CRM Solutions

A Method for Preparing Aluminum Alloys for Analysis by ICP using Infrared Digestion Technology

[fa icon="calendar"] Apr 5, 2018 4:24:44 PM / by Mitchell Planty

Mitchell Planty

 

The ColdBlock digestion system is a unique instrument  capable of rapidly dissolving materials for analysis by ICP.  The system uses infrared radiation to speed up  the digestion process and a cooling block  to condense escaping vapor.   In previous posts  described methods for digesting  316 Stainless Steel and 718 Nickel alloy using this sample preparation system.   In this post we present a method for digesting Aluminum 2024 alloy.

The  digestion method presented was validated using five replicate digestions of a certified reference material and then analyzed using an ICP-OES.

 Digestion Procedure

 5 separate 0.5g aliquots of CRM IARM 104A were prepared using 20mL of aqua regia in a quartz digestion tube.  The 5 digestion vessels were loaded into a 6 position ColdBlock digestion system and digested for 10 minutes at 30% power. The digested samples were diluted to a total volume of 50ml using deionized water and transferred to a centrifuge tube.  1 ml of HF was then added to each centrifuge tube to stabilize the solution. The samples were then analyzed on a Spectro Arcos ICP-OES in our laboratory.  The results are detailed in the table below.  The reproducibility of the replicate digestions was excellent and the average values agree well with the certified concentrations.

The total sample preparation time for each sample including weighing, digestion and dilution was only 15 minutes.    

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 IARM 104A - Aluminum 2024
Values in %
  Bi       Cr  
Sample 1 0.0154     Sample 1 0.0163  
Sample 2 0.0151     Sample 2 0.0158  
Sample 3 0.0156     Sample 3 0.0160  
Sample 4 0.0151     Sample 4 0.0170  
Sample 5 0.0151     Sample 5 0.0174  
Average 0.0153     Average 0.0165  
Standard Deviation 0.0002     Standard Deviation 0.0007  
Certified Value 0.015 ± 0.0046   Certified Value 0.016 ± 0.0022
             
  Cu       Fe  
Sample 1 4.7229     Sample 1 0.2522  
Sample 2 4.5694     Sample 2 0.2477  
Sample 3 4.6889     Sample 3 0.2529  
Sample 4 4.6471     Sample 4 0.2529  
Sample 5 4.6773     Sample 5 0.2634  
Average 4.6611     Average 0.2538  
Standard Deviation 0.0580     Standard Deviation 0.0058  
Certified Value 4.66 ± 0.0752   Certified Value 0.25 ± 0.0092
             
  Mg       Mn  
Sample 1 1.6627     Sample 1 0.6566  
Sample 2 1.6372     Sample 2 0.6644  
Sample 3 1.7009     Sample 3 0.6680  
Sample 4 1.6561     Sample 4 0.6633  
Sample 5 1.6497     Sample 5 0.6635  
Average 1.6613     Average 0.6631  
Standard Deviation 0.0240     Standard Deviation 0.0041  
Certified Value 1.65 ± 0.0536   Certified Value 0.65 ± 0.0122
             
  Ni       Pb  
Sample 1 0.0300     Sample 1 0.0241  
Sample 2 0.0297     Sample 2 0.0238  
Sample 3 0.0303     Sample 3 0.0249  
Sample 4 0.0306     Sample 4 0.0245  
Sample 5 0.0300     Sample 5 0.0240  
Average 0.0301     Average 0.0243  
Standard Deviation 0.0004     Standard Deviation 0.0004  
Certified Value 0.03 ± 0.0027   Certified Value 0.025 ± 0.0025
             
  Si       Sn  
Sample 1 0.3055     Sample 1 0.0196  
Sample 2 0.3004     Sample 2 0.0196  
Sample 3 0.3089     Sample 3 0.0202  
Sample 4 0.3097     Sample 4 0.0201  
Sample 5 0.3091     Sample 5 0.0202  
Average 0.3067     Average 0.0200  
Standard Deviation 0.0039     Standard Deviation 0.0003  
Certified Value 0.31 ± 0.0150   Certified Value 0.020 ± 0.0033
             
  Ti       V  
Sample 1 0.0308     Sample 1 0.0101  
Sample 2 0.0310     Sample 2 0.0103  
Sample 3 0.0309     Sample 3 0.0104  
Sample 4 0.0306     Sample 4 0.0103  
Sample 5 0.0307     Sample 5 0.0102  
Average 0.0308     Average 0.0103  
Standard Deviation 0.0002     Standard Deviation 0.0001  
Certified Value 0.030 ± 0.0002   Certified Value 0.01 ± 0.0019
             
  Zn       Zr  
Sample 1 0.0170     Sample 1 0.0123  
Sample 2 0.0170     Sample 2 0.0117  
Sample 3 0.0171     Sample 3 0.0124  
Sample 4 0.0171     Sample 4 0.0118  
Sample 5 0.0169     Sample 5 0.0119  
Average 0.0170     Average 0.0120  
Standard Deviation 0.00006     Standard Deviation 0.0003  
Certified Value 0.017 ± 0.0042   Certified Value 0.012 ± 0.0018
              

Topics: icp sample preparation, coldBlock, aluminum Alloys, Sample Preparation

Mitchell Planty

Written by Mitchell Planty

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