School of GeoSciences

Compositions

Samples of 13 resins were mounted together with approximately ten, 1.5-2.5mm glass balls (VWR, Product number 332134Y) in individual 25mm diameter, 5mm deep, Al-rings. The remaining three; Araldite, Araldite rapid-set and Varian Torr Seal were mounted in Al-rings without the glass balls.

 

X-Ray Analysis: Sample preparation

SEM

All 13 mounts were then ground so a section could be seen through the balls using Beuhler UltrPrep nickel bonded diamond 74 micron and 20 micron discs followed by 1200 and 2500 silicon carbide paper. They were polished with 3 micron diamond for 15 minutes and then 0.3 micron Al-oxide for 10 minutes, washed and then ultrasonically cleaned with 10% Decon 90. The samples were finally cleaned with ethanol prior to carbon coating using a Deton coater to produce a thin conducting film across the sample surface.

All samples were treated identically and following the routine grinding and polishing procedures used at Edinburgh University.

 

X-Ray Analytical Conditions

Energy dispersive X-ray analysis of the resins was performed using a Philips XL30CP with PGT Spirit X-ray analysis software. The X-ray spectra were collected for a livetime of 600 seconds using a 20Kv, 5nA current measured with a Faraday Cup and Keithley picoamplifier (Model 486).

All the X-ray spectra may be downloaded:

 

X-Ray Results

Epoxy Resin EDS Spectra Comments
EpoThin X-Ray spectra show high C, O and moderate Cl concentrations
EpoHeat X-Ray spectra show high C, Si, Cl and moderate O concentrations
EpoxiCure RT X-Ray spectra show high C, O and Cl
EpoxiCure 65 X-Ray spectra show high C, O and Cl
TransOptic X-Ray spetra show high C and O concentrations, by far the cleanest spectra
ProbeMet Composition highly variable. Contains fragments of Si and Cu.
KonductoMet Composition highly variable. Contains fragments of C and Si with O, Al, Cl, Na and S
SpeciFix-20 X-Ray spectra show high C, O and Cl, as well as Si and S
EpoFix X-Ray spectra show C, O and Cl
Ciba Geigy MY778 & HY951 X-Ray spectra show high C, O and Cl
Robnor Resins PX771c X-Ray spectra show high C, O and Si
Korapox 439 X-Ray spectra shows high C, O, Si, and Cl
Domestic Rapid set Araldite X-Ray spectra variable significant S levels and C, O, Al and Cl
Domestic Araldite X-Ray spectra show high C, O and Si with small amount of Cl
Varian Torr Seal X-Ray spectra show significant amounts of C, O, Mg, Si, S and Ca as well as Cl, k, Ti, Na and Al.
Petropox X-Ray spectra show large amounts of C and O as well as F, Si and Cl

 

SIMS Analysis: Sample Preparation

Secondary Ion Mass Spectrometry (SIMS) analysis was performed on the all 13 resins mounted in two blocks together with 3 separate 25mm diameter blocks. All samples were ground and polished using the procedure outlined above, then coated with a ~30nm layer of gold, and pre-pumped in the instruments air-lock for >12hrs prior to analysis.

 

SIMS Analytical Procedure: Positive Ions

The analyses were performed using a Cameca ims-4f at Edinburgh University using a 5nA, O- primary beam with a net impact energy of ~14KeV. High energy (75eV +/20eV) positive secondary ions were extracted and detected by an electron multiplier.

 

SIMS Results: Positive Ions

A subset of the analysed species is presented below. The complete data set is available for Excel:

 

Avg Cps 7Li 11B 23Na 27Al 30Si 39K 40Ca 56Fe
Araldite 10.1 200.6 8424.8 9318.7 37.9 2414 556.9 9.3
Ciba-Geigy 0.3 0.1 341.1 68.6 1.8 76.6 90.9 1.0
Epofix   1.3 0.0 424.6 12.5 1.2 88.5 104.3 0.6
Epoheat   0.0 0.0 180.1 167.0 1.1 127.3 24.6 5.1
Epotech 0.3 0.4 259.9 77.4 1.3 47.0 89.0 22.5
Epothin   1.8 0.1 419.3 78.4 0.6 84.4 125.1 1.0
Epoxicure (65) 0.1 0.3 208.4 43.8 1.5 89.5 22.1 5.0
Epoxicure (RT) 0.1 0.3 225.5 24.1 1.0 87.5 16.9 4.8
Konductomet 1 673.6 33.9 56253.9 111765.7 1301.7 6021.4 339154 3206.7
Konductomet 2 399.9 55.4 3638.8 122379.9 1808.3 4399.9 10249.0 2850.9
Korapox 1.0 0.0 316.8 51.5 47.4 101.9 32.1 4.9
Petropoxy 0.6 4140.5 2338.7 66.0 0.1 226.8 121.0 1.6
Probemet 1 126.3 1.6 1924.7 13690.9 25036.9 1411.5 21510.3 2222.8
Probemet 2 29.4 4.1 188.4 11213.2 266174.3 495.3 523.6 5334.4
Robnor 0.4 0.1 266.0 90.4 0.5 76.3 17.0 5.9
Specifix 1 5.5 0.0 330.1 14.0 60.5 55.8 79.6 0.8
Specifix 2 5.8 0.1 325.3 18.5 70.0 57.0 72.1 0.8
Transoptic 0.0 0.0 183.5 272.4 0.1 46.1 38.0 4.1
Varian 5939.6 12384.0 29995.3 27368.6 123524.6 9921.8 453257.0 5025.2

 

SIMS Analytical Procedure: Negative Ions

The analyses were performed using a Cameca ims-4f at Edinburgh University using a 5nA, O- primary beam with a net impact energy of ~5.5KeV. High energy (50eV +/20eV) negative secondary ions were extracted and detected by an electron multiplier.

 

SIMS Results: Negative Ions

A subset of the analysed species is presented below. The complete data set is available for Excel:

 

Avg cps 1H 12C 16O 19F 31P 34S 35Cl
Araldite 1 103210.9 604142.4 278431.2 143.3 8.4 5018.1 24472.2
Araldite 2 97462.0 570725.2 279737.4 166.3 9.8 4682.9 24972.1
Ciba-Geigy 1 152547.1 577036.3 183923.0 26.1 0.0 2.4 44100.9
Ciba-Geigy 2 151389.8 575994.9 183455.1 20.6 0.1 2.0 43813.3
Epofix 1 161630.3 595732.2 182977.7 50.6 0.3 3.4 47323.3
Epofix 2 161114.4 601145.2 186002.8 51.5 0.5 2.3 47705.0
Epoheat 1 155836.1 562125.1 177080.4 40.9 0.0 1.9 6639.5
Epoheat 2 150379.4 546604.9 172108.5 12.3 0.3 2.8 6331.7
Epotek 1 165913.1 646453.1 206876.6 14.4 0.3 3.5 10445.8
Epotek 2 167596.9 630934.7 202268.4 20.4 0.1 6.8 10825.3
Epothin 1 161557.8 587276.6 181599.8 32.4 0.5 3.5 34409.7
Epothin 2 160408.6 582454.5 180029.7 25.6 0.4 3.3 34142.0
Epoxicure (65) 1 157012.4 576122.8 182511.5 34.4 0.0 2.4 29574.3
Epoxicure (65) 2 154937.4 568578.2 179551.5 36.1 0.0 2.0 29439.9
Epoxicure (RT) 1 157278.1 583654.5 185593.4 33.6 0.1 2.5 28972.0
Epoxicure (RT) 2 154156.6 572434.0 183487.0 34.0 0.0 2.1 28857.7
Konductomet 1 10171.9 163485.6 178398.7 253.3 4.4 22.5 768.5
Konductomet 2 4743.8 141963.3 160235.0 208.1 15.8 38.6 753.0
Korapox 1 140811.5 518964.3 161783.3 10.8 1.4 6.9 41518.1
Korapox 2 128456.8 462115.3 142529.1 9.0 1.1 5.9 37258.4
Petropoxy 1 161916.1 590259.9 198452.0 229900.7 40.4 0.6 4490.5
Petropoxy 2 164242.5 590249.7 199616.4 231140.6 40.1 0.3 4437.8
Probemet 1 42260.4 348691.5 3864146.3 77.3 8.9 29.1 4912.4
Robnor 1 39980.3 171837.7 53335.3 13.1 0.0 1.1 12257.9
Robnor 2 41091.7 174377.7 53995.6 13.0 0.1 2.0 12451.6
Specifix 1 150713.4 606233.2 204969.0 36.5 1.1 60.1 76316.9
Specifix 2 150336.5 609250.7 205630.9 35.3 1.3 56.8 76274.7
Transoptic 1 44923.6 340304.6 89027.6 8.8 0.0 0.6 52.5
Transoptic 2 43148.9 326341.4 85378.4 6.1 0.3 0.0 42.4
Varian 1 88726.9 537679.1 3873067.6 44173.8 77.4 1561.9 14268.6
Varian 2 15984.1 125548.3 865925.6 11518.3 13.0 381.4 2846.4

 

High Mass Resolution Scans Over Mass 32

In order to determine the relative abundance of Sulphur in the resins a high mass resolution scan was performed using a Cameca ims-1270 at Edinburgh University using a 5nA, Cs+ primary beam with a net impact energy of 20KeV. Low energy (40eV window) negative secondary ions were extracted and detected by an electron multiplier. The mass resolution was ~4000. High Mass Resolution Scans:

 

Discussion

  • The Konductomet, Probemet, Varain Torr Seal and the domestic Araldite all contain high and variable quantities of elements that could compromise the accuracy of a SIMS analysis and should therefore be avoided.
  • Petropoxy contains high F and B together with Na and certainly should be avoided if studying B isotopes.
  • Varian Torr Seal also contains high F and variable amounts of S.
  • Domestic rapid set Araldite contains an unacceptable level of S.
  • High Mass Resolution scans confirm that Specifix has high S content while Petropoxy contains P as shown by the 31PH mass displayed and high F as shown by the 13C+19F peak.
  • Only Transoptic has a low Cl content, the majority of the other resins contain high Cl concentrations that could compromise the accuracy of a SIMS analysis.