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EML-582

REPORT OF THE DEPARTMENT OF ENERGY, OFFICE OF ENVIRONMENTAL MANAGEMENT,

QUALITY ASSESSMENT PROGRAM, INORGANIC INTERCOMPARISON STUDY

Pamela D. Greenlaw 4

Environmental Measurements Laboratory U. S. Department of Energy New York, NY 10014-4811

July 1, 1996

DISCLAIMER

"This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do no1 necessarily state or reflect those of the United States Government or any agency thereof."

This report has been reproduced directly from the best available copy.

Available from the National Technical Information Service, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161.

Table of Contents

QAP 44 Soil lntercomparison Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ii

Aluminum (AL) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i

Arsenic(AS) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

Barium (BA) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ! . . . . . 3

Calcium (CA) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

Cadmium(CD) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

Chromium (CR) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

Copper(CU) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

lron(FE) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

Magnesium(MG) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

Manganese(MN) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Sodium(NA) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

Nickel(N1) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Vanadium0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

Zinc(ZN) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Participating Laboratories ..................................... 15

i

QAP 44 Soil Inorganic lntercomparison Study

Data for inorganic constituents of the QAP soil sample were collected as part of this distribution. This was a voluntary intercomparison study. The samples were analyzed for RCRA metals using methods 3050 and 3051 for digestion. Unfortunately the measured values for the elements varied with the digestion method. The value from the 3050 digestion seemed to be most comparable with the values reported by the other participants so that value was used for the statistical comparison with the participating laboratories. The microwave values are reported as well. We are planning to research the discrepancies between digestion methods and provide more information in the next QAP distribution.

ACKNOWLEGEMENT: The US Environmental Protection Agency Region I1 Technical Support Branch provided confirmatory analysis of the sample for EML.

ii

QAP 44 Results by Element

Identification Element Result Error Microwave HN03 m o w a v e HN03/HCI EML AL 7085.0 235.0 12850.0 14900.0 9603SOAG1 9603SOAR1 9603SOCH1 9603SODC1 9603SOES 1 9603SOFG1 9603SOGAI 9603SOHL1 9603SOIS 1 9603SOJP1 9603SOLAI 9603SOLA1 9603SOLA1 9603SOLH1 9603SONL1 9603SOOB1 9603SOOR1 9603SOSCl 9603SOSW1 9603SOSW1 9603SOSW1 9603SOUC1 9603SOUP1

AL AL AL AL AL AL AL AL AL AL AL AL AL AL AL AL A1 AL AL AL AL AL AL

7150.0 6200.0

12200.0 9200.0

48100.0 0.0

7580.0 7100.0 6940.0

41000.0 6424.0 8423.0 951 5.0 8360.0 5369.0 6900.0 9200.0 7760.0 6500.0 6560.0 6700.0

10782.0 7560.0

0.0 620.0

1220.0 920.0

0.0 4600.0

0.0 0.0 0.0

2000.0 206.0 281 .O 304.0

0.0 0.0 0.0

20.0 0.0 0.0 0.0 0.0

1078.2 0.0

Records printed: 24

Statistical Summary (excluding outliers as determined by KolmogorovSmimov Test) Mean 7786 Standard Deviation 1638 Median 71 50 15 percentile 6473 85 percentile 931 0 N 21

EML results were determined using SW846 method 3050 hotplate digestion with ICP or graphite furnace AA determination. The samples did not appear to totally digest using this method so closed vessel microwave digestion, method 3051, was used resulting in higher analyte recovery.

Page 1


Identification EML 9603SOAG1 9603SOARl 9603SOCH1 9603SODC1 9603SOESl 9603SOFG1 9603SOGA1 9603SO H L l 9603SOISl 9603SOJPI 9603SOLA1 9603SOLA1 9603SOLAl 9603SOLH1 9603SONA1 9603SONL1 9603SOOBl 9603SOSCl 9603SOSW 1 9603SOSW1 9603SOSWl 9603SOUCl

Element AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS AS

Result 2.4 2.8

16.0 2.4 3.0 5.9 2.3

18.5 I .9 3.0 4.0 2.2 2.5 2.5 2.2 3.8 0.0 2.3 2.4 q.5 1.6 1.6 1.3

Error Microwave HN03 Microwave HN03/HCI 0.1 2.3 0.0 1.6 0.2 0.3 0.0 0.0 0.0 0.0 0.0 0.2 0.5 0.5 1.4 0.0 0.0 2.0 0.0 0.0 0.0 0.0 0.0 0.1

Records printed: 23

Statistical Summary (excluding outliers as determined by Kolmogorov-Smimov Test) Mean 2.4 Standard Deviation 0.71 Median 2.4 15 percentile 1.6 85 percentile 2.7 N 19


Page 2

Identification EM1 9603SOAGl 9603SOARl 9603SOC H 1 9603SODCl 9603SOES1 9603SOFG1 9603SOGA1 9603SOHLl 9603SOISl 9603SOJP1 9603SOLA1 9603SOLA1 9603SOLA1 9603SOLHl 9603SONAl 9603SONLl 9603SOOB1 9603SOOR1 9603SOSCl 9603SOSWl

'9603SOSW1 9603SOSWl 9603SOUCl 9603SOUP 1

Records prinf

Page 3

---

Element BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA BA

:ed: 25


Result 60.5 60.7 54.0 69.1 70.0

229.0 46.0 59.5 60.0 62.8

190.0 56.0 66.2 72.0 67.5 82.9 51.7 60.0 71.1 63.1 59.2 59.6 60.7 73.4 66.3

1

Error Microwave HN03 Microwave HN03/HCI 0.5 84.5 106.5 0.0 5.4 6.9 7.0 0.0 0.0 0.0 0.0 0.0 0.0 7.0 8.3 2.0 0.0 0.0 0.0 0.0 0.3 0.0 0.0 0.0 0.0 7.3 0.0

Statistical Summary (excluding outliers as determined by Koimogorov-Smirnov Test) Mean 63.1 Standard Deviation 8.0 Median 60.7

85 percentile 71.1 N 23

15 percentile 55.9


Identification EML 9603SOAGl 9603SOARl 9603SOCHl 9603SODCl 9603SOES 1 9603SOFGl 9603SOGAl 9603SOHLl 9603SOIS 1 9603SOJPl 9603SOlA1 9603SOlA1 9603SOLA1 9603SOLHl 9603SONLl 9603SOOB1 9603SOOR1 9603SOSCl 9603SOSWl 9603SOSWl 9603SOSWl 9603SOUC1 9603SOUPl

Element CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA CA


Result 4050.0 4480.0 3900.0 4650.0 4400.0 61 00.0 4400.0 3850.0 4200.0 4640.0 5700.0 3871 .O 41 15.0 41 87.0 4670.0 3932.0 4000.0 4730.0 3950.0 4430.0 4450.0 4470.0 4073.0 471 0.0

1

Error Microwave HN03 Microwave HN03/HCI 30.0 3870.0 41 90.0 0.0

390.0 465.0 440.0

0.0 0.0 0.0 0.0 0.0

870.0 248.0 118.0 174.0

0.0 0.0 0.0 50.0 0.0 0.0 0.0 0.0

407.0 0.0

Records printed: 24

Statistical Summary (excluding outliers as determined by Kolmogorov-Smirnov Test) Mean 4280 Standard Deviation 301 Median 4300 15 percentile 3926 85 percentile 4654 N 22

EML results were determined using SW846 method 3050 hotplate digestion with ICP or graphite furnace AA determination. The samples did not appear to totally digest using this mlethod so closed vessel microwave digestion, method 3051, was used resulting in higher analyte remvery.

Page 4

Identification Element EML CD 9603SOAGl CD 9603SOARl CD 9603SOCHl CD 9603SODC1 CD 9603SOESl CD 9603SOFGl CD 9603SOGAl CD 9603SOHLl CD 9603SOIS1 CD 9603SOJPl CD 9603SOLA1 CD 9603SOLA1 CD 9603SOLA1 CD 9603SOLH1 CD 9603SONL1 CD

~9603SOOB1 CD 9603SOOR1 CD 9603SOSCl CD 9603SOSWl CD

Records printed: 20


Result <I 0.29 0 0.21 8 0.13 0.083 0 1.8 0.03 0 7 0.256 0.279 0.492 0.23 0 0

0 0.072

0.889

Error Microwave HN03 Microwave HN03/HCI <I <I

0.0 0.5

0.0

0.0 0.0

0.0 0.0

0. I 0.1 0.0 1 .o

0.2 0.0 0.0



Pagl e 5


Identification EM1 3603SOAG 1 3603SOAR1 3603SOCH1 3603SODC1 3603SOESl 3603SOFG1 3603SOGA1 3603SOHL1 3603SOIS 1 3603SOJP1 3603 SO LA 1 3603SO LA1 3603SOLA1 3603SOLH1 3603SONA1 3603SONL1 3603SOOB1 3603SOOR1 3603SOSC1 3603SOSW1 3603SOSW1 3603SOSW1 3603SOUC1 3603SOUP 1

Element CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR CR

Result 12.5 13.9 15.0 15.9 19.0 51.5 9.3

15.4 17.0 12.9 34.0 13.2 15.2 17.9 16.2 22.2 12.7 13.0 17.0 16.3 11.4 11.6 11.8 31 .O 14.5

3ecords printed: 25

Statistical Summary (excluding outliers as determined by Kolmogorov-Smirnov Test) Mean 14.7 Standard Deviation 2.9 Median 14.8 15 percentile 11.8 85 percentile 17.2 N 22

1

Error Microwave H N 0 3 Microwave HN03/HCI 0.5 18.5 21.5 0.0 1.5 1.6 1.9 0.0 0.0 0.0 0.0 0.0 I .o 2.1 2.4 6.9 0.0 0.0 0.0 0.0 0.2 0.0 0.0 0.0 0.0 3. I 0.0

EML results were determined using SW846 method 3050 hotplate digestion with ICP or graphite furnace PA determination. The samples did not appear to totally digest using this method so closed vessel microwave digestion, method 3051, was used resulting in higher analyte recovery.

Page 6


ldentificati on EML 9603SOAG1 9603SOAR1 9603SOCH1 9603SODC1 9603SOES1 9603SOFG1 9603SOGA1 9603SOHL1 9603SOISl 9603SOJP1 9603SOLAl 9603SOLAl 9603SOLA1 9603SONL1 9603SOOB1 9603SOOR1 9603SOSCl 9603SOSW1 9603SOSW1 9603SOSW1 9603SOUC1 9603SOU P 1

Element cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu cu

Result 9.5 8.8 9.0

14.9 11.0 7.1 6.4 8.0 8.6 8.0

300.0 6.9 7.6 7.9 6.0 8.0

10.0 8.3 8.1 8.3 8.4

10.7 9.4

Error Microwave HN03 m r o w a v e HNOYHCI 1.5 10.5 11.0 0.0 0.9 1.5 1.1 0.0 0.0 0.0 0.0 0.0 0.0 0.5 0.5 0.6 0.0 0.0 0.3 0.0 0.0 0.0 0.0 1.1 0.0

Records printed: 23


EML results were determined using SW846 method 3050 hotplate digestion with ICP or graphite furnace AA determination. The samples did not appear to totally digest using this method so closed vessel microwave digestion, method =I, was used resulting in higher analyte recovery.

Page 7 t

I ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! ! !

,;lentifcation Elemenl Result EML FE 11450.0 3603SOAGl FE 3603SOAR1 FE 9603SOCHl FE 3603SODC1 FE 3603SOES1 FE 3603SOFGl FE 3603SOGA1 FE 3603SOHL1 FE 3603SOIS1 FE 3603SOJP1 FE 3603SOLA1 FE 3603SOLA1 FE 3603SOLA1 FE 3603SOLH1 FE 3603SONL1 FE 3603SOOB1 FE 3603SOOR1 FE 3603SOSC1 FE 3603SOSW1 FE 3603SOSW1 FE 3603SOUCl FE 3603SOUP1 FE

Records printed: 23

13600.0 10000.0 14200.0 1 1900.0 13700.0 8100.0

101 00.0 12000.0 1 1900.0 15000.0 10238.0 11776.0 12320.0 I 2600.0 10750.0 12000.0 1301 0.0 1 1500.0 10800.0 1 1000.0 13074.0 I 1900.0

.-


Error 250.0

0.0 1000.0 1420.0

0.0 0.0 0.0 0.0 0.0 0.0

300.0 362.0 365.0 380.0

0.0 0.0 0.0

10.0 0.0 0.0 0.0

1307.4 0.0

Microwave HN03 Microwave HN03/HCI 14400.0 12750.0

t

I

Statistical Summary (excluding outliers as determined by Kolmogorov-Smimov Test) Mean 11866 Standard Deviation 1538 Median 1 1900 15 percentile 10231 85 percentile 13605 N 23


Page 8


2990.0 2600.0 3470.0

380.0 2140.0 2300.0 2790.0 3200.0 3120.0

12000.0 2780.0 3005.0 31 16.0 3290.0 2528.0 2700.0 3250.0 2940.0 2830.0 2850.0 3325.0 3290.0

Error Microwave HN03 mrowave HN03/HCI 5.0 3095.0 341 0.0 0.0

260.0 347.0 38.0 0.0 0.0 0.0 0.0 0.0

1 100.0 50.0 54.0 56.0 0.0 0.0 0.0 10.0 0.0 0.0 0.0

333.0 0.0



Idenj EML


fication Element Result MN 355.5

9603SOAG1 9603SOAR1 9603SOCH1 9603SODC1 9603SOES1 9603SOFG 1 9603SOGAl 9603SOHLl 9603SO IS I 9603SOJP1 9603SOLA1 9603SOLAl 9603SOLA1 9603SOLH I 9603SONL1 9603SOOB1 9603SOOR1 9603SOSC1 9603SOSW1 9603SOSW1 9603SOSWl 9603SOUC 1 9603SOUP1

MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN MN

380.0 340.0 390.0

3100.0 401 .O 280.0 338.0 380.0 370.0 430.0 317.0 338.0 350.0 366.0 342.0 350.0 372.0 353.0 369.0 371 .O 372.0 401 -0 406.0

Error 0.5 0.0

34.0 39.0

310.0 0.0 0.0 0.0 0.0 0.0 8.0

16.0 17.0 20.0 0.0 0.0 0.0 I .o 0.0 0.0 0.0 0.0

40.1 0.0

Microwave HN03 Microwave HN03/HCI 351 .O 372.0

Records printed: 24



Page I O

Identification EML 9603SOAG1 9603SOARl 9603SOCHl 9603SODC1 9603SOES1 9603SOFGl 9603SOGAl 9603SOHL1 9603SOISl 9603SOJP1 9603SOLA1 9603SOLA1 9603SOLAl 9603SON L1 9603SOOB 1 9603SOOR1 9603SOSC1 9603SOSWl 9603SOSWl 9603SOSWl 9603SOUC1

Element NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA

9603SOUPl NA

Records printed: 23


Result <500 234 290 450 340 5040 170 301 380 283 71 00 273 31 1 348 0 400 283 324 247 252 255 500 300

1

Error Microwave HN03 Microwave HN03IHCI <500 -600

0.0 29.0 45.0 34.0 0.0 0.0 0.0 0.0 0.0

50.0 32.0 37.0 41 .O

2000.0 0.0 1 .o 0.0 0.0 0.0 0.0

50.0 0.0

Statistical Summary (excluding outliers as determined by Kolmogorov-Smirnov Test) Mean 31 3 Standard Deviation 76 Median 300 15 percentile 250 85 percentile 390 N 19

EML results were determined using SW846 method 3050 hotplate digestion with ICP or graphite furnace AA determination. The samples did not appear to totally digest using this method so closed vessel microwave digestion, method 3051, was used resutting in higher analyte recovery.

Page 11


Identification EML 3603SOAG1 3603SOARl 3603SOCH1 3603SODCI 3603SOFGl 3603SOGA1 3603SOHL1 3603SOIS 1 3603SOJP1 3603SOLA1 3603SOLA1 3603SO LA 1 3603SOtH1 3603SON L I 3603SOOB1 3603SOOR1 3603SOSC1 3603SOSW1 3603SOSWl 3603SOSWl 3603SOUCl 3603SOUP1

Element NI NI NI NI NI NI NI NI NI NI NI NI NI Nt NI NI NI NI NI NI NI NI NI

Result 24.5 25.5 24.0 27.4 27.0 20.0 25.2 28.0 25.7 60.0 34.4 35.0 38.9 28.9 23.8 24.0 26.3 25.7 25.4 25.5 26. I 45.2 28.3

Error Microwave HN03 Microwave HN03/HCI 0.5 26.0 26.0 0.0 2.4 2.7 2.7 0.0 0.0 0.0 0.0 0.0 2.3 2.0 2.6 0.0 0.0 0.0 1.1 0.0 0.0 0.0 0.0 4.5 0.0

3ecords printed: 23

Statistical Summary (excluding outliers as determined by Kolmogorov-Smirnov Test) Mean 26.5 Standard Deviation 3.4 Median 25.7 15 percentile 24 85 percentile 28.6 N 20


Page 12


Identification Element EML V 9603SOAGl V 9603SOAR1 V 9603SOCH1 V 9603SODCl V 9603SOESl V 9603SOFG1 V 9603SOGA1 V 9603SOHL1 V 9603SOISl V 9603SOJP1 V 9603SOLA1 V 9603SOLA1 V 9603SOlA1 V 9603SOLHl V 9603SONL1 V 9603SOOB1 V 9603SOOR1 V 9603SOSCl V 9603SOSWl V 9603SOSWl V 9603SOSWl V 9603SOUC1 V 9603SOUP1 V

Result 8.0 9.0 7.2

10.2 11.0 19.0 5.8

10.5 9.3 6.5

34.0 6.8 9.7

10.4 10.0 0.0 8.0

10.7 9.1 7.9 8.6 8.9

34.4 9.3

b

Error Microwave HN03 mrowave HN03/HCI 0.0 14.5 18.5 0.0 0.7 1 .o 1.1 0.0 0.0 0.0 0.0 0.0 2.9 1.5 2.1 0.6 0.0

10.0 0.0 0.2 0.0 0.0 0.0 0.0 3.4 0.0

Records printed: 24



Page 13

---


Identification EML 9603SOAG1 9603SOAR1 9603SOCH 1 9603SODC1 9603SOES1 9603SOFG1 9603SOGA1 9603SOHL 1 9603SOlSl 9603SOJP1 9603SOLAl 9603SOLAl 9603SOLAl 9603SOLH1 9603SONA1 9603SONL1 9603SOOB1 9603SOORI 9603SOSC1 9603SOSW1 9603SOSW1 9603SOSW1 9603SOUC1 9603SOUP1

Element ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN ZN

Result 33.0 35.2 33.0 44.0 35.0 32.7 25.0 33.7 38.0 34.0 35.0 36.6 39.4 39.8 38.0 45.0 30.2 33.0 41 .O 35.2 33.9 33.8 34.7 42.5 38. 1

Error Microwave HN03 Microwave HN03/HCI 0.0 35.5 35.0 0.0 3.3 4.4 3.5 0.0 0.0 0.0 0.0 0.0 3.0 1.6 1.7 9.3 0.0 0.0 0.0 0.0 0.5 0.0 0.0 0.0 0.0 4.3 0.0

Records printed: 25



Page 14

Participating Laboratories in EM1 QAP44

laboratories Reporting Data

Code

AG AR CH DC ES FG GA H l IS JP LA LH N A N l OB OR sc sw uc UP

Total Reporting labs: 20

laboratory Name

Paragon Analytics, Inc., Fort Collins, CO Accu-Labs Research Inc., Golden, GO California State Dept. Health Senr. Sanitation & Radiation Laborat, Berkeley, CA Datachem Laboratories, Salt Lake City, UT Environmental Sci. & Engr., Inc. Inorganic Analyt.Chem., Gainesville, FL FGL Environmental, Santa Paula, CA Lockheed Martin Rm. 333 Bldg X710, Pikton, OH Heritage Laboratories, Inc. , Romeoville, IL Quanterra St. Louis , Earth City, MO Japan Chemical Analysis Center 295-3 Sanno-Cho, Chiba 263, Japan Analytical Services, CST-3 MS K484, Los Alamos, NM Lockheed Analytical Laboratory, Las Vegas, NV USEPA NAREL , Montgomery, A1 FERMCO BLDG 15, room C-11, Cincinnati, OH OBG Laboratories, East Syracuse, NY Oak Ridge National Lab Bldg 4500-N Rm G-5, Oak Ridge, TN S-3 Division Maxwell Labs, La Jolla, CA Southwest Research Institute, Div. 01 P.O. Drawer 28510, San Antonio, TX Lockheed Martin RM 60 BLDG C-710, Paducah, KY Y-12 Plant, ASO, QC Laboratory 113C Union Valley Road, Oak Ridge, TN

15

Environmental MIsasurements Laboratory U. S. Department of Energy 201 Varick Street New York, New York 10014-481 1 U. S. A.

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