background image

 

6875D Freezer/Mill 

 

1300-87052-1A, REV 1 

 

SPEX SamplePrep LLC 

         Page 25 of 36 

6.5 Opening, Emptying, and Cleaning Freezer/Mill Vials

 

(Cont’d)

 

 
polycarbonate center section.  The best way to prevent the Extractor from jamming is to make 
sure both the Extractor and the threaded end plugs are dry and clean before you use them.   
 
If the Extractor/Vial Opener jams when being threaded into a cold end plug, it is probably due 
to water condensing and freezing on the extractor screw.  The water freezes when it contacts a 
cold end plug.  Wipe off the screw with a paper towel before each use.  Note that the end of 

the screw is tooled with an “X” cut to help remove any ice that forms on the end plug. 

 Chilled 

vials can also be opened easily and quickly with the optional accessory 6808 Extractor for Large 
Freezer/Mill Vials. 
 
On rare occasions an end plug will stick in the vial when cold, even if the Extractor screw and 
end plug threads are dry and clean.  If this happens do not force the end plug out, as the vial 
and/or the Extractor may become damaged.  Allow the vial to warm up.  The end plug can be 
extracted easier by allowing the vial to warm up gradually, or by wrapping vial in several layers 
of cloth or paper towels.   
 

CAUTION:

  

Pressure can develop inside a Freezer/Mill vial as it is warming.  As pressure builds, 

an end plug can pop out with force and the sample can be lost.  For this reason 
handle vials with care.  It is best to open chilled vials immediately after removing 
them from the Freezer/Mill.

 

 

 

6.5.2 Emptying a Vial 

As soon as an end plug is removed from a cold vial, empty the contents of the vial into a 
suitable container, the quicker the better as condensation on a cold sample occurs rapidly.  
Often it is helpful to tap the closed end of the vial to release the ground sample.  Remember 
that the impactor may slide out ahead of the contents or with them, and that the longer the 
sample is exposed to air, the more moisture it will acquire.  Note, samples which were tacky, 
spongy, etc., at room temperature will return to that state as they warm up, and may 
agglomerate. 
     
The impactor will have to be separated from the sample and can be handled with gloved 
fingers, a strong magnet, or tongs.  Tools without a good gripping surface are likely to slip off 
the impactor.  The 6870L and 6870S Accessory Packs include a Magnetic Extractor (6791).  This 
is a rod with a magnetic tip that can be used to remove the impactor from a vial before 
emptying the contents. 
 
If some condensation on a cold sample is unacceptable, either wait for the sample vial to warm 
up before opening and emptying it, or open and empty a chilled vial in a glove box filled with 
dry nitrogen gas. 
 
Small amounts of sample usually adhere to 

the vial’s impactor, end plugs, and plastic cylinder.  

Brushing or scraping these surfaces of the vial can often recover this fraction of the sample.  
Again, speed is important to minimize condensation and other effects of warming. 

Summary of Contents for 6875D

Page 1: ...V 1 65 Liberty St Metuchen NJ 08840 1 855 GET SPEX 438 7739 or 732 623 0465 www spexsampleprep com 6875D LARGE FREEZER MILL OPERATING MANUAL For 6875D 115 and 6875D 230 Freezer Mills this manual is Pa...

Page 2: ...the work may be reproduced or transmitted in any form or by any means electronic or mechanical including photocopying and recording except as may be expressly permitted by the 1976 Copyright Act or in...

Page 3: ...nel 13 5 3 Changing Settings 17 5 4 Saved Protocols 18 6 0 Operation 20 6 1 Standard Auto Fill 20 6 2 Manually Adding Liquid Nitrogen 21 6 3 Loading Vials into the Freezer Mill 24 6 4 Removing Vials f...

Page 4: ...o not set up the 6875D Freezer Mill in an insulated or confined space The Freezer Mill should be run on an open countertop in ambient air with recommended maximum relative room humidity 70 from 5 C 31...

Page 5: ...nce of any vial sample combination depends on sample properties cooling time grinding time desired outcome etc Effective capacity for a given sample is determined by experiment Overfilling a vial grea...

Page 6: ...ories We recommend storing the packaging materials in the event there is a need to return the unit for warranty service or repairs Grinding vials must be purchased separately and are available in four...

Page 7: ...RJ45 Ethernet cable connector At the back of the controller is an USB Port to download run data or to upgrade software Caution 4 1 Electrical Connection Plug the electrical cord into the AC Inlet on...

Page 8: ...scribed and illustrated in Section 5 2 The programmable parameters include Cycles number of grinding periods Precool Time initial chilling of sample Run Time grinding period Cool Time time between gri...

Page 9: ...e a male 3 8 inch 9 5 mm NPT outlet SPEX transfer hoses come with a matching female 3 8 inch NPT fitting Excessively long transfer hoses are not recommended LN Tanks come in two types high pressure an...

Page 10: ...Chamber 1 and Chamber 2 of the assembly The Gate keeps the vial s in place during grinding for Chambers 1 and 2 only The vials in the precooling chambers will remain secure and unaffected by the magne...

Page 11: ...from being interrupted by low liquid nitrogen levels use the Auto Fill mode with LN Tank connected In the optional Manual Fill mode the unit will not run if the proper LN level is not maintained The...

Page 12: ...the screen with a fingertip or stylus Do not use a sharp point as this can damage or deface the screen 5 1 Logo Screen When the power is switched ON at the back of the mill Please Wait appears during...

Page 13: ...Chamber 1 will run as indicated by the MONO button color highlighted blue 1 Precool the coil is inactive while the vial cools in liquid nitrogen for 1 minute Samples must be precooled before grinding...

Page 14: ...or paused in the middle of a grinding program from the button selections to the right of the screen The Auto Fill or Manual Fill buttons are also displayed on Control Panel When a button is selected...

Page 15: ...tub is filled with liquid nitrogen to the correct level and the lid is securely latched the STATUS BAR will turn green and begin counting down The PRECOOL sequence will start indicating the beginning...

Page 16: ...indicating by the yellow symbol At the end of each Cool Time period a green check mark is placed next to that field The Rate is 10 cps cycles per second The STATUS BAR top of screen counts down the t...

Page 17: ...d after the program has stopped then the entire program will start over To pause during a grinding program touch the button The RUN will hold the settings at that moment elapsed time cycle etc To resu...

Page 18: ...s the last programed run setting that was not saved The Default protocol can be changed without saving the new settings as described in section 5 4 5 4 1 Storing a new program To store the new program...

Page 19: ...e anything on the screen but returns the display to the SAVED PROTOCOLS screen To run the newly saved protocol touch the protocol to highlight BLUE the name Then touch the LOAD button to send protocol...

Page 20: ...the Freezer Mill and pressure is relieved through this vent 6 1 Standard Auto Fill When the 6875D Freezer Mill is set up for the first run of the day with a loaded vial s in the grinding Chamber s ma...

Page 21: ...only be added to 6875D Freezer Mill with the lid open To open the lid hold the lid down with one hand and with the other hand pull the upper end of the latch toward you Then pull the lower end of the...

Page 22: ...vial and fill the vial 1 3 to 1 2 the volume with sample pieces Typical sample sizes for the various size of vials are shown below in Table 1 Table 1 Typical Sample Sizes Sample Large Vial 6801 6803...

Page 23: ...aped piece of bone or a tough polymer can act as a wedge to push a moving impactor through the side of the polycarbonate tube 6 2 3 Loading a Sample into a Vial at Room Temperature Attach the end plug...

Page 24: ...e lid must be closed and latched for the Freezer Mill to run Push the lid down hold it down while engaging the bottom part of the latch and then lock the latch by pushing its top end toward the cabine...

Page 25: ...st For this reason handle vials with care It is best to open chilled vials immediately after removing them from the Freezer Mill 6 5 2 Emptying a Vial As soon as an end plug is removed from a cold via...

Page 26: ...samples uses but as soon as they begin to crack they should be discarded Liquid nitrogen can enter through cracks and vaporize when vial is removed from Freezer Mill As the vial warms vaporized LN wi...

Page 27: ...ources button On the Resources screen as seen in Figure 15 are additional buttons to recall the run history technical support accessories e g vials holders etc and training information e g how to vide...

Page 28: ...ractors as shown in Figure 17 To open any of the categories listed touch the button to the right of the screen For example pressing the button for the Extractors displays the screen for items availabl...

Page 29: ...g button on the Resources screen In the Training screen the operating manual instructions and how to use videos are listed To open any of the categories listed on the screen touch the button name as d...

Page 30: ...en 7 5 Technical Support To access the Technical Support screen touch the Tech Support button on the Resources screen SPEX contact information for the USA Headquarters and Europe Sales Office is liste...

Page 31: ...ny samples powder materials or liquids are spilled inside the unit during a sample run wait until Freezer Mill is finished for the day the liquid nitrogen has evaporated and the mill has warmed up to...

Page 32: ...mpletely Close the lid and latch Push the lid closed and latch into place Screen displays LN LEVEL LOW Liquid nitrogen sensor detects inadequate liquid nitrogen level In Auto Fill mode check LN Tank a...

Page 33: ...and start again Flanged end plug doesn t come out the cold vial End plug tube joint too tight when very cold Allow vial to warm up Blunt end plug doesn t come out room temperature vial Hard to grip W...

Page 34: ...negligence or misuse 10 1 Product Specifications Every effort has been made to provide complete and accurate product operating information in this Manual However since specifications are subject to ch...

Page 35: ...ent with the disposal symbol must not be disposed of with general waste See Figure 22 Throughout the European Community guidelines regarding disposal regulations may vary from territory to territory P...

Page 36: ...e www spexsampleprep com E mail sampleprep spex com In Europe please contact our European Sales Office at SPEX Europe 2 Dalston Gardens Stanmore Middlesex HA7 1BQ United Kingdom Tel 44 0 208 204 6656...

Reviews: