Final Notes July 9, 2010

Steam Study Data Review Notes

Standard Operating Procedure (SOP) for Inductively Coupled Plasma Mass 

Spectrometry for Trace Element Analysis in Flue Gas Desulfurization 

Wastewaters

1. For the determination of total elements, the sample should acidified at the laboratory with 

1 to 1 nitric acid to a pH less than 2 within two weeks of collection (200.8/8.3).

2. After acidification, the sample should be mixed and allowed to sit for 16 hours, and then 

confirmed to have a pH less than 2. If the pH was greater than or equal to 2 the sample 

should be acidified, mixed, held for 16 hours, and tested again (200.8/8.3).

3. An aliquot of all samples should be acidified with nitric acid and hydrochloric acid and 

digested using the closed vessel digestion techniques outlined in Section 10.2 of the FGD 

SOP. If reported, indicate the amount of nitric and hydrochloric acids used in digestion

and note any deviations reported in the lab’s digestion procedures. Note: The lab should 

use 0.5 mL of concentrated nitric acid and 0.25 mL of hydrochloric acid.

4. *For FGD influent samples that contain greater than 1% suspended solids, the laboratory 

should separate the solid and liquid portions of the sample and analyze each portion 

separately. 

5. Before initiating analysis and every year thereafter, the linear range for each analyte of 

interest should be established. If reported, note if the results of the analysis were within 

10% of the actual value (FGD SOP/9.5). If reported, indicate the LDRs reported by the 

lab and the date the LDRs were done.

6. Before initiating analysis and at least every 3 months all individual interference check 

solutions specified in Section 7.2.6 of the FGD SOP should be analyzed. If reported, were 

all results for elements of interest < the RL unless the presence of an element can be 

confirmed and in this case was the result < 5 times the RL? (FGD SOP/ 9.3) 

7. The system should be washed with a rinse blank for ≥ 30 seconds between the analysis of 

every sample and standard (FGD SOP/10.4.2). If reported, indicate how many rinse 

blanks were run and any contamination noted.

8. *For aqueous samples, a field blank should be prepared and analyzed at each sample 

point during one of the four days of sample collection. If the analyte concentration was 

greater than the MDL, indicate the concentration.

9. All masses that could influence results should be monitored for each run and this 

information should be used by the laboratory to correct data for interferences (FGD 

SOP/10.4.3).
Steam Study Data Review Notes

Standard Operating Procedures for Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

Page 2 of 2

Final Notes July 9, 2010

10. *If the analyte concentration in a sample was less than 5 times the analyte concentration 

in the laboratory reagent blank, the result should be reported as a nondetect. List all 

affected samples:

11. *If the analyte concentration in a sample was less than 10 times but greater than 5 times 

the analyte concentration in the laboratory reagent blank, the result should be reported as 

an estimated value. List all affected samples: