CRM Solutions

The ColdBlock system uses infrared radiation to rapidly digest metal alloy samples and a cooling block to condense out escaping vapors minimizing the loss of volatile elements.  Our preliminary results, detailed in a previous blog post (A New Sample Preparation Technique for  Metal Alloys), looked promising so we are now conducting validation studies with IARM CRM’s of various alloys.  This post details our validation study using CRM IARM 5I, a Grade 316 stainless steel alloy.

Digestion Procedure

5 separate 0.5g aliquots of CRM IARM 5I 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 15 minutes at 28% 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 below.  The reproducibility of each of the 5 digestions is very good, and the average values agree well with the certified values for all elements including Si and volatile elements such as As and S.     We will be posting the resuts of  validation studies on other alloys in the near future so subscribe to our blog to be sure you are automatically notified.

If you would like to learn more about this technology you can visit our product page Learn More

                                 Sample in Aqua regia at time = 0                                    

 

Diluted sample after 15 minutes of digestion time

 

IARM -5I Stainless Steel Grade 316
	Co	Standard Deviation			Ti	Standard Deviation
Run #1	0.18448	0.00409		Run #1	0.00215	0.00000
Run #2	0.18744	0.00597		Run #2	0.00179	0.00000
Run #3	0.18842	0.00343		Run #3	0.00189	0.00002
Run #4	0.18645	0.00282		Run #4	0.00194	0.00001
Run #5	0.18250	0.00651		Run #5	0.00191	0.00001
Average	0.18586	0.00456		Average	0.00194	0.00001
Certified Value	0.185+/-0.001			Certified Value	0.0025+/-0.0009
	Cr	Standard Deviation			Al	Standard Deviation
Run #1	16.7000	0.1963		Run #1	0.00454	0.00005
Run #2	16.6400	0.2765		Run #2	0.00447	0.00013
Run #3	16.5800	0.0735		Run #3	0.00462	0.00002
Run #4	16.6500	0.1091		Run #4	0.00454	0.00007
Run #5	16.4900	0.2255		Run #5	0.00447	0.00004
Average	16.6120	0.1762		Average	0.0045	0.00006
Certified Value	16.67+/-0.02			Certified Value	0.004+/-0.001
	Mo	Standard Deviation			As	Standard Deviation
Run #1	1.9820	0.0317		Run #1	0.00509	0.00000
Run #2	1.9840	0.0261		Run #2	0.00380	0.00000
Run #3	1.9930	0.0100		Run #3	0.00457	0.00000
Run #4	1.9830	0.0096		Run #4	0.00460	0.00000
Run #5	1.9830	0.0153		Run #5	0.00454	0.00000
Average	1.9850	0.0185		Average	0.00452	0.00000
Certified Value	2.027+/-0.003			Certified Value	0.006+/-0 .001
	Ni	Standard Deviation			V	Standard Deviation
Run #1	10.1300	0.1165		Run #1	0.06299	0.00028
Run #2	10.1200	0.1747		Run #2	0.06438	0.00031
Run #3	10.0400	0.0275		Run #3	0.06267	0.00035
Run #4	10.1200	0.0867		Run #4	0.06336	0.00027
Run #5	10.0200	0.1659		Run #5	0.06350	0.00019
Average	10.0860	0.1143		Average	0.06338	0.00028
Certified Value	10.04+/-0.03			Certified Value	0.064+/-0.002
avg	Mn	Standard Deviation			Si	Standard Deviation
Run #1	1.4430	0.0080		Run #1	0.44330	0.00323
Run #2	1.4680	0.0130		Run #2	0.45730	0.00050
Run #3	1.4550	0.0184		Run #3	0.43360	0.00350
Run #4	1.4410	0.0367		Run #4	0.42540	0.00041
Run #5	1.4520	0.0069		Run #5	0.41890	0.00098
Average	1.4518	0.0166		Average	0.43570	0.00173
Certified Value	1.443+/-0.009			Certified Value	0.433+/-0.004
	Cu	Standard Deviation			Nb	Standard Deviation
Run #1	0.48054	0.00005		Run #1	0.01405	0.00008
Run #2	0.48474	0.00005		Run #2	0.01434	0.00002
Run #3	0.47920	0.00005		Run #3	0.01394	0.00010
Run #4	0.48049	0.00005		Run #4	0.01422	0.00001
Run #5	0.48164	0.00005		Run #5	0.01467	0.00002
Average	0.48132	0.00005		Average	0.01424	0.00005
Certified Value	0.487+/-0.003			Certified Value	0.0133+/- 0.0009
	P	Standard Deviation
Run #1	0.02809	0.00019
Run #2	0.02916	0.00026
Run #3	0.02837	0.00030
Run #4	0.02814	0.00021
Run #5	0.02805	0.00019
Average	0.02836	0.00023
Certified Value	0.0279+/-0.0005

 

---