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Direct Method for the Analysis of Low Vapor Pressure Compounds on Electronic Parts

IP.com Disclosure Number: IPCOM000088243D
Original Publication Date: 1977-May-01
Included in the Prior Art Database: 2005-Mar-04
Document File: 3 page(s) / 43K

Publishing Venue

IBM

Related People

Anderson, FW: AUTHOR [+3]

Abstract

Shown are modifications made to a Finnigan 1015D Quadrupole Gas Chromatographic (GC) Mass Spectrometer (MS). This includes a bypass of the GC unit, which routes and controls the carrier gas, but makes use of the GC oven (programmable temperature) and the jet orifice separator (which removes most of the carrier gas before it reaches the MS). In place of the normal GC column (which is used to separate an organic solvent mixture into individual components), a modified sampling device was inserted.

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Direct Method for the Analysis of Low Vapor Pressure Compounds on Electronic Parts

Shown are modifications made to a Finnigan 1015D Quadrupole Gas Chromatographic (GC) Mass Spectrometer (MS). This includes a bypass of the GC unit, which routes and controls the carrier gas, but makes use of the GC oven (programmable temperature) and the jet orifice separator (which removes most of the carrier gas before it reaches the MS). In place of the normal GC column (which is used to separate an organic solvent mixture into individual components), a modified sampling device was inserted.

Fig. 1 shows the overall design. The first two sections, I and II, are the modifications to the GC unit; III and IV are not modified, but are illustrated because they are part of the total system.

Fig. 2 is an exploded diagram of the sampling device only. Equipment 1. GC/MS - Finnigan 1015D Quadrupole GC/MS Normal instrument conditions for flux analysis Mode - electron impact Mass Range - 200-310 atomic mass units (a.m.u.) Sensitivity - 10/-7/ amp/volts Scan Time - 10 seconds Filter - 10 a.m.u./second Filament current - 500 microamps Electron Energy - 70 electron volts 2. Micron Gauge - NCR 802-A 3. Vacuum Valve - Stainless Steel Bellows Valve 4. Ball and Socket joints (modified) - 65/40 Kontes (K671300-6540) 5. TEFLON* Fiber Glass Filled Ferrules - Finnigan Corp., or Polyimide Ferrules - Supelco Inc. 6. Al Clamp - custom made 7. Viton 0-ring - supplied with joints Advantages of the modification include: 1. In situ analysis of trace low vapor pressure organic (process) residual on electronic components. 2. Nondestructive analytical technique. 3. Can also be used to detect volatiles. 4. Sensitive (10 mu g of flux). Procedure for Analysis (Flux).

1. The sample is loaded in the sample device which is sealed with the Al clamp.

2. The wing nuts on the bolts are tightened sufficiently to compress the Viton 0-ring.

3. The bottom of the sample device is connected to copper tubing via a union with a SWAGELOK** (or equivalent) nut using the TEFLON or polyimide ferrules.

4. Similarly, the top of the sample device is connected to another union.

5. The sample device is supported from the top of the oven with two clamps and springs. This is a precautionary step in case the upper seal expands during later temperature programming.

6. The sample device is then evacuated using a 25 liters/min. forepump and a 600 liters/sec. silicone oil diffusion pump. The g...