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 | |||
