Loading (50 kb)...'
(continued)
Note: 4. In place of filtering, the sample after diluting and mixing may be centrifuged or allowed to settle by gravity overnight to remove insoluble material.
9.3 For the determination of total elements, choose a measured volume of the well mixed acid preserved sample appropriate for the expected level of elements and transfer to a Griffin beaker. (See Note 5.) Add 3 mL of conc. HNO3. Place the beaker on a hot plate and evaporate to near dryness cautiously, making certain that the sample does not boil and that no area of the bottom of the beaker is allowed to go dry. Cool the beaker and add another 5 mL portion of conc. HNO3. Cover the beaker with a watch glass and return to the hot plate. Increase the temperature of the hot plate so that a gently reflux action occurs. Continue heating, adding additional acid as necessary, until the digestion is complete (generally indicated when the digestate is light in color or does not change in appearance with continued refluxing.) Again, evaporate to near dryness and cool the beaker. Add 10 mL of 1+1 HCl and 15 mL of deionized, distilled water per 100 mL of final solution and warm the beaker gently for 15 min. to dissolve any precipitate or residue resulting from evaporation. Allow to cool, wash down the beaker walls and watch glass with deionized distilled water and filter the sample to remove insoluble material that could clog the nebulizer. (See Note 4.) Adjust the sample to a predetermined volume based on the expected concentrations of elements present. The sample is now ready for analysis (See Note 6). Concentrations so determined shall be reported as “total.”
Note: 5. If low determinations of boron are critical, quartz glassware should be used.
Note: 6. If the sample analysis solution has a different acid concentration from that given in 9.4, but does not introduce a physical interference or affect the analytical result, the same calibration standards may be used.
9.4 For the determination of total recoverable elements, choose a measured volume of a well mixed, acid preserved sample appropriate for the expected level of elements and transfer to a Griffin beaker. (See Note 5.) Add 2 mL of (1+1) HNO3 and 10 mL of (1+1) HCl to the sample and heat on a steam bath or hot plate until the volume has been reduced to near 25 mL making certain the sample does not boil. After this treatment, cool the sample and filter to remove insoluble material that could clog the nebulizer. (See Note 4.) Adjust the volume to 100 mL and mix. The sample is now ready for analysis. Concentrations so determined shall be reported as “total.”
10. Procedure
10.1 Set up instrument with proper operating parameters established in Section 6.2. The instrument must be allowed to become thermally stable before beginning. This usually requires at least 30 min. of operation prior to calibration.
10.2 Initiate appropriate operating configuration of computer.
10.3 Profile and calibrate instrument according to instrument manufacturer's recommended procedures, using the typical mixed calibration standard solutions described in Section 7.4. Flush the system with the calibration blank (7.5.1) between each standard. (See Note 7.) (The use of the average intensity of multiple exposures for both standardization and sample analysis has been found to reduce random error.)
Note: 7. For boron concentrations greater than 500 µg/L extended flush times of 1 to 2 minutes may be required.
10.4 Before beginning the sample run, reanalyze the highest mixed calibration standard as if it were a sample. Concentration values obtained should not deviate from the actual values by more than ±5 percent (or the established control limits whichever is lower). If they do, follow the recommendations of the instrument manufacturer to correct for this condition.
10.5 Begin the sample run flushing the system with the calibration blank solution (7.5.1) between each sample. (See Note 7.) Analyze the instrument check standard (7.6.1) and the calibration blank (7.5.1) each 10 samples.
10.6 If it has been found that methods of standard addition are required, the following procedure is recommended.
10.6.1 The standard addition technique (14.2) involves preparing new standards in the sample matrix by adding known amounts of standard to one or more aliquots of the processed sample solution. This technique compensates for a sample constitutent that enhances or depresses the analyte signal thus producing a different slope from that of the calibration standards. It will not correct for additive interference which causes a baseline shift. The simplest version of this technique is the single-addition method. The procedure is as follows. Two identical aliquots of the sample solution, each of volume VX, are taken. To the first (labeled A) is added a small volume Vs of a standard analyte solution of concentration cs. To the second (labeled B) is added the same volume Vs of the solvent. The analytical signals of A and B are measured and corrected for nonanalyte signals. The unknown sample concentration cX is calculated:
where SA and SB are the analytical signals (corrected for the blank) of solutions A and B, respectively. Vs and cs should be chosen so that SA is roughly twice SB on the average. It is best if Vs is made much less than VX, and thus cs is much greater than cX, to avoid excess dilution of the sample matrix. If a separation or concentration step is used, the additions are best made first and carried through the entire procedure. For the results from this technique to be valid, the following limitations must be taken into consideration:
1. The analytical curve must be linear.
2. The chemical form of the analyte added must respond the same as the analyte in the sample.
3. The interference effect must be constant over the working range of concern.
4. The signal must be corrected for any additive interference.
11. Calculation
11.1 Reagent blanks (7.5.2) should be subtracted from all samples. This is particularly important for digested samples requiring large quantities of acids to complete the digestion.
11.2 If dilutions were performed, the appropriate factor must be applied to sample values.
11.3 Data should be rounded to the thousandth place and all results should be reported in mg/L up to three significant figures.
12. Quality Control (Instrumental)
12.1 Check the instrument standardization by analyzing appropriate quality control check standards as follow:
12.1.1 Analyze and appropriate instrument check standard (7.6.1) containing the elements of interest at a frequency of 10%. This check standard is used to determine instrument drift. If agreement is not within ±5% of the expected values or within the established control limits, whichever is lower, the analysis is out of control. The analysis should be terminated, the problem corrected, and the instrument recalibrated.
Analyze the calibration blank (7.5.1) at a frequency of 10%. The result should be within the established control limits of 2 standard deviations of the meal value. If not, repeat the analysis two more times and average the three results. If the average is not wihin the control limit, terminate the analysis, correct the problem and recalibrate the instrument.
12.1.2 To verify interelement and background correction factors analyze the interference check sample (7.6.2) at the beginning, end, and at periodic intervals throughout the sample run. Results should fall within the established control limits of 1.5 times the standard deviation of the mean value. If not, terminate the analysis, correct the problem and recalibrate the instrument.
12.1.3 A quality control sample (7.6.3) obtained from an outside source must first be used for the initial verification of the calibration standards. A fresh dilution of this sample shall be analyzed every week thereafter to monitor their stability. If the results are not within ±5% of the true value listed for the control sample, prepare a new calibration standard and recalibrate the instrument. If this does not correct the problem, prepare a new stock standard and a new calibration standard and repeat the calibration.
13. Precision and Accuracy
13.1 An interlaboratory study of metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of the twenty-five elements listed in Table 4 were added to reagent water, surface water, drinking water and three effluents. These samples were digested by both the total digestion procedure (9.3) and the total recoverable procedure (9.4). Results for both digestions for the twenty-five elements in reagent water are given in Table 4; results for the other matrices can be found in Reference 14.10.
14. References
14.1 Winge, R.K., V.J. Peterson, and V.A. Fassel, “Inductively Coupled Plasma-Atomic Emission Spectroscopy: Prominent Lines, EPA–600/4–79–017.
14.2 Winefordner, J.D., “Trace Analysis: Spectroscopic Methods for Elements,” Chemical Analysis, Vol, 46, pp. 41–42.
14.3 Handbook for Analytical Quality Control in Water and Wastewater Laboratories, EPA–600/4–79–019.
14.4 Garbarino, J.R. and Taylor, H.E., “An Inductively-Coupled Plasma Atomic Emission Spectrometric Method for Routine Water Quality Testing,” Applied Spectroscopy 33, No. 3 (1979).
14.5 “Methods for Chemical Analysis of Water and Wastes,” EPA–600/4–79–020.
14.6 Annual Book of ASTM Standards, Part 31.
14.7 “Carcinogens—Working With Carcinogens,” Department of Health, Education, and Welfare, Public Health Service, Center for Disease Control, National Institute for Occupational Safety and Health, Publication No. 77–206, August 1977.
14.8 “OSHA Safety and Health Standards, General Industry,” (29 CFR Part 1910), Occupational Safety and Health Administration, OSHA 2206, (Revised, January 1976).
14.9 “Safety in Academic Chemistry Laboratories, American Chemical Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
14.10 Maxfield R. and Minak B., “EPA Method Study 27, Method 200.7 Trace Metals by ICP,” National Technical Information Service, Order No. PB 85–248–656, November 1983.
Table 1_Recommended Wavelengths \1\ and Estimated Instrumental Detection
Limits
------------------------------------------------------------------------
Estimated
detection
Element Wavelength, limit,
nm µg/L
2
------------------------------------------------------------------------
Aluminum....................................... 308.215 45
Arsenic........................................ 193.696 53
Antimony....................................... 206.833 32
Barium......................................... 455.403 2
Beryllium...................................... 313.042 0.3
Boron.......................................... 249.773 5
Cadmium........................................ 226.502 4
Calcium........................................ 317.933 10
Chromium....................................... 267.716 7
Cobalt......................................... 228.616 7
Copper......................................... 324.754 6
Iron........................................... 259.940 7
Lead........................................... 220.353 42
Magnesium...................................... 279.079 30
Manganese...................................... 257.610 2
Molybdenum..................................... 202.030 8
Nickel......................................... 231.604 15
Potassium...................................... 766.491 3
Selenium....................................... 196.026 75
Silica (SiO2).................................. 288.158 58
Silver......................................... 328.068 7
Sodium......................................... 588.995 29
Thallium....................................... 190.864 40
Vanadium....................................... 292.402 8
Zinc........................................... 213.856 2
------------------------------------------------------------------------
\1\The wavelengths listed are recommended because of their sensitivity
and overall acceptance. Other wavelengths may be substituted if they
can provide the needed sensitivity and are treated with the same
corrective techniques for spectral interference. (See 5.1.1).
\2\The estimated instrumental detection limits as shown are taken from
``Inductively Coupled Plasma-Atomic Emission Spectroscopy-Prominent
Lines,'' EPA-600/4-79-017. They are given as a guide for an
instrumental limit. The actual method detection limits are sample
dependent and may vary as the sample matrix varies.
\3\Highly dependent on operating conditions and plasma position.
Table 1_Analyte Concentration Equivalents (mg/L) Arising From Interferents at the 100 mg/L Level
--------------------------------------------------------------------------------------------------------------------------------------------------------
Interferent_
Analyte Wavelength, -----------------------------------------------------------------------
nm A1 Ca Cr Cu Fe Mg Mn Ni Ti V
--------------------------------------------------------------------------------------------------------------------------------------------------------
Aluminum........................................................... 308.214 ..... ..... ..... ..... ...... ...... 0.21 ..... ..... 1.4
Antimony........................................................... 206.833 0.47 ..... 2.9 ..... 0.08 ...... ..... ..... 0.25 0.45
Arsenic............................................................ 193.696 1.3 ..... 0.44 ..... ...... ...... ..... ..... ..... 1.1
Barium............................................................. 455.403 ..... ..... ..... ..... ...... ...... ..... ..... ..... .....
Beryllium.......................................................... 313.042 ..... ..... ..... ..... ...... ...... ..... ..... 0.04 0.05
Boron.............................................................. 249.773 0.04 ..... ..... ..... 0.32 ...... ..... ..... ..... .....
Cadmium............................................................ 226.502 ..... ..... ..... ..... 0.03 ...... ..... 0.02 ..... .....
Calcium............................................................ 317.933 ..... ..... 0.08 ..... 0.01 0.01 0.04 ..... 0.03 0.03
Chromium........................................................... 267.716 ..... ..... ..... ..... 0.003 ...... 0.04 ..... ..... 0.04
Cobalt............................................................. 228.616 ..... ..... 0.03 ..... 0.005 ...... ..... 0.03 0.15 .....
Copper............................................................. 324.754 ..... ..... ..... ..... 0.003 ...... ..... ..... 0.05 0.02
Iron............................................................... 259.940 ..... ..... ..... ..... ...... ...... 0.12 ..... ..... .....
Lead............................................................... 220.353 0.17 ..... ..... ..... ...... ...... ..... ..... ..... .....
Magnesium.......................................................... 279.079 ..... 0.02 0.11 ..... 0.13 ...... 0.25 ..... 0.07 0.12
Manganese.......................................................... 257.610 0.005 ..... 0.01 ..... 0.002 0.002 ..... ..... ..... .....
Molybdenum......................................................... 202.030 0.05 ..... ..... ..... 0.03 ...... ..... ..... ..... .....
Nickel............................................................. 231.604 ..... ..... ..... ..... ...... ...... ..... ..... ..... .....
Selenium........................................................... 196.026 0.23 ..... ..... ..... 0.09 ...... ..... ..... ..... .....
Silicon............................................................ 288.158 ..... ..... 0.07 ..... ...... ...... ..... ..... ..... 0.01
Sodium............................................................. 588.995 ..... ..... ..... ..... ...... ...... ..... ..... 0.08 .....
Thallium........................................................... 190.864 0.30 ..... ..... ..... ...... ...... ..... ..... ..... .....
Vanadium........................................................... 292.402 ..... ..... 0.05 ..... 0.005 ...... ..... ..... 0.02 .....
Zinc............................................................... 213.856 ..... ..... ..... 0.14 ...... ...... ..... 0.29 ..... .....
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 3_Interferent and Analyte Elemental Concentrations Used for Interference Measuremelts in Table 2
----------------------------------------------------------------------------------------------------------------
Analytes (mg/L) Interferents (mg/L)
----------------------------------------------------------------------------------------------------------------
Al.................. 10 ......... Al.................. 1,000 .................
AS.................. 10 ......... Ca.................. 1,000 .................
B................... 10 ......... Cr.................. 200 .................
Ba.................. 1 ......... Cu.................. 200 .................
Be.................. 1 ......... Fe.................. 1,000 .................
Ca.................. 1 ......... Mg.................. 1,000 .................
Cd.................. 10 ......... Mn.................. 200 .................
Co.................. 1 ......... Ni.................. 200
Cr.................. 1 ......... Ti.................. 200
Cu.................. 1 ......... V................... 200 .................
Fe.................. 1
Mg.................. 1
Mn.................. 1
Mo.................. 10
Na.................. 10
Ni.................. 10
Pb.................. 10
Sb.................. 10
Se.................. 10
Si.................. 1
Tl.................. 10
V................... 1
Zn.................. 10
----------------------------------------------------------------------------------------------------------------
Table 4_ICP Precision and Recovery Data
----------------------------------------------------------------------------------------------------------------
Concentration Total digestion (9.3) Recoverable digestion
Analyte µg/L µg/L (9.4) µg/L
----------------------------------------------------------------------------------------------------------------
Aluminum...................................... 69-4792 X=0.9273(C)+3.6 X=0.9380(C)+22.1
................ S=0.0559(X)+18.6 S=0.0873(X)+31.7
................ SR=0.0507(X)+3.5 SR=0.0481(X)+18.8
Antimony...................................... 77-1406 X=0.7940(C)-17.0 X=0.8908(C)+0.9
................ S=0.1556(X)-0.6 S=0.0982(X)+8.3
................ SR=0.1081(X)+3.9 SR=0.0682(X)+2.5
Arsenic....................................... 69-1887 X=1.0437(C)-12.2 X=1.0175(C)+3.9
................ S=0.1239(X)+2.4 S=0.1288(X)+6.1
................ SR=0.0874(X)+6.4 SR=0.0643(X)+10.3
Barium........................................ 9-377 X=0.7683(C)+0.47 X=0.8380(C)+1.68
................ S=0.1819(X)+2.78 S=0.2540(X)+0.30
................ SR=0.1285(X)+2.55 SR=0.0826(X)+3.54
Beryllium..................................... 3-1906 X=0.9629(C)+0.05 X=1.0177(C)-0.55
................ S=0.0136(X)+0.95 S=0.0359(X)+0.90
................ SR=0.0203(X)-0.07 SR=0.0445(X)-0.10
Boron......................................... 19-5189 X=0.8807(C)+9.0 X=0.9676(C)+18.7
................ S=0.1150(X)+14.1 S=0.1320(X)+16.0
................ SR=0.0742(X)+23.2 SR=0.0743(X)+21.1
Cadmium....................................... 9-1943 X=0.9874(C)-0.18 X=1.0137(C)-0.65
................ S=0.557(X)+2.02 S=0.0585(X)+1.15
................ SR=0.0300(X)+0.94 SR=0.332(X)+0.90
Calcium....................................... 17-47170 X=0.9182(C)-2.6 X=0.9658(C)+0.8
................ S=0.1228(X)+10.1 S=0.0917(X)+6.9
................ SR=0.0189(X)+3.7 SR=0.0327(X)+10.1
Chromium...................................... 13-1406 X=0.9544(C)+3.1 X=1.0049(C)-1.2
................ S=0.0499(X)+4.4 S=0.0698(X)+2.8
................ SR=0.0009(X)+7.9 SR=0.0571(X)+1.0
Cobalt........................................ 17-2340 X=0.9209(C)-4.5 X=0.9278(C)-1.5
................ S=0.0436(X)+3.8 S=0.0498(X)+2.6
................ SR=0.0428(X)+0.5 SR=0.0407(X)+0.4
Copper........................................ 8-1887 X=0.9297(C)-0.30 X=0.9647(C)-3.64
................ S=0.0442(X)+2.85 S=0.0497(X)+2.28
................ SR=0.0128(X)+2.53 SR=0.0406(X)+0.96
Iron.......................................... 13-9359 X=0.8829(C)+7.0 X=0.9830(C)+5.7
................ S=0.0683(X)+11.5 S=0.1024(X)+13.0
................ SR=0.0046(X)+10.0 SR=0.0790(X)+11.5
Lead.......................................... 42-4717 X=0.9699(C)-2.2 X=1.0056(C)+4.1
................ S=0.0558(X)+7.0 S=0.0779(X)+4.6
................ SR=0.0353(X)+3.6 SR=0.0448(X)+3.5
Magnesium..................................... 34-13868 X=0.9881(C)-1.1 X=0.9879(C)+2.2
................ S=0.0607(C)+11.6 S=0.0564(X)+13.2
................ SR=0.0298(X)+0.6 SR=0.0268(X)+8.1
Manganese..................................... 4-1887 X=0.9417(C)+0.13 X=0.9725(C)+0.07
................ S=0.0324(X)+0.88 S=0.0557(X)+0.76
................ SR=0.0153(X)+0.91 SR=0.0400(X)+0.82
Molybdenum.................................... 17-1830 X=0.9682(C)+0.1 X=0.9707(C)-2.3
................ S=0.0618(X)+1.6 S=0.0811(X)+3.8
................ SR=0.0371(X)+2.2 SR=0.0529(X)+2.1
Nickel........................................ 17-47170 X=0.9508(C)+0.4 X=0.9869(C)+1.5
................ S=0.0604(X)+4.4 S=0.0526(X)+5.5
................ SR=0.0425(X)+3.6 SR=0.0393(X)+2.2
Potassium..................................... 347-14151 X=0.8669(C)-36.4 X=0.9355(C)-183.1
................ S=0.0934(X)+77.8 S=0.0481(X)+177.2
................ SR=0.0099(X)+144.2 SR=0.0329(X)+60.9
Selenium...................................... 69-1415 X=0.9363(C)-2.5 X=0.9737(C)-1.0
................ S=0.0855(X)+17.8 S=0.1523(X)+7.8
................ SR=0.0284(X)+9.3 SR=0.0443(X)+6.6
Silicon....................................... 189-9434 X=0.5742(C)-35.6 X=0.9737(C)-60.8
................ S=0.4160(X)+37.8 S=0.3288(X)+46.0
................ SR=0.1987(X)+8.4 SR=0.2133(X)+22.6
Silver........................................ 8-189 X=0.4466(C)+5.07 X=0.3987(C)+8.25
................ S=0.5055(X)-3.05 S=0.5478(X)-3.93
................ SR=0.2086(X)-1.74 SR=0.1836(X)-0.27
Sodium........................................ 35-47170 X=0.9581(C)+39.6 X=1.0526(C)+26.7
................ S=0.2097(X)+33.0 S=0.1473(X)+27.4
................ SR=0.0280(X)+105.8 SR=0.0884(X)+50.5
Thallium...................................... 79-1434 X=0.9020(C)-7.3 X=0.9238(C)+5.5
................ S=0.1004(X)+18.3 S=0.2156(X)+5.7
................ SR=0.0364(X)+11.5 SR=0.0106(X)+48.0
Vanadium...................................... 13-4698 X=0.9615(C)-2.0 X=0.9551(C)+0.4
................ S=0.0618(X)+1.7 S=0.0927(X)+1.6
................ SR=0.0220(X)+0.7 SR=0.0472(X)+0.5
Zinc.......................................... 7-7076 X=0.9356(C)-0.30 X=0.9500(C)+1.82
................ S=0.0914(X)+3.75 S=0.0597(X)+6.50
................ SR=0.0130(X)+10.7 SR=0.0153(X)+7.78
----------------------------------------------------------------------------------------------------------------
AAAAAX=Mean Recovery, µg/L
AAAAAC=True Value for the Concentration, µg/L
AAAAAS=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
[49 FR 43431, Oct. 26, 1984; 50 FR 695, 696, Jan. 4, 1985, as amended at 51 FR 23703, June 30, 1986; 55 FR 33440, Aug. 15, 1990]
Appendix D to Part 136—Precision and Recovery Statements for Methods for Measuring Metals
top
Twenty-eight selected methods from “Methods for Chemical Analysis of Water and Wastes,” EPA–600/4–79–020 (1979) have been subjected to interlaboratory method validation studies. The following precision and recovery statements are presented in this appendix and incorporated into part 136:
Method 202.1
For Aluminum, Method 202.1 (Atomic Absorption, Direct Aspiration) replace the Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in water by Atomic Absorption Spectroscopy (Direction Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For a concentration range of 500–1200 µg/L
X=0.979(C)+6.16
S=0.066(X)+125
SR=0.086(X)+40.5
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 206.4
For Arsenic, Method 206.4 (Spectrophotometric-SDDC) add the following to the Precision and Accuracy Section:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For a concentration range of 20–292 µg/L
X=0.850(C)-0.25
S=0.198(X)+5.93
SR=0.122(X)+3.10
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 213.1
For Cadmium, Method 213.1 (Atomic Absorption, Direct Aspiration) replace the Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For a concentration range of 14–78 µg/L
X=0.919(C)+2.97
S=0.108(X)+5.08
SR=0.120(X)+0.89
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 218.1
For Chromium, Method 218.1 (Atomic Absorption, Direct Aspiration) replace the Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June 1986.
For a concentration range of 74–407 µg/L
X=0.976(C)+3.94
S=0.131(X)+4.26
SR=0.052(X)+3.01
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 220.1
For Copper, Method 220.1 (Atomic Absorption, Direct Aspiration) replace the Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For concentration range 60–332 µg/L
X=0.963(C)+3.49
S=0.047(X)+12.3
SR=0.042(X)+4.60
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 236.1
For Iron, Method 236.1 (Atomic Absorption, Direct Aspiration) replace the Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trade Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For concentration range 350–840 µg/L
X=0.999(C)-2.21
S=0.022(X)+41.0
SR=0.019(X)+21.2
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-Laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 239.1
For Lead, Method 239.1 (Atomic Absorption, Direct Aspiration) replace Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7 Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”; National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For concentration range of 84–367 µg/L
X=0.961(C)+13.8
S=0.028(C)+33.9
SR=0.011(X)+16.1
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 243.1
For Manganese, Method 243.1 (Atomic Absorption, Direct Aspiration) replace Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J.A. and Britton, P.W., June, 1986.
For concentration range 84–469 µg/L
X=0.987(C)-1.27
S=0.042(X)+8.95
SR=0.023(X)+4.90
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 289.1
For Zinc, Method 289.1 (Atomic Absorption, Direct Aspiration) replace the Precision and Accuracy Section with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water and a natural water or effluent of the analyst's choice. The digestion procedure was not specified. Results for the reagent water are given below. Results for other water types and study details are found in “USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry”, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB86–208709/AS, Winter, J. A. and Britton, P. W., June, 1986.
For concentration range 56–310 µg/L
X=0.999(C)+0.033
S=0.078(X)+10.8
SR=0.049(X)+1.10
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 202.2
For Aluminum, Method 202.2 (Atomic Absorption, Furnace Technique) replace the Precision and Accuracy Section statement with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques), “National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 0.46-125 µg/L
X=1.1579(C)-0.121
S=0.4286(X)-0.124
SR=0.2908(X)-0.082
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 204.2
For Antimony, Method 204.2 (Atomic Absorption, Furnace Technique) replace the Precision and Accuracy Section statement with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this manual as modified by this method. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques),” National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 10.50-240 µg/L
X=0.7219(C)-0.986
S=0.3732(X)+0.854
SR=0.1874(X)-0.461
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 206.2
For Arsenic, Method 206.2 (Atomic Absorption, Furnace Technique) add the following to the existing Precision and Accuracy statement:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques),” National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 9.78-237 µg/L
X=0.9652(C)+2.112
S=0.1411(X)+1.873
SR=0.0464(X)+2.109
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 208.2
For Barium, Method 208.2 (Atomic Absorption, Furnace Technique) add the following to the existing Precision and Accuracy information:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques),” National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 56.50–437 µg/L
X=0.8268(C)+59.459
S=0.2466(X)+6.436
SR=0.1393(X)-0.428
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 210.2
For Beryllium, Method 210.2 (Atomic Absorption, Furnace Technique) replace the existing Precision and Accuracy statement with the following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques),” National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 0.45–11.4 µg/L
X=1.0682(C)-0.158
S=0.2167(X)+0.090
SR=0.1096(X)+0.061
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Deviation, µg/L
Method 213.2
For Cadmium, Method 213.2 (Atomic Absorption, Furnace Technique) add the following to the existing Precision and Accuracy information:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring System Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques),” National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 0.43–12.5 µg/L
X=0.9826(C)+0.171
S=0.2300(X)+0.045
SR=0.1031(X)+0.116
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Devision, µg/L
Method 218.2
For Chromium, Method 218.2 (Atomic Absorption, Furnace Technique) add the following to the existing Precision and Accuracy Section:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the Environmental Monitoring Systems Laboratory—Cincinnati (EMSL-CI). Synthetic concentrates containing various levels of this element were added to reagent water, surface water, drinking water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the reagent water are given below. Results for other water types and study details are found in “EPA Method Study 31, Trace Metals by Atomic Absorption (Furnace Techniques),” National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161, Order No. PB 86–121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
For a concentration range of 9.87–246 µg/L
X=0.9120(C)+0.234
S=0.1684(X)+0.852
SR=0.1469(X)+0.315
where:
C=True Value for the Concentration, µg/L
X=Mean Recovery, µg/L
S=Multi-laboratory Standard Deviation, µg/L
SR=Single-analyst Standard Devision, µg/L
Method 219.2
For Cobalt, Method 219.2 (Atomic Absorption, Furnace Technique), replace the Precision and Accuracy Section statement with the following:
Precision and Accuracy (continued)