chloride ?ats may be used for infrared analysis.These?ats are nominally24mm (1in.)in diameter by3.2mm(0.125in.)thick and are supported edgewise in a metal holder that?ts into the collector plate receptacle.On completion of the test,the?ats are placed into an infrared salt?at holder for examination by an infrared spectrophotometer.As an alternative method, the condensate may be dissolved from the metallic collector,the solvent evaporated,and the residue deposited on a salt?at for infrared tests. Sodium chloride?ats shall not be used for CVCM determinations.
4.3After the specimen has been weighed to determine the TML,the WVR can be determined,if desired,as follows:the specimen is stored for24h at23°C and50%relative humidity to permit sorption of water vapor.The specimen mass after this exposure is determined.From these results and the specimen mass determined after vacuum exposure,the percentage WVR is obtained.
4.4Two or three empty specimen chambers in the heater bar and collector plates on the cold bar,selected for each test at random,can be used as controls to ensure that uniform cleaning procedures have been followed after each test.
4.5A typical test apparatus can have24specimen chambers with24associated collector plates so that a number of specimens of different types can be tested each time the foregoing operations are conducted.Three specimen compart-ments can serve as controls and three can be used for each type of material being tested.The total time required for specimens requiring no prior preparation is approximately4days.The equipment should be calibrated at least once a year by using previously tested materials as test specimens.
4.6The apparatus may be oriented in any direction as long as the con?guration shown in Fig.1is maintained and bulk material does not fall from the sample holder nor obstruct the gas-exit hole.The dimensions for critical components given in Fig.2and Table1are provided so that apparatus constructed for the purpose of this test may provide uniform and compa-rable results.
5.Signi?cance and Use
5.1This test method evaluates,under carefully controlled conditions,the changes in the mass of a test specimen on exposure under vacuum to a temperature of125°C and the mass of those products that leave the specimen and condense on a collector at a temperature of25°C.
5.2Comparisons of material outgassing properties are valid at125°C sample temperature and25°C collector temperature only.Samples tested at other temperatures may be compared only with other materials which were tested at that same temperature.
5.3The measurements of the collected volatile condensable material are also comparable and valid only for similar collector geometry and surfaces at25°C.Samples have been tested at sample temperatures from50to400°C and at collector temperatures from1to30°C by this test technique.Data taken at nonstandard conditions must be clearly identi?ed and should not be compared with samples tested at125°C sample tem-perature and25°C collector temperature.
4Muraca,R.F.,and Whittick,J.S.,“Polymers for Spacecraft Applications.”SRI Project ASD-5046,NASA CR-89557,N67-40270,Stanford Research Institute, September
1967.
FIG.1Schematic of Critical Portion of Test Apparatus(Section
A-A of Fig.2
)
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5.4The simulation of the vacuum of space in this test method does not require that the pressure be as low as that encountered in interplanetary ?ight (for example,10?12Pa
(10?14torr)).It is sufficient that the pressure be low enough that the mean free path of gas molecules be long in comparison to chamber
dimensions.
FIG.2Critical Portion of Test Apparatus (See Table 1for
Dimensions)
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5.5This method of screening materials is considered a conservative one.It is possible that a few materials will have acceptable properties at the intended use temperature but will be eliminated because their properties are not satisfactory at the test temperature of125°C.Also,materials that condense only below25°C are not detected.The user may designate addi-tional tests to qualify materials for a speci?c application. 5.6The determinations of TML and WVR are affected by the capacity of the material to gain or lose water vapor. Therefore,the weighings must be accomplished under con-trolled conditions of23°C and50%relative humidity.
5.7Alternatively,all specimens may be put into open glass vials during the24-h temperature and humidity conditioning. The vials must be capped before removal from the conditioning chamber.Each specimen must be weighed within2min after opening the vial to minimize the loss or absorption of water vapor while exposed to an uncontrolled humidity environment. While control of humidity is not necessary at this point,the temperature for the weighing should be controlled at23°C,the same temperature prescribed for the24-h storage test.
6.Apparatus
6.1The apparatus used in the determination of TML and CVCM typically contains two resistance-heated copper bars. Generally,each bar is650mm(25.5in.)in length with a 25-mm(1-in.)square cross section and contains twelve speci-men chambers.The open section of each specimen chamber allows vapors from the specimen to pass through a hole into a collector chamber where it impinges on a removable chromium-plated collector plate maintained at25°C through-out the test.(See Figs.1and2.)Variations in test apparatus con?gurations are acceptable if critical dimensions are main-tained as prescribed in Table1.
6.2Typically,a total of24specimen chambers is used for testing during a24-h vacuum operation;3of the chambers are maintained as controls.The test apparatus can be mounted on the base plate of a vacuum system within a narrow vacuum bell,260mm(101?4in.)in diameter,that rests on a specially adapted feed-through collar,also supported by the base plate.
6.3The operation of the vacuum chamber system and any device for raising the vacuum bell can be automatically controlled.Power to the heating element mounted in the copper bars is generally controlled by variable transformers through temperature controllers.Recorders with an electronic icepoint reference junction feedback may be used to monitor the heater bar temperatures.A heat exchanger using a suitable?uid may be used to maintain the collector plate at25°C during the test.4 6.4It is recommended that the vacuum chamber system include automatic controls to prevent damage in the event of power failure or cooling?uid supply failure when in unat-tended operation.Care must be taken to prevent backstreaming of oil from vacuum or diffusion pumps into the vacuum chamber.
6.5The controller thermocouple should be mechanically attached to the heater bar or ring to prevent the thermocouple from loosening over time.It is essential that the ori?ce of the sample heater and collector plate be aligned and checked regularly.A good test of alignment and stability is to run the same material in every sample chamber.The results should agree within the accuracy of the test per Section11.
7.Test Specimen
7.1Finished products(for example,elastomers,hardware, and structural parts)are cut into small pieces on the order of 1.5-to3.0-mm(1?16-to1?8-in.)cubes to?t into the specimen
TABLE1Test Apparatus Dimensions(See Fig.2)
A Critical dimensions that must be maintained for test results to be comparable.
B Diameters must be concentric to60.1mm(60.005in.)for test results to be comparable.
C Dimensions include plating thickness.Satisfactory surfaces have been produced by making substrate surface?nish,1.6-μm RMS(63-μin.RMS),highly polished, plated with electroless nickel,0.0127mm(0.0005in.)thick,and?nished with electroplated chromium,0.0051mm(0.0002in.)thick.
boat.Boats approximately10by6by12mm(3?8by1?4by1?2 in.)have been found satisfactory.
7.2Products that require compounding are normally mixed in10-g batches to ensure representative samples.Materials shall be cured as sheets,thin slabs,or thicker sections to simulate application in actual use;then they shall be sectioned in accordance with the foregoing dimensions for specimen cubes.
7.3Adhesive tapes shall be applied to a surface,such as a preweighed aluminum ring or foil,to simulate actual use. Paints can be applied to aluminum foil by brushing,dipping,or spraying to approximate the as-used thickness,then cured before testing.A paint can also be cured on an inert surface such as TFE-?uorocarbon,removed as a?lm,and treated as bulk material.Some adhesives or sealants may be applied to preweighed aluminum foil and cured.
7.4Greases shall be placed into a boat.Liquids shall be placed directly in a boat or absorbed in an ignited neutral?ller such as silica and then placed in a boat.The technique used shall be stated in the report.Liquids and greases,especially silicones,are prone to creep;if the material exhibits creep to such an extent that some?ows out of the boat,the test results shall be disregarded.
7.5Minimum specimen masses on the order of200mg are required.If smaller quantities are used,the accuracy of the measurements may be impaired.
7.6It is absolutely essential that specimen materials not be contaminated at any step in the specimen fabrication process. Most importantly,specimen material shall not be handled with the bare hands as oils from human skin are volatile and condensable and thus will cause false TML and CVCM results.
7.7The following specimen handling procedures are rec-ommended to control contamination:
7.7.1Wear suitable gloves or?nger cots during all specimen preparation steps.
7.7.2All previously prepared materials can be assumed to be contaminated in the“as-received”condition and must be cleaned.
7.7.3Use cleaning solvents that are known to be nonreac-tive with the specimen material and that are known to leave no residue.
7.7.4When possible,discard exterior surfaces of materials when preparing specimens.A clean razor blade can be used to shave off exterior surfaces of rubbers,foams,and other soft materials.Exterior surfaces of harder materials can be removed with a clean jewelers’saw.A clean jewelers’drill can be used to remove specimen material from the center part of material suspected of being contaminated.
8.Procedure
8.1Weigh a prepared aluminum foil boat and return it to its storage beaker in a glass desiccator using silica gel desiccant.
8.2Weigh a prepared collector and mount it into its cooling-plate receptacle.
8.3Add the test specimen(100to300mg)to the boat and condition the sample at50%relative humidity and23°C for a minimum of24h.
8.4Weigh the conditioned specimen(see 4.6)using a balance having61-μg sensitivity.
8.5Place the specimen and boat into a specimen compart-ment of the heating bar in the microvolatile condensable system.4
N OTE3—Before the operation noted in8.5,the copper compartment bar,separator,and cooling plate shall be clean,in position,and awaiting the specimen boats and collector plates.
8.6Mount and screw down the respective cover plates onto the entry end of each specimen compartment.
8.7Close the vacuum system and evacuate it to7310?3Pa (5310?5torr)or less within1h,using proper operating procedures.
8.8Control of the collector plate temperature at25°C(or other temperature if a nonstandard test is being conducted) shall be achieved within the?rst hour of pump-down.
8.9When a pressure of7310?3Pa(5310?5torr)is reached,turn on the heater bar and adjust the variable trans-formers to raise the heater bar temperature to125°C(or other nonstandard test temperature)within60min.If the sample temperature will exceed150°C,up to2h may be required to reach temperature.Temperature controllers should maintain bar temperatures at125°C(or other desired temperature). 8.10Maintain the collector plate temperatures at25°C(or other nonstandard temperature).
8.11Maintain the heater bar temperature at125°C(or other nonstandard temperature)for24h,then close the high vacuum valve to the pumping system and turn off the heater bar current.
8.12Open the vent valve and back?ll with clean,dry nitrogen regulated within a gage pressure range from10to30 kPa(2to4psi)above atmosphere to cool the bars rapidly.
8.13Allow the heater bar to cool sufficiently to permit handling(nominally2h to reach50°C).Then turn off the collector-plate heat exchangers,return the vacuum chamber to room pressure using the clean,dry nitrogen,and open the chamber.
8.14Store aluminum boats with specimens and respective collector plates in desiccators(using active silica gel desiccant) immediately.After specimens have cooled to approximately room temperature,but no longer than1?2h,remove and weigh each specimen within2min of its removal from the desicca-tors.Control collector plates are used to detect cross contami-nation or poor technique.Mass loss of greater than20μg by a control is usually due to poor preparation and cleaning of the collector plate.Mass gain of greater than50μg is an indication of poor cleaning,poor bakeout of the heater assembly,cross contamination,or poor vacuum technique.Any change of50μg(0.05%of a100-mg control mass)or greater is reason for concern and for a review of or change in techniques.All data acquired during runs when this occurs shall be discarded or retained with a note indicating the discrepancy.
8.15Return the foregoing samples to the relative humidity chamber for24h if the WVR is to be determined.Weigh the conditioned specimens(see5.6).
N OTE4—Annex A1contains recommended cleaning and storage pro-
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9.Calculation
9.1Calculate TML as follows:
Initial Mass,g Final Mass,g Specimen and
boat
S I+B I S F+B I
Boat B I B I
Specimen alone(S I+B I)?
B I=S I (S F+B I)?B I=S F
Difference or mass loss L=S I?S F
L/S I3100=%TML
Specimen on aluminum
foil and boat
S I+Al I+B I S F+Al I+B i
Aluminum foil
and boat
Al I+B I Al I+B I
Specimen alone(S I+Al I+B I)?(S F+Al I+B I)?
(Al I+B I)=S I(Al I+B I)=S F
Difference or
mass loss
L=S I?S F
L/S I3100=%TML
9.1.1A correction may be made using control boats when calculating TML.This correction is recommended but not required unless an excessive mass change occurs as described in8.14.
9.2Calculate CVCM as follows:
S C O
S I
D31005%CVCM(1)
where:
C O=mass of condensables,g=C F?C I;
C I=initial mass of collector plate,g;
C F=?nal mass of collector plate and condensables,g;and S I=initial specimen mass,g.
9.2.1A correction may be made using control collector plates when calculating CVCM.This correction is recom-mended but not required unless an excessive mass change occurs as described in8.14.
C S5C CF2C CI(2) where:
C S=change in mass of control collector plate,g;
C CF=?nal mass of control collector plate,g;and
C CI=initial mass of control collector plate,g.
9.3Calculate WVR as follows:
S F82S F
S I31005%WVR(3) where:
S F8=reconditioned mass of specimen and boat after24h at50%relative humidity,g and
S F=?nal specimen mass,g.
9.4Calibrate the balance periodically(at least every six months)and apply the appropriate calibration factors.
10.Report
10.1Report the following information:
10.1.1Trade name and number of the material,the manu-facturer,the batch or lot number,or other such identi?cation, 10.1.2Summary of the preparation schedule(mixing pro-portions,cure time and temperature,post-cure,cleaning pro-cedures),date prepared,
10.1.3Number of samples(nominally three for each mate-rial,but many organizations use only two samples per test), 10.1.4Samples con?guration(size,shape,and so forth). Statement of technique used in handling liquids or greases(see 7.4),
10.1.5Statement of sample test temperature(125°C),col-lector plate temperature(25°C),and duration of test and dates of test,
10.1.6If nonstandard sample or collector temperatures are used,clearly mark the test report NONSTANDARD CONDI-TIONS,and note the actual test temperature,
10.1.7Initial mass of conditioned samples,S I,
10.1.8Mass of samples as taken from test chamber,S F, 10.1.9Final mass of samples after optional reconditioning for24h at50%relative humidity and23°C,S F8,if WVR determination is conducted,
10.1.10Percentage of total mass loss,TML(normally three values for each material and the average value),
10.1.11Percentage of water vapor regained,WVR(nor-mally three values for each material and the average value),if determined,
10.1.12Initial mass of the dried collector plates,C I,
10.1.13Change in mass of the control collector plate,C S,in grams,
10.1.14Final mass of the collectors,C F,
10.1.15Percentage of collected volatile condensable mate-rial,CVCM(normally three values for each material and the average value),
10.1.16Infrared spectrum or other analytical description of the condensed contamination when determined,and
10.1.17Remarks about any noticeable incident or deviation from standard conditions observed during the test.
11.Precision and Bias
11.1Precision of these measurements was established by interlaboratory tests of7materials by13organizations.Preci-sion for particular materials is affected by the nature of the material as well as testing variance.For example,monolithic, homogeneous materials with relatively low TML and CVCM values will have high precision and low standard deviation. Materials that are mixed and cured individually before testing may not be homogeneous or completely comparable from organization to organization.Despite such possible variations, the test can successfully identify“good”and“bad”lots of materials,and screen out relatively low outgassing materials from relatively high outgassing materials.For example,DC340 grease was tested and found to have an average TML value of 0.0867%60.03459%for the15organizations.Polyethylene beads had an average TML value of0.3849560.0047%for the15organizations and an average VCM of0.14416 0.0039%.The same polyethylene beads were tested twice previously.TML values were0.3798660.0077%and0.3649 60.0375%.VCM values were0.125360.01317%
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0.141560.038%.Precision for this test method is610% (95%con?dence level)for TML and620%for CVCM. 11.2Bias for this test method has not been determined. 11.3Precision of WVR is in?uenced greatly by whether or not the material is hydrophilic.For example,CV2566silicone WVR was measured by15organizations as0.019216 0.00313%,or a3sigma uncertainty of48.8%.G569glass tape had WVR of0.0936860.01314%,or a3sigma uncertainty of42.1%.A reasonable approximation is40to 50%uncertainty in WVR for most materials with low WVR.
12.Keywords
12.1Collected V olatile Condensable Material(CVCM); material selection;material test;Outgassing;screening test; spacecraft materials;Total Mass Loss(TML);V olatile Con-densable Materials(VCM)
ANNEX
A1.CLEANING AND STORAGE
A1.1Cleaning
A1.1.1General—The components shall be cleaned after fabrication to remove any residual oils,and so forth,from the fabrication process.The cleaning operations in A1.1.2-A1.1.9 shall be performed before each test run unless otherwise speci?ed.
A1.1.2Aluminum Boats—Vapor degrease the boats for5or more min.A1:1by volume acetone:ethanol solvent blend has been used successfully for this purpose.Dry the boats at1256 5°C for at least4h.
A1.1.3Collector Plates—Immerse and agitate collector plates in the solvent.Pure acetone rinse followed by rinsing in reagent grade or denatured ethanol has been used successfully. Rinsing may be followed with vapor-degreasing for15min.A 1:1by volume acetone:ethanol solvent blend has been used successfully for this purpose.Dry the collectors for4h minimum at12565°C.
A1.1.4Specimen Chamber and Heating Bar—Take special care with the bar between test runs to avoid contamination during subsequent tests.Wash the bar cavities and surface with a suitable solvent.A1:1by volume acetone:ethanol solvent blend or reagent grade or denatured ethanol has been used successfully for this purpose.Mount the bar into the system without specimens.Evacuate the system to1310?4Pa (1310?6torr)and degas the bar at150°65°C for4h minimum.This is25°C above the normal test temperature. Then turn off the heater to the bar and allow the bar to cool under vacuum.Leave the heater chamber bar in place in the vacuum system.It need only by removed after the test for recleaning.The vacuum system can be con?gured to close off the bell volume,if necessary,thus permitting the vacuum-pumping system to be off over a weekend.
A1.1.5Separator Plate—Wash the separator plate with a suitable solvent.A1:1by volume acetone:ethanol solvent blend or reagent grade or denatured ethanol has been used successfully for this https://www.wendangku.net/doc/3012479230.html,e?ltered dry nitrogen gas to remove particulates and to evaporate solvents.
A1.1.6Collector Plate Support—Following the system de-gassing described in A1.1.4,wipe the collector plate support using a suitable solvent.Reagent grade or HPCL grade ethanol has been used successfully for this purpose.
A1.1.7Vacuum Bell—Poor vacuum is frequently caused by material outgassing from the internal bell surface.Wipe down the bell interior with a suitable solvent as required to restore vacuum-operating efficiency.Reagent grade or HPCL grade ethanol has been used successfully for this purpose.
A1.1.8Other Items—Various other items such as brackets and standoffs can be cleaned as required by wiping with a suitable solvent.A1:1by volume acetone:ethanol solvent blend or reagent grade or HPCL grade ethanol has been used successfully for this purpose.
A1.1.9Cleaning Materials—All wiping materials and swabs shall be preextracted using solvents with which they will be used.(See Note A1.1).All solvents shall be of spectro-grade or equivalent purity.The nitrogen gas shall be99.9%pure or better and shall have a dew point of?60°C(?76°F)or less.The gas shall be?ltered using a Molecular Sieve5A or equivalent. Metal tubing(for example,stainless steel or copper)that is used for gas transfer shall be cleaned before use.
N OTE A1.1—A recommended extraction procedure for cleaning wiping material is a24-h treatment in a Soxhlet extractor charged with a mixture of1:1by volume acetone:ethanol solvent blend or reagent grade or HPCL grade ethanol.
A1.2Storage
A1.2.1Boats—After cleaning,the boats can be placed in 5-cm3beakers with designated compartment numbers,then stored in a desiccator that contains indicating silica gel.Seal the unit with a low-vapor pressure grease for ground glass joints.The boats shall be weighed within one day of being stored.
A1.2.2Collector Plates—The plates can be mounted on a circular plate rack and stored in a desiccator that contains indicating silica gel.Seal the unit with a low-vapor pressure grease for ground glass joints.Plates shall be weighed within one day of being stored.
A1.2.3Handling and Storage—Because of the nature of this method,it is imperative that good cleaning procedures be followed to minimize handling of cleaned parts and the introduction of contaminants after cleaning.Hence,all com-ponents that have been cleaned must be stored in such a manner as to maintain their clean state.
A1.2.4Vacuum System—Perform periodic maintenance in accordance with the manufacturer’s recommended practices to ensure good vacuum system
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APPENDIX
(Nonmandatory Information)
X1.TEST REPORTING FORM X1.1The following format is suggested for reporting raw
data and test results:
OUTGASSING DATA SHEET
Material:(name,part number,lot,and so forth)
Description:(material type,sample form,color,and so forth)
Condition:(mix and cure,pre or post condition,as received,on substrate,and so forth)
Manufacturer:
Requestor: Date:
Location:
Charge No.:
Telephone:
Blanks:
Heater Position No.()()()
Initial holder mass,g_____________________________________________
Final holder mass,g_____________________________________________
Initial collector mass,g_____________________________________________
Final collector mass,g_____________________________________________
Sample:
Heater Position No.()()()
Initial holder mass,g_____________________________________________
Initial holder plus sample_____________________________________________
Final holder plus sample_____________________________________________
Reweighed sample plus holder,24h50%RH,g A_____________________________________________
Initial collector mass,g_____________________________________________
Final collector mass,g_____________________________________________
Total mass loss(TML)%____________________________________________________________
Ave.%TML Total mass gain(CVCM)%____________________________________________________________
Ave.%CVCM Total water regained A____________________________________________________________
Ave.%WVR (Sample WVR)
____________
A WVR measurement is optional
Remarks:(Sample appearance,collector appearance after test,any test anomalies,nonstandard conditions,problems,and so forth)
Date test begun:
Sample temperature,°C:
Collector temperature,°C:
Date test completed:
Pressure torr:
Time at test temperature hours:
Operator signature:
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密室逃脱计划书
密室逃脱计划书 一、项目介绍 真人密室逃脱，打破了电脑游戏的局限和束缚，原汁原味的展现了密室的精髓，让玩家能过通过自己的双眼和双手，经过逻辑思考和观察力，不断的发现线索和提示，最重要的是团队的合作，能够顺利的逃脱。整个过程充满了未知性和不确定性，在紧张的场景氛围中，真正的融入到故事背景中去，这是电脑游戏所无法提供的乐趣。 真人密室也是在2011年才在国内正式起步，相较于国外已经成熟的体系，还未完全被大众所接受。2011年9月20日，第一家主营真人密室逃脱的俱乐部，在杭州正式成立。据可靠统计，全国目前已经有超过500家以上真人密室逃脱俱乐部，其中以北上广三地发展最为迅速。福州地区2013年3月左右，开始出现第一家真人密室逃脱俱乐部。我们的密室逃脱俱乐部名为八度空间，于2013年5月开始经营，属于福州地区比较早的密室商家。 二、市场分析 1.市场前景分析： 我们都是生活在平静生活中的普通人，每天重复着相同的事情，毫无生机。即便有着看电影、唱K、泡吧等种种休闲活动，但是对于追求新鲜的年轻人来说，闲暇时间还是显得越来越乏味。而要脱离这种提不起劲的困境，逐渐兴起的真人主题密室逃脱无疑会是一个最好的选择。密室逃脱实体游戏项目，既好玩刺激，又可以让每个体验者在游戏中充分调用智慧和体力，享受酐畅淋漓的畅快感觉。 据调查，福州2010年人口711万，现在福州的密室逃脱有6家（有实力），一年的订单数为22100个，票价35左右。和福州的土地面积差不多大小的洛阳和北京，与之比较，洛阳和北京的密室逃脱比福州早一年开始，2010年洛阳人口680万，现在洛阳一年的订单数为27200个，但是只有一家的密室逃脱（有实力），为寡头市场。2012年北京人口2069万，现在北京一年的订单数为49000个，票价70元，11家密室逃脱。福州与洛阳比较：店铺越多，接收客源面积越大，订单数越多。所以福州的未来市场的需求量为增幅状态。福州与北京比较：价钱越贵，订单数越少。所以福州的未来市场的需求量为增幅状态。 注：以上数据来源于美团网和中国知网，店铺收入不单单来源于网络的团购，还有其他收入，所以这只是代表部分的收入，所以当做消极悲观者的眼光来看待市场的需求量也是为增幅状态。 作为一个新兴行业，它的市场是还没有饱和的，你的质量比别家的好，有吸引力，客源量就会增加。结论：2014年起，至少一年，市场的需求量为增幅状态。 2.与传统娱乐项目对比的优势 ①体验刺激 或许过山车的尖叫只是生理上的一种释放，但是主题密室逃脱却能够从心理上让体验者感受刺激。各种精心布置的主题场景，暗含玄机的种种物品，还有与场景相配的音乐，这些都能够让体验者产生一种身临其境的感觉，从而可以更快地融入密室逃脱当中。当然，情节悬疑也是好玩的密室逃脱中一个重要影响因素。只有环环相扣的故事情节以及层层迭进的线索，才能够带动体验者更充分地享受推理和逃脱的过程。 ②高科技力挺 密室逃脱要做得好仅仅依靠故事情节和环境布置就太单薄了，高科技产品的使用也是使密室逃脱更加真实的一个诀窍。运用高科技物理机械和电子幻灯制造悬疑的场景气氛，炫酷的室内特技效果让场景显得更加逼真，而红外线、夜视仪等道具的使用也充分调动了体验者的紧张感和积极性。这些高科技的使用让密室逃脱不仅仅只是一个游戏项目，还成为一场科技产品展示的体验与经历。 ③价值无限 如果只将其当作是一个娱乐项目未免有点太低看真人密室逃脱了，因为在整个的逃脱过程当中，除了让体验者感受刺激和悬疑以外，还考验了每个体验者的智力、耐性以及良好的团队协作力。只有将团队中每个人找到的线索结合起来，才能够找到正确的出路。当然，这中间也需要有人指挥，有人配合，一旦团
小游戏----密室逃脱
活动名称：大班数学探索活动----密室逃脱 设计思路： 偶然的机会听孩子们分享自己玩游戏的经验，发现他们对比较有挑战性的游戏如密室逃脱闯关等非常感兴趣，于是，我就想：能不能用游戏这样一个载体，将数学这一学科的某些知识呈现在里面？于是，我就按照自己的理解，把生活中常见的物品分成几个层次：将游戏材料有的散点状放置，有的向不同方向有序排列，有的重叠排列等，投放到科学探索区内，观察幼儿的游戏情况。在幼儿操作材料过程中，我发现他们数数时的方法、速度、能力等都有异同，因此，我梳理了幼儿的一些数数经验，结合大班幼儿的年龄特点，生成了本次活动。 活动目标：1、在幼儿观察、比较、推理中，尝试通过操作材料，探索可以将物品数正确的方法。 2、仔细倾听同伴的想法，乐意分享观察方式。 活动准备：幼儿操作卡（每人2张）、PPT4张、笔、夹子、照片。 活动过程： 1、呈现密室，激发幼儿兴趣：了解幼儿数数的能力。 出示PPT1，谈话引出课题 1、讲解密室逃脱游戏规则。 师：今天，老师带你们玩密室逃脱，你知道这个游戏怎么玩吗？师讲解游戏规则：密室逃脱就是我们进入房间，通过数房间里各种物品的数量来推算出房门的密码，从而打开房门，逃出密室。 2、报数游戏：让幼儿数数接龙。 师：清点人数完毕，请你们摆一个最漂亮、最帅气的姿势跟老师们打个招呼，不然，待会出不来可能没有人来救你。 3、谈话：你能数到几？ 师：刚才集体报数完全正确，现在，我问问小朋友，你最多能数到几？我说一个数字，你接着往下数，往下数（）个数。（教师一方面关注幼儿数数是否正确，另一方面关注幼儿从十位数数到百位数数的能力，同时，观察其他幼儿，聆听每个幼儿的数数情况。）师：小朋友们都能数到很大的数，真了不起！但你们数数的正确性怎么样呢？老师会在游戏中检查你们的本领。 2、进入密室：探索正确数数的方法。 第一环节：来到密室一：出示PPT2 师：我们已经进入密室，现在，赶紧来找找怎打开房门的密码。（引导幼儿找到门上的密码锁，通过寻找密码打开锁从而逃出密室。）密码锁提示我们找哪些物品？ 1、幼儿完成相应操作卡，正确数出PPT上相框、靠枕、猫及红花的数量。 师：密码锁提示我们：要仔细找找密室里有几幅相框？靠枕有几个?猫有几只？红花有几朵？把你观察到的结果记录在对应的空格里，不会写数字的用圆点代替。（教师重点关注猫和红花的记录情况） 2、幼儿交流自己的观察结果。教师及时提升幼儿表达的数数要领： A、一起告诉我，相框有几幅？靠枕有几个？师总结：东西比较少，数起来很方便； B、数猫可就不简单了，请您告诉我，你数到有几只猫？你在哪里找到了第×只猫？师总结：要把东西数清楚是需要讲究方法，要从上到下、从左到右、从前到后，只要按照一定的顺序就能数清楚。（教师要重点关注幼儿的表达，如方位是否正确，语句是否完整，还要关注幼儿数猫的方法） C、这里的花特别多，你是怎么数的？你是怎么数的？黄花能不能数进去？引导幼儿说出2个2个一起数的规律。师总结：数东西的时候，不但要讲究顺序，而且要仔细看清楚题目，
密室逃脱相关 (2)
Q1:别人做密室逃脱 从大二时，开始接触密室逃脱游戏，到今年寒假一天能玩上三、四次，“既然大家都喜欢，干嘛不自己也开一个呢？”黄皓月介绍，决定开一个“密室逃脱”店，很偶然，也很仓促。5个爱玩密室的女孩当即一拍即合，其中有两个女生已经工作，三个在校生中，黄皓月也即将本科毕业，她还“跨界”选修了金融专业的双学位。 三月份，考察江汉路所有密室逃脱店、玩遍40多个主题，敲定店址； 四月份，店面装修，自己设计主题、自己安装机关、自己制作装置……； “五一”，新店开张，首日客流量过百，不大的客厅里，挤满了前来“尝鲜”的同龄人。 开业的前一天，女孩们都在店里通宵加班，“创业比考研费精力多了，四月份的时候，天天熬夜。”黄皓月告诉记者，开店，比想象中的复杂、琐碎。对于“学霸”的称号，她觉得那是上高中以前的事了，从高二起，一直到现在，她更愿意把自己定义为“学霸班上的玩货”。 中考前，黄皓月因成绩优秀，提前保送到当地最好的学校——新洲一中“火箭班”。然而高一的第一次月考，成绩仅排在班上十几名，随后几次月考，更是滑落到二十几名。“我已经很努力了，学习成绩就是上不去。”家长的不理解，老师的不重视，让曾经的“神童公主”的骄傲光环瞬间破碎，从台上最闪亮的“明星”，跌落成台下普通观众，巨大的落差，让她一度“放松”自己，按照自己的意愿学习、生活，成为学霸班上的“另类”。 “其实二十几名已经很好了，至少可以考上武大华科，但那个时候没有人告诉我，我以为自己真的很差。”说到这里的时候，黄皓月的眼中有一丝伤感和落寞，虽然之后成绩时常徘徊在班上倒数几名，但高考总分依然超过一本分数线，考入湖北大学生物科学专业。
小游戏----密室逃脱
活动名称： 大班数学探索活动----密室逃脱 设计思路： 偶然的机会听孩子们分享自己玩游戏的经验，发现他们对比较有挑战性的游戏如密室逃脱闯关等非常感兴趣，于是，我就想： 能不能用游戏这样一个载体，将数学这一学科的某些知识呈现在里面？于是，我就按照自己的理解，把生活中常见的物品分成几个层次： 将游戏材料有的散点状放置，有的向不同方向有序排列，有的重叠排列等，投放到科学探索区内，观察幼儿的游戏情况。在幼儿操作材料过程中，我发现他们数数时的方法、速度、能力等都有异同，因此，我梳理了幼儿的一些数数经验，结合大班幼儿的年龄特点，生成了本次活动。 活动目标： 1、在幼儿观察、比较、推理中，尝试通过操作材料，探索可以将物品数正确的方法。 2、仔细倾听同伴的想法，乐意分享观察方式。 活动准备： 幼儿操作卡（每人2张）、PPT4张、笔、夹子、照片。 活动过程： 1、呈现密室，激发幼儿兴趣： 了解幼儿数数的能力。 出示PPT1，谈话引出课题 1、讲解密室逃脱游戏规则。 师：
今天，老师带你们玩密室逃脱，你知道这个游戏怎么玩吗？师讲解游戏规则： 密室逃脱就是我们进入房间，通过数房间里各种物品的数量来推算出房门的密码，从而打开房门，逃出密室。 2、报数游戏： 让幼儿数数接龙。 师： 清点人数完毕，请你们摆一个最漂亮、最帅气的姿势跟老师们打个招呼，不然，待会出不来可能没有人来救你。 3、谈话： 你能数到几？ 师： 刚才集体报数完全正确，现在，我问问小朋友，你最多能数到几？我说一个数字，你接着往下数，往下数（）个数。（教师一方面关注幼儿数数是否正确，另一方面关注幼儿从十位数数到百位数数的能力，同时，观察其他幼儿，聆听每个幼儿的数数情况。）师： 小朋友们都能数到很大的数，真了不起！但你们数数的正确性怎么样呢？老师会在游戏中检查你们的本领。 2、进入密室： 探索正确数数的方法。 第一环节： 来到密室一： 出示PPT2
《密室逃脱》碧绿色房间闯关攻略详解
《密室逃脱》碧绿色房间闯关攻略详解 继博士的家之后，小编接下来要为大家介绍密室逃脱碧绿色房间闯关攻略。密室逃脱，又 叫TAKAGISM ，是一款密室闯关游戏，游戏需要玩游戏者在游戏中寻找线索，一步一步地走出 密室。《密室逃脱》游戏的玩法很简单，只需用鼠标即可。整个游戏过程都是在一间房子里进行的，游戏的主人公不知道为什么被困在这里(每集都交待了不同的原因，但这些原因都是相当的 离奇)T akagism的逃离房间系列是非常经典的解迷小游戏，自从作者推出第一个版本Crimson Room后便深受世界各地网友的喜爱，并因此掀起了一股“逃离房间热”。本文将详细介绍密室逃脱碧绿色房间如何闯关。 1、开灯，左转(点画面的左下角,右转同理)在鞋橱的鞋下边发现“若”字图片;鞋橱底发现镜框。 2、左转，在土黄色的垫子底下发现“般”字图片。 3、左转，在壁橱的最上一格中左右边分别发现“多”字图片和一束香。二格的红笔记本有锁打 不开，在最下面的小橱里发现黄影集里两张照片。 4、点地上的红毯子，发现骷髅！点击靠近，在左手手腕处发现钥匙,右手发现药瓶，点小腿处的红绳物体可以把毯子叠起，并发现脚上有密码锁(暂时不开)，点物品栏中的红毯，再点下边的“查看物体”(即"About Item")，可放大，点大图的红毯子得到十字架状物体。 百度攻略&口袋巴士提供 1
5、左转，在斜对着蓝门处，（就是那个有窟窿的蓝门，不是一开始的那个门）。点头顶的 灯罩，在灯罩上发现“罗”字图片（小红块，仔细点），在墙上发现“ 蜜”字图片（小白块）。 6、左转，在小冰箱里发现“ 波”字图片和一罐啤酒（啤酒先不要拿，因为骷髅要冰冻的）。在旁边的红桶里发现张纸，打开是些黑头发。记住：点装黑头发的纸，然后点击查看物体，放大纸，多点几下纸，然后就可以在红桶底下得到打火机。 7、用钥匙开红笔记本打开，在日记中可以找到女孩的生日，那就是开骷髅脚上的密码。(通常会是在日记的第四页，里面有一句话“The day after tomorrow is her birthday”，这一天的简单写法 就是密码。你先看你所翻到的那页日记上是几月几号，再在那个日期后加两天，就是小女孩子的 生日，那一天的简写就是密码。（如9月10日，简写就是0910，这就是密码），记下密码。继续翻日记，翻到最后得到一张CD。 8、放大装有头发的纸，点打火机，再点纸，可以烧出东西来，放大药瓶，里面有两粒药，一 张写有箴言的纸。放大绿十字，按照箴言的顺序位置和烧出来得数字相对应（形位相同），把字（ 6张图片）填在十字架状物体上（位置随机的），放对会变成个四方体，放下暂不用。 9、在壁橱的第3格，有香炉和磬（旁边红的是槌），把装有CD的CD盒放在香炉后面,把香放香炉左，罐啤放香左（要冰镇的啊，冰一两分钟就可以拿出来了，先把啤酒从冰箱拿出来，点显 百度攻略&口袋巴士提供 2
真人密室逃脱指南
现在，非常流行真人密室逃脱的游戏，让你进入密室里面，想尽一切办法逃出来。很多人不明白这个怎么玩，小编今日以自己的经验为你介绍。 方法/步骤 1首先，你在网上查一下在你所在的地方，有什么真人的密室。最好去的人比较多，年龄是不受限制的，但是尽量不要带16岁以下的，带去了没用，而且又花费了一张票钱。 2真人密室有很多主题。比如，诅咒；医院；梦游等等。还有很多电影的，比如，生化危机；电锯惊魂；盗墓，都是很火热的主题。所谓，主题，就是说密室里面的道具、背景、风格是哪种。 3选好主题之后。价格方面，其实所以密室都是差不多的价格，除非它的规模很大。价格基本在40到65一人，团购价，如果是选择在网上团购，那么要先打电话预约时间。注意：如果你明天要去，最好是提前半天打电话。这种真人游戏需要预约。 4打电话联系，会定下你们的时间，要求是提前15分钟到她们店里。如果你不选择网上团购，那么就到现场再付费，但是也是需要预约的。因为，真人密室非常受人追捧。而且，每场游戏时间都是一个小时。 5一定要提前去。去了之后，店内都有桌游可以随便玩，有饮料供应。所以也不必担心无聊。去之前最好少带随身物品，女士包包，都要少带。进去之前，工作人员会让你交出手机（有干扰），放在保险箱里。大可放心。 6进去之后，会有纸张写密室的故事背景。进去之后，一定要注意看周围的东西。一般来说，密室里面大多都是机械化的东西，像空调就不用找了，有纸张会提示你们什么东西不用去找。然后你们就要去找东西，也就是线索。手能够得到的地方都去摸一摸。 7但是这个也不是完全凭找东西就可以通关的。要靠线索去联想怎么回事。而且，如果没有用到的东西一定要把它带在身上，很多没用到的下一关就有可能用。工作人员会发给你传呼器，是给你提示用的，你们想不出来，就可以问问他。 选择加盟魔魔岛密室逃脱的5大理由 理由1：逼真代入感，如侦探小说一般，抽丝剥茧，环环相扣的逻辑，挑战你的IQ与思维。理由2：中型线索类密室最为考验玩家的逻辑推理能力，你不仅要具有当代福尔摩斯般敏锐的观察力和想象力，还要能勇敢的探索和决断。团队配合，将会是您胜出的关键！ 理由3：体验过PC密室逃脱类游戏的玩家在体会找东西和解密快感的同时，还能体会到真实场景角色扮演的快乐。 理由4：各种梦幻场景，给玩家创造一个个惊喜。让玩家体会设计者的用心。 理由5：大型主题剧情机关解谜场景相结合，完美结合所有环节，更精致，更专业。
密室逃脱相关完整版
密室逃脱相关
Q1:别人做密室逃脱 从大二时，开始接触密室逃脱游戏，到今年寒假一天能玩上三、四次，“既然大家都喜欢，干嘛不自己也开一个呢？”黄皓月介绍，决定开一个“密室逃脱”店，很偶然，也很仓促。5个爱玩密室的女孩当即一拍即合，其中有两个女生已经工作，三个在校生中，黄皓月也即将本科毕业，她还“跨界”选修了金融专业的双学位。 三月份，考察江汉路所有密室逃脱店、玩遍40多个主题，敲定店址； 四月份，店面装修，自己设计主题、自己安装机关、自己制作装置……； “五一”，新店开张，首日客流量过百，不大的客厅里，挤满了前来“尝鲜”的同龄人。 开业的前一天，女孩们都在店里通宵加班，“创业比考研费精力多了，四月份的时候，天天熬夜。”黄皓月告诉记者，开店，比想象中的复杂、琐碎。对于“学霸”的称号，她觉得那是上高中以前的事了，从高二起，一直到现在，她更愿意把自己定义为“学霸班上的玩货”。 中考前，黄皓月因成绩优秀，提前保送到当地最好的学校——新洲一中“火箭班”。然而高一的第一次月考，成绩仅排在班上十几名，随后几次月考，更是滑落到二十几名。“我已经很努力了，学习成绩就是上不去。”家长的不理解，老师的不重视，让曾经的“神童公主”的骄傲光环瞬间破碎，从台上最闪亮的“明星”，跌落成台下普通观众，巨大的落差，让她一度“放松”自己，按照自己的意愿学习、生活，成为学霸班上的“另类”。 “其实二十几名已经很好了，至少可以考上武大华科，但那个时候没有人告诉我，我以为自己真的很差。”说到这里的时候，黄皓月的眼中有一丝伤感和落寞，虽然之后成绩时常徘徊在班上倒数几名，但高考总分依然超过一本分数线，考入湖北大学生物科学专业。 高中时期的那一段心路历程，对她触动很大，并且让“学霸班上的玩货”这一身份，一直保持到现在。今年，她们班上41名同学中，有三十几个考研，“没有同学相信我会考上，别人在学习的时候，我在玩。”她笑着说，作为前学生会副主席，如果她呆在寝室里安静的看书超过一周，所有人都会奇怪她没有不出去“活动”。 5月9日，小店开张后迎来的第一个双休日，女孩子们正在努力积累经验，希望在暑假旺季到来前，将自己打造成一个“全能女孩”。“我最大的优点，就是没有拖延症。”黄皓月觉得，“把今天做好”才是最重要的，至于最终结果是输是赢，只要自己努力过就好。她笑称，对未来没有明确的计划，如果读博的话，或许会考虑出国吧。 Q2采访5专家，2业主 业主1： 我是12年4月，5月的时候接触的密室逃脱，当时在武汉的EP逃逸层第一次接触到真人密室逃脱，当时整个武汉就两家，第一次体验了他们家的密室之后，我自己动了心思。6月我在创建了X-space真人密室逃脱。7月装修完开业，总共资金消耗6W不到，所有的谜题设计都是自己想的。那个时候也没什么房型啊，格局啊，什么的，一点纸片信息，一些文字内容，一点点的氛围，就用上房东家的家具，我们开业了。每天发发传单，做做问答，一个月的，收回了全部的成本还有不少的收益。当时也动了心思，想看看其他地方的密室逃脱是怎么做的，下一步，应该怎么发展。 永远要记住一点，你的视线永远要看着前方，比你能看到的位置更远的位置，然后收回来看脚下离目标有多远，选好节点，去执行。 我们的创业路径上很强调一个词，节点。后面也会不停的提到。