WSRC-TR-2003-00063

Final Report on Jobin Yvon Contained Inductively Coupled
Plasma Emission Spectrometer (ICP-ES)

F.M. Pennebaker and J.C. Hart
Westinghouse Savannah River Company
Aiken, SC 29808

1.0 Summary

A new Inductively Coupled Plasma - Emission Spectrometer (ICP-ES) was recently purchased and installed in Lab B-147/151 at SRTC. The contained JY Model Ultima 170-C ICP-ES has been tested and compared to current ADS ICP-ES instrumentation. The testing has included both performance tests to evaluate instrumental ability, and the measurement of matrix standards commonly analyzed by ICP-ES at Savannah River. In developing operating procedures for this instrument, we have implemented the use of internal standards and off-peak background subtraction. Both of these techniques are recommended by EPA SW-846 ICP-ES methods and are common to current ICP-ES operations. Based on the testing and changes, the JY Model Ultima 170-C ICP-ES provides improved performance for elemental analysis of radioactive samples in the Analytical Development Section.

Keywords: ICP-ES, waste tank analysis, RCRA

2.0 Introduction

2.1 Background

Late in FY 1998, ADS received capital funding (project S-W281) to purchase a contained Inductively Coupled Plasma Emission Spectrometer (ICP-ES) for radioactive sample analysis. The new instrument replaced the existing contained ARL 3580 ICP-ES, which was 15 years old. The new instrument was built by Jobin Yvon (JY) in France and is installed in laboratory B-147. A series of performance tests detailed in the specifications were performed prior to awarding the bid. These tests included spectral resolution, dynamic range, short and long term stability, sensitivity and interference control. The tests were also performed on the completed instrumentation in France and following installation at SRTC. JY had difficulty with several of the tests and spent about 6 months at SRTC reconfiguring the instrument and completing the tests. This report will document subsequent testing performed at SRTC to confirm accurate analyses.

2.2 Instrument Description

The instrument is an Inductively Coupled Plasma Emission Spectrometer (ICP-ES) with a 1.5 kWatt 40 MHz solid-state generator contained in a radiological fume hood. The spectrometer section of the instrument consists of a polychrometer for simultaneous analysis of 30 wavelengths and a monochrometer for wavelength flexibility. The monochrometer is a high-resolution design using a 1.0-m focal length Czerny-Turner (CZ) configuration, which covers from 120 nm - 800 nm with an argon purge to remove absorbing contaminants. The monochrometer uses a 2400 g/mm grating in the second order for 120-320 nm, resulting in a (D l ) resolution of 0.005-0.006 nm, full-width at half max (FWHM) and the same grating in first order from 320-800 nm resulting in resolution of 0.010-0.012 nm. Light is then measured with a high-dynamic range detection system (HDD) photomultiplier tube (PMT), which can vary the gain to accommodate a wide variety of intensities. The polychrometer uses a Paschen-Rungen mount (Rowland Circle) design with 0.5-m focal length and a 3000 g/mm grating in first order. The polychrometer also contains a flat-field segment to detect Na, Li and K. Table A-1 (Appendix) lists some of the elements/wavelengths on the polychrometer. The two main advantages to the polychrometer are speed and thermal stability. The main disadvantages are poorer resolution and stray light rejection. Thus, the monochrometer has better sensitivity while the polychrometer is more stable.

2.3 SRTC Hood Modifications

The design of the radiological fume hood in B-147 was found to be inadequate for the needs of SRTC. The radioactive fume hood had several concerns, including inadequate viewing into the hood and a large amount of torque on the glass window for stabilization. Jerry McCarty designed a new window, sash and frame, which were subsequently built and welded together by the machine shop and a local area vendor. The new equipment has been successfully installed in lab B-147. Minor modifications were also made to the brackets and counterweights for easier sash movement.

3.0 SRTC Instrument Testing

ADS evaluated the system for sensitivity, dynamic range, short and long term stability and spectral interference. The tests were similar to the performance tests, but under typical operating conditions (i.e. MDL's were measured for polychrometer lines rather than for optimum detection limits). Testing was also performed to identify typical problems such as PMT overrange and document polychrometer peak locations. The tests are listed in Table 2, and a complete listing of the results are available in Notebook WSRC-NB-2000-120. Most elements showed good stability and reasonable sensitivity. Corrective actions were taken for those elements with poor stability or sensitivity. Several operational changes were made due to the new instrumentation. These operational changes include background correction, gain settings on PMT's, use of guassian mode of peak calculation and use of an internal standard.

3.1 Initial Documentation

Initial tests were performed to document ICP performance after installation. We measured the signal and Relative Standard Deviation (%RSD) for 10 mg/L analyte, background intensity, detection limits and polychrometer position location with centering on Cr for a variety of wavelengths. This initial documentation will provide a baseline to evaluate performance over time. This documentation should also help evaluate problems during instrument breakdown.

3.2 Spectrometer Resolution

The JY ICP performed very well on the resolution performance tests at SRTC and France. Results demonstrated the 0.005-0.006 nm resolution in second order and 0.010-0.012 nm resolution in first order. We found no need for further testing on the resolution. The results are included below.

Table 1. Performance Test 3.1.1 Resolution

Description

Bid Package

SRTC Results

FWHM of Al 167 nm

0.0044 nm

0.0044 nm

Resolution of Tl doublet at 190.84

0.005 nm

0.00489 nm

Fe 310.04 - 3 peaks should be resolved and 4th partially resolved

ok

ok

As and Cd resolved at 228.802

resolved (D l = 0.0043)

Resolved (D l = 0.0042)

Ce and Fe resolved at 395.25 nm

resolved (D l = 0.0068)

Resolved (D l = 0.010)

Nd and Ce resolved at 401.22 nm

resolved (D l = 0.009)

Resolved (D l = 0.010)

3.3 ICP Wavelength Stability

One of our concerns was stability of the analytical signal. There were no stipulations for ICP operating conditions in the performance tests; thus, the instrument was run with slits at maximum during testing. ICP sensitivity and interference is significantly hampered by operation in this mode. Also, SRTC has temperature fluctuations, which can significantly impact ICP stability. We performed our own stability tests to obtain a true picture of ICP long term and short term stability. Our tests showed good short-term stability for performance times less than two hours. Long-term stability was very good for polychrometer elements, but very poor for monochrometer elements.

We believe that temperature instability was a major cause of poor results on several of the performance tests at France and SRTC. The result is that monochrometer wavelengths significantly move during operation of the instrument (see Figure 1). This instability can cause as much as a 50% decrease in signal after 8 hours. Temperature instability is not evident on the polychrometer, even after 9 hours of run time. We must use an alternate mode of peak calculation called the guassian mode to prevent recalibration every hour or two for monochrometer wavelengths. For this method, 9 points are collected over the spectral region and a guassian curve is drawn from the best 5 points. If the wavelength shifts, the program should still find the maximum intensity of the peak. We are hopeful that recent modifications of the ventilation ducts in B-147/151 will improve temperature instability and allow other calculation methods.

Figure 1. Change in monochrometer wavelength position of Molybdenum 202.03 nm from 9:00 (red) to 5:00 (black) during constant operation.

Figure 1. Change in monochrometer wavelength position of Molybdenum 202.03 nm
from 9:00 (red) to 5:00 (black) during constant operation.

3.4 Background Interference

The existing ARL 3580 instrument had very good rejection of stray light, which has enabled SRTC to avoid using background correction until now. The JY polychrometer has approximately 30 times the stray light of the ARL. Table 2 compares the P 178.225 nm intensities on the ARL 3580 and the JY ICP-ES instruments. Some of the interference, i.e. Mo, is from direct overlap from a nearby wavelength; however, most of the increases in signal are from an increased background level caused by inadequate rejection of stray light. This increased background would cause inaccurate measurements for trace analysis. Background correction is a common practice in ICP-ES to eliminate this problem. Two points on either side of the peak are measured, averaged and subtracted from the peak. However, this is a significant change from our previous "hot" operation. The CTF over the instrument will need to be cognizant of background interference biasing numbers low. We have looked at interference on the polychrometer elements and selected the best correction positions based on common matrices and interference intensity.

Table 2. Comparison of measured concentration of ARL 3580 and JY ICP-ES instruments
for P at 178 nm. High concentrations are mostly the result of background interference,
which can be eliminated with background subtraction.

Solution

JY ICP-ES

ARL ICP-ES

JY with Bk Corr

1P 10 mg/L

7.90

10.0

9.12

Mn 100 mg/L

11.4

0.383

0.161

Fe 100 mg/L

3.24

0.090

-0.003

Mo 100 mg/L

0.854

0.292

0.579

Zr 100 mg/L

1.52

0.025

0.038

Ti 100 mg/L

0.46

0.042

0.014

Sn 100 mg/L

0.09

0.026

-0.010

1 Instrument was calibrated with High Purity mutielement standard: ADS Mix 1 Solution A. Low value
for JY ICP indicates interference from Mn and Fe in standard.

3.5 Gain and Internal Standards

We have made other modifications to the operation of the instrument to accommodate the needs of SRTC. First, gain settings on the PMT's in the polychrometer were set at the factory for optimum detection limits rather than dynamic range. We have reset the gains in several cases to measure higher concentrations typical of ADS solutions. For example, Si could measure a maximum of 20 mg/L without PMT over-range (requiring additional dilution for successful quantitation). We have reset the gain to measure at least 100 mg/L.

Second, we have added the use of an internal standard. This change should improve analysis of high concentrations of salt. At first, we attempted to use scandium on the monochrometer as an internal standard; however, the JY software automatically shifts from the guassian mode to peak height mode. We used Ce 399.924 nm on the polychrometer as an internal standard for Comparison Testing (Section 4.0). We have added a Scandium channel to the polychrometer since that time for internal standard correction.

4.0 SRTC Comparison ICP-ES Testing

Common analytical samples were analyzed on the current SRTC ICP-ES systems, "cold" ICP-ES (Optima 3000) and "hot" ICP-ES (ARL 3580), and compared to the JY. All samples and standards were non-radioactive and represent the wide range of samples analyzed by ADS. The results are split into common samples (Section 4.1) from selected ADS customers and solid and liquid standards (Section 4.2) from various labs.

4.1 ICP-ES Comparison of Common Samples

We selected two sets of samples for analysis by the JY: 300170118-300170129 and 300166455-300166465. These samples were selected because they had a relatively small number of elements and were representative of the high salt samples typically analyzed by ADS. The samples were run at 1000-fold dilution to measure sodium and 100-fold dilution to measure aluminum and silicon. The results for samples 170118-170129 are compiled below in Tables 3 and 4.

Table 3. Comparison of sodium and silicon analysis with both JY and Optima
Instruments. Concentrations are measured in units of mg/L.

Sodium Analysis

Silicon Analysis

Sample ID

JY

Optima

% Difference

JY

Optima

% Difference

170118

77000

80700

-4.7

116

97

18

170119

77200

80600

-4.3

128

107

18

170120

78200

81000

-3.5

214

193

10

170121

78000

80100

-2.7

217

201

7.5

170122

77800

81900

-5.1

401

376

6.4

170123

78700

82400

-4.6

405

384

5.4

170124

81700

84500

-3.4

119

108

9.2

170125

81800

84900

-3.7

112

105

6.6

170126

82700

86500

-4.5

229

219

4.2

170127

81100

82700

-2.0

205

197

4.2

170128

82000

86800

-5.7

346

330

4.7

170129

82000

86300

-5.1

321

319

0.8

 

Table 4. Comparison of aluminum analysis with JY and Optima ICP-ES Instruments.
Concentrations are measured in units of mg/L.

Al Analysis

Sample ID

JY

Optima

% Difference

170118

3410

3330

2.4

170119

3490

3440

1.4

170120

3220

3190

0.9

170121

3350

3320

0.9

170122

3260

3280

-0.6

170123

3140

3110

1.0

170124

4830

4790

0.8

170125

4970

4930

0.8

170126

4420

4400

0.5

170127

4290

4290

0.0

170128

4780

4700

1.7

170129

4360

4380

-0.5

 

Figure 2. Comparison of Si measurements in samples 170118-170129 from Tank 38 Si removal studies.

Figure 2. Comparison of Si measurements in samples 170118-170129
from Tank 38 Si removal studies.

For these samples, the two instruments compared well for Al and Na measurements. Theinstruments also compared well for Si except for the first three samples, which contain low levels of Si in a high sodium matrix. A high bias for low levels of Si was found for the JY instrument and is discussed in ADS document SRT-ADS-2002-0343. Figure YY shows a comparison plot of Si concentration in each sample.

A comparison of samples 166455-166465 was also performed by the two ICP-ES systems. The results are shown in Tables 5 and 6 below.

Table 5. Comparison of sodium and aluminum analysis with both JY and
Optima Instruments. Concentrations are measured in units of mg/L.

Sodium Analysis

Aluminum Analysis

Sample ID

Optima

JY

% Difference

Optima

JY

% Difference

166455

160000

158000

-1.3

3440

3350

-2.8

166456

136000

135000

-0.7

37.0

31.0

-18.3

166457

134000

137000

2.2

222

207

-6.6

166458

137000

137000

0.0

452

436

-3.7

166459

137000

139000

1.5

634

607

-4.3

166460

150000

144000

-4.1

986

944

-4.4

166461

150000

150000

0.0

1480

1410

-4.9

166462

155000

157000

1.3

1980

1880

-5.3

166463

168000

161000

-4.3

2210

2070

-6.6

166464

163000

165000

1.2

2130

2020

-5.5

166465

170000

166000

-2.4

2060

1940

-5.7

 

Table 6. Comparison of silicon analysis with JY and Optima ICP-ES Instruments.
Concentrations are measured in units of mg/L.

Si Analysis

Sample ID

Optima

JY

% Difference

166455

2980

2970

-0.4

166456

80.3

79.4

-1.1

166457

230

222

-3.6

166458

437

413

-5.5

166459

597

561

-6.1

166460

886

850

-4.2

166461

1290

1220

-5.3

166462

1660

1570

-5.4

166463

1810

1690

-6.9

166464

1680

1580

-6.4

166465

1570

1470

-6.8

These samples had a much higher variation in Si and Al concentration, but the measurements for these elements were very good with the JY instrument. In all cases, except for Al in sample 166456, the results were within 7% of the concentration found by the current ADS "non-radioactive" ICP-ES. In the single anomalous case, Al concentration after dilution was very low, and the difference is within the expected error for such a low measurement.

4.2 ICP-ES Comparison of Common Standards

While the results of section 4.1 demonstrated the consistency in measurement between the two instruments, accuracy can only be demonstrated on standard materials with known concentrations. Nine different solid and liquid standards traceable to NIST were prepared and analyzed by all three ADS ICP-ES instruments for comparison. The results are shown in Tables 7-15 below. The results demonstrate very good accuracy for the elements measured. There are a few exceptions to note. First, Aluminum measured low for the BCR sludge standard for all three instruments, most likely due to incomplete dissolution. Second, analyses of trace components (i.e. Cd) in solids and drinking water were difficult due to the low concentration in the final solution. Lastly, line selection on the polychrometer played a significant role in the analysis. Trace levels of barium consistly measured high on JY and ARL ICP’s due to the use of different wavelength from the Optima instrument. Overall, the instrument performed very well on these standards and should improve, as the operators become more familiar with the instrument and its operation.

Table 7. Elemental analysis of LOAM-B soil sample digested by fusion and microwave
ADS followed by ICP-ES analysis. Concentrations are measured in units of ug/g.

LOAM B – soil sample ADS 165864 (Concentration in ug/g)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

51000

49800

51600

51400

-0.8

Ca

3400

3470

3420

3390

0.3

Fe

27700

27600

29200

27400

1.1

Mg

3970

3730

4190

4040

-1.7

Mn

1570

1520

1670

1590

-1.3

Na

4630

4250

4710

4110

12.7

Si

363000

346000

352000

NA

NA

Sr

146

166

174

142

2.8

Ti

7700

7640

7630

(5700)

NA

Cd

116

93

105

92

26.1

 

Table 8. Elemental analysis of ARG glass standard by fusion and microwave digestions
followed by ICP-ES analysis. Concentrations are measured in units of ug/g.

ARG Glass Std - ADS 165865 (Concentration in ug/g)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

24500

24600

24800

25000

-2.0

B

24300

26400

NA

26900

-9.7

Ba

983

803

969

790

24.4

Ca

10100

10300

10800

10200

-1.0

Cr

723

669

811

640

12.9

Fe

99700

98000

103000

97900

1.8

Li

15200

14800

15800

14900

2.0

Mg

5220

4800

5540

5200

0.4

Mn

14900

14200

15400

14600

1.7

Na

89500

84500

89100

85200

5.0

Ni

8270

8020

8250

8270

6.9

Si

227000

222000

240000

224000

1.3

Ti

7110

6900

7150

6900

3.0

 

Table 9. Elemental analysis of LRM glass standard by fusion and microwave digestions
followed by ICP-ES analysis. Concentrations are measured in units of ug/g.

LRM Glass Std - ADS 165866 (Concentration in ug/g)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

51600

50800

52700

50600

2.0

B

22400

24700

25400

24800

-9.0

Ca

3900

3920

3690

3830

1.8

Cd

1450

1420

1450

1380

5.1

Cr

1470

1360

1390

1310

11.9

Fe

10300

10300

10400

9940

4.2

Li

522

512

485

497

4.9

Mg

660

545

648

615

7.3

Mn

601

579

595

608

-1.2

Na

161000

156000

163000

153000

5.6

Ni

1610

1500

1360

1460

10.2

Pb

815

904

672

891

-8.6

Si

263000

241000

260000

257000

2.3

Ti

657

622

607

629

4.3

Zr

7710

7100

7290

6740

14.4

 

Table 10. Elemental analysis of BCR Sludge standard by fusion and microwave digestions
followed by ICP-ES analysis. Concentrations are measured in units of ug/g.

BCR Sludge Standard - ADS 165867 (Concentration in ug/g)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

25900

24600

27600

47600

-45.6

Ca

92600

95600

98800

101000

-8.8

Cd

106

81

85

78

36.4

Fe

19400

19100

20300

18500

4.7

Mg

17000

15900

18000

19900

-14.6

Mn

608

571

633

588

3.4

Na

2190

2410

2220

2230

-1.6

Ni

330

316

246

280

17.9

P

28900

28900

31000

25700

12.2

Pb

1430

1230

1200

1270

12.6

Si

107000

103000

124000

107000

0.4

Ti

17100

16900

18000

17400

-2.0

Zn

4230

4080

3850

4060

4.2

Table 11. Elemental analysis of SRS Frit 202 by fusion and microwave digestions
followed by ICP-ES analysis. Concentrations are measured in units of ug/g.

Frit 202 - ADS 165868 (Concentration in ug/g)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

1490

1920

1070

1800

-17.2

B

22800

24900

26900

24500

-6.9

Ca

2780

2870

2870

NA

NA

Fe

308

338

301

266

15.9

Li

31600

30300

32500

32100

-1.6

Mg

12500

11900

13100

11900

4.9

Na

46000

45000

47200

43900

4.8

Si

368000

356000

362000

356000

3.4

Ti

1650

1630

1640

NA

NA

 

Table 12. Elemental analysis of Drinking Water Standard from High Purity Standards
by ICP-ES analysis. Concentrations are measured in units of mg/L.

Drinking Water Standard - ADS 165824 (Concentration in mg/L)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

0.120

0.132

0.123

0.120

-0.1

Ba

0.044

0.051

0.050

0.050

-12.7

Ca

31.2

34.9

36.5

35.0

-10.8

Cd

0.007

0.011

0.013

0.010

-30.0

Cr

0.019

0.021

0.041

0.020

-5.0

Cu

0.018

0.024

0.020

0.020

-9.5

Fe

0.094

0.099

0.104

0.100

-6.0

Mg

8.81

9.22

8.99

9.00

-2.1

Mn

0.038

0.040

0.040

0.040

-5.0

Na

5.98

6.42

6.09

6.00

-0.3

Ni

0.060

0.060

0.062

0.060

0.0

P

<0.012

<0.076

<0.035

NA

NA

Pb

<0.066

<0.077

0.070

0.040

NA

Si

<0.008

<0.014

0.114

NA

NA

Sr

0.24

0.26

0.25

0.25

-5.2

Ti

0.001

<0.016

<0.001

NA

NA

Zn

0.066

0.077

0.069

0.070

-5.7

 

Table 13. Elemental analysis of Hanford Envelope A Simulant by ICP-ES analysis.
Concentrations are measured in units of mg/L. No standard values available.

Envelope A Simulant - ADS 165825 (Concentration in mg/L)

Element

JY

Optima

ARL

Al

1060

954

1260

B

2.09

2.49

3.30

Ba

<0.08

<0.12

<0.03

Ca

3.01

3.04

3.22

Cd

<0.06

<0.14

0.132

Cr

57.6

57.6

68.7

Cu

<0.40

<0.50

0.058

Fe

<0.04

<0.44

0.133

Mg

<0.2

<0.84

0.59

Mn

<0.007

<0.09

0.032

Na

11300

10700

11000

Ni

<0.32

<0.62

0.15

P

19.1

19.6

21.1

Pb

<5.9

<6.9

2.69

Si

6.8

16.7

10.5

Sr

<0.004

<0.020

0.021

Ti

0.050

<1.4

0.266

V

NA

<1.3

0.090

Zn

<0.30

<3.7

0.45

Zr

<0.050

<0.48

0.062

Ag

NA

<3.0

0.080

 

Table 14. Elemental analysis of SPEX Multi-Element Standard by ICP-ES analysis.
Concentrations are measured in units of mg/L.

SPEX Multi-element Standard - ADS 165826 (Concentration in mg/L)

Element

JY

Optima

ARL

Expected

% Difference (JY)

B

494

535

532

500

-1.2

Li

483

493

519

500

-3.4

Mg

482

496

543

500

-3.6

Na

508

517

530

500

1.6

P

498

502

530

500

-0.4

Si

476

459

558

500

-4.8

Ti

479

510

529

500

-4.2

 

Table 15. Elemental analysis of In-house Standard by ICP-ES analysis.
Concentrations are measured in units of mg/L.

ADS Standard 1 - ADS 165827 (Concentration in mg/L)

Element

JY

Optima

ARL

Expected

% Difference (JY)

Al

501

490

586

500

0.20

Na

2360

2200

2470

2200

7.3

Si

208

208

242

200

4.0

Pb

9.55

9.87

11.9

10.0

-4.5

Ag

NA

9.67

14.3

10.0

NA

Ba

9.89

10.0

11.2

10.0

-1.1

Cd

9.80

10.0

11.2

10.0

-2.0

Cr

9.58

9.82

12.0

10.0

-4.2

Be

NA

9.66

NA

10.0

NA

5.0 Data Export and Workup

Data work-up for the JY ICP-ES was accomplished using a new Excel Macro (designed by ADS) called "JY_NewMacro_ves1" and Excel computational workbooks called "JY Template Rev 1.xls" and "JY Template Solids Rev 1.xls." The macro is documented in Notebook WSRC-NB-2001-120 pp. 56-64. For routine operations of the instrument, an excel template "JY _Liquid_Template_U_Poly.xls" is used in tandem with "JY_MDL_Master.xls." The spreadsheets have been designed by ADS and confirmed with ICP-ES data that has been calculated by hand.

6.0 Conclusions

While installation of the instrument was time-consuming for the vendor and ADS, the overall result was a reliable instrument for routine measurements of radioactive samples at SRTC. In developing operating procedures for this instrument, we have implemented the use of internal standards and off-peak background subtraction. Both of these techniques increased the accuracy of results from the ICP-ES for samples with difficult matrices. Improved accuracy has been demonstrated by the performance tests described in section 4.0 of this document. Overall, the instrument performed very well on these standards and should improve, as the operators become more familiar with the instrument and its operation.

Appendix

These tables are included to record performance and set parameters at the beginning of operation.

Table A-1. Background correction positions for polychrometer wavelengths.

Element

Wavlength (nm)

Left Background (nm)

Right Background (nm)

Al

308.215

0.0127

0.0199

B

208.959

0.0199

0.0199

Cd

226.502

0.0127

0.0199

Ce

399.924

0.0199

0.0199

Cr

205.599

0.0199

0.0199

Cu

224.700

0.0199

0.0199

Fe

259.940

0.0127

0.0199

K

766.490

0.0199

0.0199

Mn

257.610

0.0199

0.0199

Na

589.582

0.0199

0.0199

Ni

216.552

0.0127

--------

P

178.225

0.0199

0.0199

Pb

220.353

0.0199

0.0199

Si

251.611

0.0127

0.0199

Zn

213.856

0.0199

0.0199

 

Table A-2. Detection limits for selected JY wavelengths using Guassian mode
for monochrometer wavelengths.

Element

Wavlength (nm)

Poly/Mono

MDL (mg/L)

Al

308.215

Poly

0.093

B

208.959

Poly

0.013

Ba

230.424

Poly

0.008

Be

313.042

Mono

0.002

Ca

393.367

Poly

0.001

Cd

226.502

Poly

0.006

Cr

205.599

Poly

0.012

Cu

224.700

Poly

0.005

Fe

259.940

Poly

0.004

K

766.490

Poly

1.16

La

408.672

Poly

0.001

Li

670.784

Poly

0.005

Mg

279.553

Poly

0.0004

Mn

257.610

Poly

0.0007

Na

589.582

Poly

0.022

Ni

216.552

Poly

0.032

P

178.225

Poly

0.111

Pb

220.353

Poly

0.038

S

181.978

Mono

0.024

Sb

217.581

Mono

0.009

Si

212.412

Mono

0.031

Si

251.611

Poly

0.055

Si

288.158

Mono

0.041

Sn

189.989

Mono

0.1

Sr

407.771

Poly

0.0004

Ti

334.940

Poly

0.0012

V

292.402

Mono

0.002

Zn

213.856

Poly

0.003

Zr

349.621

Poly

0.005

Zr

343.823

Mono

0.010

Ce

413.765

Mono

0.094

Ce

413.380

Mono

0.097

Eu

381.965

Mono

0.0006

La

398.852

Mono

0.003

La

379.478

Mono

0.0018

Nd

406.109

Mono

0.010

Nd

401.225

Mono

0.003

Pr

414.311

Mono

0.012

Sm

359.262

Mono

0.006

Br1

76.557

Mono

0.630

Cl1

67.362

Mono

1.100

Hg

253.652

Mono

0.008

U

385.958

Poly

1.12

                    1 Cl and Br wavelengths are 1/2 of true wavelengths.

Table A-3. Optimized gain settings for the JY ICP-ES instrument.

Element

Channel

Factory Gain (on)

Factory Gain (off)

New Gain (on)

New Gain (off)

Ba

11

6,5,4,3,2

1

6,5,3,1

4,2

Ca

22

6

5,4,3,2,1

4

6,5,3,2,1

Cd

10

6,5,4,3

2,1

6,5,4

3,2,1

La

25

6,4,3,2

5,1

6,4,3,2

5,1

Li

27

6,5,4

3,2,1

6,5,3

1,2,4

Mg

15

6

5,4,3,2,1

3,4

6,5,2,1

Si

12

6,5,4,3,2

1

6,4,2

5,3,1

Sr

24

6,4,2,1

3,5

4,3

6,5,2,1

Zn

6

6,5,4,2

1,2

6,4,3

5,1,2

Zr

20

6,5,4

3,2,1

3,4

6,5,1,2