IR 05000293/1990017

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Insp Rept 50-293/90-17 on 900624-29.No Violations Noted. Major Areas Inspected:Radiological & Nonradiological Chemistry Programs
ML20058L719
Person / Time
Site: Pilgrim
Issue date: 07/25/1990
From: Bores R, Kottan J, Mcnamara N
NRC OFFICE OF INSPECTION & ENFORCEMENT (IE REGION I)
To:
Shared Package
ML20058L706 List:
References
50-293-90-17, NUDOCS 9008080045
Download: ML20058L719 (15)
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Text

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n"im V'. S. NUCLEAR REGULATORY COMMISSION

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Report'N /90-17 s: Docket N .. t I 

', License N DPR-63

Licensee: Boston Edison C I 800 Boylston Street Boston, MA 02199 , 

 .. Facility Name: Pilgrim Nuclear Power Station   -

Inspection At: plymouth, Massachusetts I-Inspection Conducted: June 24-29, 1990 . 

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 ' Inspectors: kfe T. k Afej   d to f 90 J N. - R Namara, Physical Science Technician date Effluents Radiation Protection Section-(ERPS)

N i: PL4fDy-J. J. Kottag, Laboratory' Specialist,'ERPS 9-2.o~90 l 

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L Approved by: b # 

  . J. B9es, Chief, ERPS, Facilities  dat Radiation Safety and Safeguards Branch  j Division'of Radiation Safety and Safeguards  !

i i Inspection Summary: Inspection on' June 24-29, 1990-(Inspection Report No.'50-293/90-17) c' Areas Inspected: Routine, unannounced inspection of the radiological and unon-radiological chemistry programs. Areas reviewed included: confirmatory measurements-radiological, standards. analyses-chemis'ry, and laboratory ; 

 -QA/Q i-Results: Of the areas reviewed, no violations were identifie J t

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i-(; DETAILS 1.0 Individuals Contacted l 

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 *N. DiMascio, Radiation Section Manager
 *C. ' Goddard, Chemistry Division . Manager
 *J. Kelly, Senior Compliance Engineer
 * Kraft, Junior, Acting Plant Manager P. Hamilton, Compliance Division Manager   ,

L. Highfill, Station Director ' 

 *D. Long, PSD Manager
 *D. McCloskey, Manager, Radwaste and Chemistry F
 *A'. Muse, Chemistry Supervisor    i
 *A. Shatas, Senior QA Engineer    ;
 *K. Snyder,' Chemistry Supervisor   i
 *D. Swanson, Regulatory Af fairs Department Manager  !

Other Personnel l i 

 *C. Carpenter, NRC Resident Inspector
 *R. Bores,-NRC:RI     l
 * Denotes those personnel who attended the exit meeting on June 29,.1990, 1 The inspectors also interviewed other licensee personnel including other !

members of the chemistry and health physics staff I 2,0 Purpose  ! The purpose of this routine inspection was to review the following area , 

      ! The licensee's ability to measure radioactivity in plant systems and ,

effluent samples, and ability to measure chemistry parameters in 

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l various plant system ' 

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 '2, _The licensee's ability to demonstrate the acceptability of analytical results through implementation of a' laboratory QA/QC j progra ' Radiological and Chemical Measurements   ,

3.1 Confirmatory Measurements (Radiological) During this part of the inspection, liquid, airborne particulate (filter) and iodine (charcoal cartridge), and gas samples were analyzed by the licensee and the NRC for purpose of intercompariso The same samples were analyzed by both the NRC and the licensee with the exception of the stack gas sample, which was an actual split sample. Where possible, the samples are actual effluent samples or inplant samples which duplicated the counting geometries used by the licensee for radioactive effluent sample analyses. The samples were . l l l l

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analyzed by'the licensee using routine methods and equipment'and by the NRC:I Mobile Radiological Measurements Laboratory. Joint analyses of actual effluent samples are used to verify the licensee's capability to measure radioactivity in effluent and other samples with respect 

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to the Technical Specifications _and other regulatory requirement , h In addition, a liquid effluent sample was sent'to the NRC reference laboratory, Department of Energy, Radiological and Environmental Sciences Laboratory (RESL), for analyses requiring wet chemistr The analyses to be performed on the sample are Sr-89, Sr-90, Fe-55, 

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H-3, and gross alpha. The results of these analyses will be compared with the licensee's results when received at a later date and will be documented in a subsequent inspection repor The results of an effluent sample split between the licensee and the 

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NRC during a previous inspection on August 12-16,1985(Inspection Report Number 50-293/85-23) were also compared during this i inspectio The licensee's Health Physics Department also_ possesses ~a gamma 

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spectrometry syste Therefore, the particulate filter, charcoal cartridge, gas samples, and a. liquid effluent sample were also analyzed using the Health Physics counting system and compared with the NRC results. Both the particulate filter and charcoal cartridge are types of samples,_which are routinely analyzed by this departmen The- results of the sample measurements comparison, presented in t Table 'I, indicated that all ef the measurements were in agreement under the criteria used for comparing results (See Attachment 1) with the exception of one measurements result. The' result-in > disagreement:was an Fe-55 analysis of a liquid radioactive water sample. This analysis was performed for the licensee by a vendor 3 laboratory which is no longer used. Therefore, the liquid sample ' that was taken during this inspection will be compared with the licensee's results obtained from the.present laboratory and those results will be documented in a subsequent inspection report. The inspector noted that the licensee's Fe-55 result using the previous vendor was higher than the NRC's result anc' was, therefor , conservative, and would not have resulted in the licensee exceeding ' any Technical Specifi_ cations effluent release limi In addition, the inspectors determined that the licensee's Health Physics Department routinely analyzes inplant air particulate filters and charcosi cartridges combined rather than separatel , < 

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The inspector discussed this matter with the licensee and stated < 

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that although the' air particulate filter and charcoal cartridge samples are taken together, they should be counted individually because-the radioactivity distribution between the filter and the , cartridge can vary from sample to sample. Under these circumstances it is very difficult to prepare a calibration standard which accurately represents the radioactivity distribution in both the 

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[  particulate filter and charcoal cartridge. The licensee responded
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,,-  by stating that air particulate and charcoal cartridge samples v  would continue to be counted together for screening purposes, but r   that if radioactivity was detected during the screening, the L ,  particulate filter and charcoal cartridge would be analyzed independently. The health physics results presented in Table I are
,  those from individual analyses of the particulate filter and charcoal cartridge
,   The inspector had no further questions in this area. No violations-
/  were identifie , i 3.2 Standards Analyses (Chemical)

During this part of the inspection, standard chemical solutions were submitted to the licensee for analysi The standards were prepared by Brookhaven National Laboratory (BNL) for the NRC, and were analyzed by the licensee using-routine methods and equipmen The analysis of standards is used to verify the licensee's capability to monitor chemical parameters in various plant systems with respect to-Technical Specifications and other regulatory requirements. In addition, the analysis of standards is used to evaluate the licensee's' procedures with respect to accuracy and precisio The standards'were submitted to the licensee for analysis in triplicate at three concentrations spread over the licensee's normal calibration and analysis range. The metals analyses performed using the directly coupled plasma spectrometer (DCP), however, were performed singly because of time constraint The results of the standards measurements comparisons, presented in Table II,' indicated that all results were in ' agreement or qualified agreement under the criteria used for comparing results (See Attachment 2), with the exception of the' nickel and boron result The licensee's initial nickel results comparison indicated one dis-agreement and two qualified agreement results. Also the licensee's nickel results had standard deviations ranging from approximately 5 percent to 13 percent while the average standard deviations of the other metal results' ranged from approximately 1 percent to 4 percen These initial nickel analyses were performed using the inductively coupled plasma spectrometer (ICP). The licensee then recalibrated the-ICP and re-ran the NRC nickel standards. This time two values were in disagreement with one value in qualified agreement. The spread of the data, however, was better with the standard deviations in the 2-4 u- percent rang The licensee then performed the metals analysis using the DCP. (The DCP was replaced by the ICP by the licensee for routine analyses and is used only as a backup instrument when the ICP is out of service.) The DCP nickel results were in agreement (two values) or qualified agreement (one value) with the NRC known value The licensee could offer no explanation for the apparent discrepancy for the nickel results obtained from the ICP. The licensee stated that k' 

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j this area would be reviewed and the reason for'the disagreement  ! determined. Just prior to this inspection the ICP had been taken out 

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      'I of service for repairs, and during this inspection the instrument vendor performed maintenance on the ICP so that it would be available .(

for analysis of the-NRC standards. Additionally, the licensee stated ! that the ICP procedure would be modified to include specific checks 'l to be' performed after maintenance to ensure proper wavelength 1 calibrations and appropriate spectral lines were used for reporting results. The initial ICP nickel analyses and re-analyses are reported 

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in Table II as well as the DCP nickel result The boron disagreements appeared to be due to the fact that'the licensee did not take the boron analysis titration to the required ' endpoint. The licensee performed boron analysis by potentiometric ' titration with sodium hydroxide af ter the addition of mannitol to the sample. Licensee procedural requirements included adjustment of the 4 sample pH to 7, addition of mannitol, then titration to an endpoint i pH of 7. The~ inspector discussed this matter with the licensee and if stated that both ASTM procedures and BNL recommended using an endpoint - beyond a pH value of 7. The' inspector gave the licensee a copy of 1 

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titration curves prepared at BNL. The licensee stated that the NRC boron standards were in the form of boric acid whereas the licensee b; normally performs boron analysis on samples containing sodium borate rather than boric acid. The licensee further stated that his boron ) analysis had been optimized for the-analysis of sodium borate rather j than boric acid. However, the inspector reviewed the licensee's a 

 .interlaboratory sodium pentaborate results for 1989 and 1990 to date j
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and noted that the results averaged 1-2 percent below the known valu The inspector stated that the licensee's method of analysis using 

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identical pH-end points appeared to introduce a slightly low bias to - the boron analysis results. The inspector further noted that this ' bias was conservative with respect to Technical Specification boron analysis requirements. The licensee stated that this area would be reviewed and appropriate corrective action taken. In addition, th ! licensee analyzed two NRC boron standards using the NRC suggested titration endpoint, and the results were in agreement with the NRC ; known values. The inspector stated that the above areas would be i reviewed during subsequent inspection The inspector had no further questions in this area, No violations were identifie l 

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4.0 Laboratory QA/QC 

 'The inspector reviewed the licensee's chemistry and radiochemistry laboratory QA/QC program. The program is described in a number of procedures including
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SI-CH-0100 Quality Control of Chemistry Laboratory Data and 

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SI-CH-0150 Quality Control of Counting Room Instrumentatio ;l

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 -These procedures provide for both an intralaboratory QA/QC program ~and an i
 . interlaboratory QA/QC program. The intralaboratory program consisted of instrument _and procedure- control charts. The interlaboratory program consisted of the analysis of unknown samples received from outside laboratories. Two outside. laboratories were used to supply unknowns for ,

chemical analyses and one outside laboratory was used to supply unknowns ' for radioactivity analyses. The licensee's procedures contained 

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acceptance criteria for comparing these results. The inspector reviewed 

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selected laboratory data generated by- the licensee's laboratory QA/QC program for 1989 and 1990 to date and noted that the licensee appeared to 

,  be implementing the laboratory QA/QC program as required. Also included in this program was the vendor laboratory used by the licensee for
 . performing radiological: analyses of ef fluents samples which require wet chemistr The inspector noted, however, that the licensee did not appear to be reviewing the data generated'by the laboratory QA/QC program and taking

_ corrective actions where necessary. For example, selected QC charts for-the gamma spectrometer appeared to be biased, but no corrective action-was. initiated. Also chemistry interlaboratory data appeared to be biased 

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or outside the licensee's acceptance criteria but no corrective. action was.19itiated because the data had not been reviewed. -The licensee-stated that a laboratory QA/QC specialist was in the process of being hired specifically to oversee the entire laboratory QA/QC program and~ this would address the above concerns identified by the inspecto The: inspectors also reviewed Audit Report No. 90-09 which covered 

 ' Chemistry and Radiological Effluent Technical Specifications (RETS). -

This audit, which was conducted during the period March 5-24, 1990, appeared to be thorough and of good technical depth with a technical specialist as-a member of the audit team. One particular area of. focus for this audit was the laboratory-QA/QC program, and the inspector noted-that the areas of concern discussed above were similarly noted by the audit tea The inspector had no further questions in this area. No violations were identifie .0 Exit Interview The-inspector met with the licensee representatives denoted in Section 1-of this report at the conclusion of the inspection on June 29, 1990. The inspector summarized the purpose, scope and findings of the inspectio , l

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R j > Table-I Pilgrim' Verification Test Results-SAMPLE- ISOTOPE NRC VALVE LICENSEE VALV COMPARISON 

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1' Results:in Total Microcurie y 

;i  si  ' Main Stack  .Ba-140 (7.010.6)E-4 (9.56110%)E-4 Agreement ,

M,: A Particulate'- j R' - Filter ,! 

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   -Main' Stack  I-131 (6.4 0.3)E-3 (6.2319%)E-3 Agreement j h  4   Charcoal  .I.-133 -(4.510.2)E-2 (4.3419%)E- Agreement U   1 Cartridge
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      .Results in Microcuries:Per Milliliter  ,j Liquid Radic- .Mn-54- L(8.310.3)E-6 (7.92 7%)E-6- Agreement j WF   r ac:tive Waste-  C0-854 (1.5410.02)E- .(1.65 6%)E-5- -Agreement 4
   :1424 hrs:  Co-60 (4.74 0.04)E-5 (5.0714%)E-5- Agreement: *

W 6-27-9 Ba-140' (2.0310.07)E-5' (2.1116%)E-5 _ Agreement t 

#   ,(Chemistry  .Na-2 (1.'80 0.03)E-5 (1.93t6%)E-5 . Agreement' J
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   ' Liquid-Radio-  H-3- -(9.6 0.5)E-6 (1~.110.1)E-5 ' Agreemen *
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L'i q uid' Rad i o- Fe-55; jl L 

      (8.63 0.17)E-6 (2.210.4)E-5 Disagreement ~
,   ~ active Waste * . H-3 ' . .(2.5610.07)E-5 (2.210.2)E-5 Agreement 3
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10-18-85.- Sr-89 (1.1 0.2)E-7 (8.113.4)E-8 Agreement o 

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Sr-90 

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h 4 . E Table I (continued) Pilgrim Verification Test Results SA"1LE ISOTOPE NRC VALUE LICENSEE _VALUE COMPARIS0N 

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:        i Results in Microcuries Per Milliliter F  Stack Ga Kr-85m (4.3 0.3)E-7 (4.8918%)E-7 Agreement
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0920 hr Xe-133 (1.83 0.06)E-6 (1.94 11%)E-6 Agreement 

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6-27-90 , g" (Chemistry-analysis) F Crud Particulate- Cr-51 (9.010.3)E-5 (8.7 8%)E-5 Agreement , Filter Mn-54 (3.03 0.06)E-5 (3.1416%)E-5 Agreement-0800 hrs .Mn-56 (1.83 0.03)E-4 (1.91 5%)E-4 Agreement 6-26-90 Co-5R (2.6010.07)E-5 (2.716%)E-5 Agreement (Chemistry , Co-60 (5.24 0.08)E-5 (5.414%)E-5 Agreement analysis) 

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 -Reactor Water I-132 (1.98i0.02)E-3 (1.8514%)E-3 Agreement 0735 hrs I-133 (7.47 0.05)E-4 (7.25 8%)E-4 Agreement 6-27-90 I-134 (6.4 0.3)E-3 (5.98 5%)E-3 Agreement 1st Count I-135 (1.90 0.03)E-3 (1.8817%)E-3 Agreement (Chemistry analysis)

w Reactor Waters 'I-131 (5.510.2)E-5 (5.518%)E-5 Agreement 0735' hrs I-133- 

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   (7.70 0.06)E-4
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    (9.24 5%)E-4 Agreement 6-27-90 I-135 (2.1210.10)E-3 (2.2314%)E-3 Agreement
 ~2nd Count (Chemistry      i-analysis).

F Offgas Kr-88 (8.6 0.3)E-3 (8.09 7%)E-3 Agreement Recombiner Xe-133 -(2.62 0.06)E-3 (2.56 10%)E-3 Agreement 6-27-90- Xe-135 (1.386 0.011)E-2 (1.25 8%)E-2 Agreement 5 hr Count (Chemistry analysis) o Main Stack Ba-140 (3.110.2)E-12 (4.2 0.9)E-12 Agreement Particulate Filter 0810 hrs 6-28-90 (health physics detector #1) ' ': ' 

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Pilorim Verification Test Results ' 

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  ',  SAMPLE -- ISOTOPE NRC -VALUE -- LICENSEE VALUE  COMPARISON; .
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lS , 3 Results in Microcuriec #- 

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Main Stack- I-131 (2.6110,14)E-11 (2.31 0.08)E-11: Agreement ! 4, .  ; Charcoal' -I-133 -(4.3 0.2)E-11 ' ( 3. 6810.13) E-11 - Agreement-P'

s Cartridge; N, L ~0810. hrs 

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e ' ' ' r Liquid _ Radio- Mn-54 (8.3 0.3)E- (8.010.4)E-6- i Agreement: 

  ^ active ~ Waste -Co-58 (1.5410.02)E-5 (1.50t0.04)E-57  Agreement
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1424 --hrs : _ Co-60 _(4.74 0.04)E-5 ~(4.7910.08)E-5 -Agreement 

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6-27-90 Ba-140 (2.03 0.07)E-5 (2.1810.13)E-5- Agreement .: 

'1  -(health ~ physics Na-24 (1,80 0.03)E-5   ' Agreement
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       (1.7710.10)E-5-detector #1)

  < Stack Gas; -Kr-85m ~(4.310.3)E- ( 5. 010. 3)' E-7 Agreement-0920 hrs-  Xe-133 (1.83 0.06)E-6_- ~(1.68 0.07)E-6  Agreement :

6-27-90 4 

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L(health physics-detector #2)- g Stack Gas Kr-85m .(4.2 0.3)E-7 _ (4.010.2)E2 Agreement :! g- :1452_ hrs Xe-133 (l.65 0.09)E-6 -(1.6210.07)E-6 ' Agreement 1 6-27-90 

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5 Crud _ Particulate 1 Cr-51- -(9.0 0.3)E-5 (9.310.3)E-5 Agreement Filte Mn-54 (3.03 0.06)E-5 (3.6110,07)E-5- . Agreement' , 0800 hr Co-58 '(2'60 0.07)E-5 

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       ( 2. 9410.'07 ) E-5 Agreement-
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l6-26-90- Co-60 (5.24 0.08)E-5- ,(6.0810.09)E-5 Agreement- 

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TABLE II I Pilgrim 

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     ' Chemistry Test Results te
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  ~ Chemical'  Method of NRC- -Licensee . . Ratio  i
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  ; Parameter _ Analysis * :Known Value Measured Value  Comparison: '
       (LIC/NRC)

Results in parts'per billion'(ppb).

~ Silica SP 4914 54.41 .11i0.09 Quali fied-- '! Agreement-11012 10813: 0.9810.03 . Agreement = 16113 16416- 1.0210.04 Agreement.' 

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TCh1or u IC , 3012 29,11 .97 0.06 Agreemen l 48 3- 44.61 .93 0.06 Agreemen . 9.5 .41 .99 0.06 Agreement-

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7 , _ Sulf ate'- ~I .6i .010.2 . Agre "nent - 

,      .30 2 29.8910.14 '1.0010,07 = Agreement: ci 6.0 .9220.06- 0.99t0.07 Agreement-

Fluoride: <IC 2412 21.2 .8810.07 Agreement 

,e     '37.011.5- 36.51 .99t0.04 : Agreement- -

7.41 ,69t0.04 1.04t0.04' Agreement * Results in=part-s per million (ppm) Iron: ICPT 198'3 199t3 1.00 0'.021 ' Agreement-392 10 413 3 l'.0510.03 Agreement 580110 61717 1.06 0.02- Agreements - 

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[  L Copper-;  ICP 1 19914 21516 1.0810.04 Agreement 9'  '

405 3 424t .0510.02- Agreement: 

     '59515- 643 1 .0810.02 Agreement
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Chromium .ICP 200110 217116 1.09 0.10 ' Agreement-40419 44815 1.11 0.03 Qualif.ied e . _ Agreement-60017- 650113 1.08 0.03- Agreemen .i 

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IC = Ion Chromatography 

  . SP L = UV - Vis. Spectrophotometry     .

Tit. =. Potentiometric Titration LICP: = Inductively Coupled Plasma. Spectrometry DCP_ =- Directly Coupled Plasma Spectrometry . ' s 

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l Chemistry Test Results-d', I w Chemical: Method of- :NRC Licensee . Ratio 

,   Parameter- Analysis * Known'Value' Measured Value- (LIC/NRC) Comparison! '

Results!i n parts per million (ppm)  ! 

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  ~ Nickel  ICP- 20315, 230 30 1.1310.15, Disagreement' m
. 40316- 440130 1.0910.02 Quali fied :

Agreement' Li k 610110- 660130 1.08 0.05' 

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3 - Quali fied Agreement 7' Nickel i IC :20315 22915' 1.1310.0 Disagreement- ! 40316 -440 10 1.09 0.03- 

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610110 670!30 1.1010.05 . Disagreement-e Iron DCP: ~19813 1782- -0.90 Qualified * Agreement s ? 392 10 3502 0.89' Qualified Agreement 

    ;580 10 5652 0.97- . Agreement ,
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  -Copper  DCP- 199 4 1912 - 0.96; 1 Agreement ~ j wm     -40513- 3832 0.95 Agreement 1
     ,5892 0.9 ~   _ Agreement /
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 :C Chromium-  =DCP 200110 '2022 1,01: Agreement- ,

40419 4242 .1.05^ Agreemen .04: Agreement 

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  : Nickel  DCP 203 5 1912 -0.94 . Agreement:

40316 3912 0.97_ Agreemen )! 610110 5712 0.94J Qualified: 

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Agreement, ;; y 4 - l NOTES . Reanalysis results after recalibration 2.- Single Analysis Only 

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IC: = . Ion Chromatography SP' = .VV Vis. Spectrophotometry ' Tit. =' Potentiometric Titration - ICP =' . Inductively Coupled P1asma Spectrometry b DCP:'= -Directly Coupled Plasma. Spectrometry 

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   ,    Resultszinpartspermillion(ppmh   [

s b _ LlBoroni Ti . 97.-71 .95 0'02 .' Disagreement  : .211.'1' O.98410.014t 1 Agreement:  : M 255 5 1244.21 .9610,02 _ Disagreement: p "' . 510 10 486.5 _0;9610'.02. - Disagreement' L! 4-. 1030i20- 10201113 248.820.53 0.9910.02 Agreement- 3= 

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4  : E4 .-q ATTACHMENT 1  ; O J* <, CRITERIA FOR-COMPARING ANALYTICAL MEASUREMENTS-1This: attachment lprovides criteria'-for comparing results of capability tests: 

  -and verification measurements'. The criteria are based on an empirical
,

Lrelationship which combines' prior experience and the accuracy needs of this 

  ' progra In'these criteria; the' judgement limits are variabletin relation to the
     -

a comparison of the-NRC Reference Laboratory's value to its. associated ' 

         '
         '
  : uncertainty. As the. ratio, referred to in this program as " Resolution",
  -increases the acceptability of a licensee's measurement should be more   ,
,   : selective. -Conversely,Epoorer agreement must be considered acceptable asith ! resolution decrease ,

Re' solution .

Ratio for Agreement 8- 

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     ..<3- . No Comparison-
     :4 - 7  0.5 - i
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8'- 15 0.~6 - 1.66: 16 - 50 . 0.75 - 1.33 3 51 - 200 0,80 -'1.25 

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     :>200  0.85 - 1.18l 2 Resolution = (NRC Referrace-Value/ Reference-Value Uncertainty)   5
  . 2Rattol== (License' Valur/NRC Reference"Value);    j 1 -
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ATTACHMENT 2-  ! 

        -I
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Criteria- for Comparing Analytical ~ Measurements This attachment.provides criteria for comparing result of capability test j 

"

In'these criteria the -judgement limits are based on-data from Table 2.1' of  ; 

"

NUREG/CR-5244, " Evaluation of Non-Radiological Water Chemistry.at Power Reactors". Licensee values within the plus or minus two standard deviation- ' r, ? range ( 2Sd) of the BNL known value are considered to be in agreement.

E Licensee values outside the plus;or minus two standard deviation range but Lwithin plus or minus:three= standard deviation. range (13Sd) of~the BNL known-values are considered to be in qualified agreement. Repeated results'which 

  .are in qualified agreement will receive additional attentio Licensee value greater than the plus or minus three~ standard deviations range of the BNL
    '
,  known value are in disagreement. -The standard deviations were computed using
 . the average- percent standard deviation values of each' analyte' in Table 2,1.- 1


 ': The; ranges for the-data in Table II are as follows:
 "

Agreement Qualified Agreement Analyte Range Range- i 

  . Silic :

146-176 138-184 Chloride 28-32 27-33 44-51- 

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*       42-53-v
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8.8-1 .5-1 , 

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  ;Su1 fate  -17-21  16-22-27-33  -26-34 5.4- ."2- i
        $

F1ouride 21-27 20-28' 32-42 30-44 i 6.5- " 6.1- . Iron- 179-217' ~169-227 i 354-430 336-448' j 524-636 496-664 i 

 ,
  ' Copper -  180-218  171-227 1
'

366-444 347-463 * 538-652 510-680 L: 

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1 . ._ _ , -Agreemen "QualifiedAgreement- 4 

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4 . m-Chromium ~ '181-219' ' 3 Mibh:. w4 171-229? h ( # f =.x , , 365-443 345-463 ( 542-658: 512-688 4 $ G@w ;r- w. .a * ' 

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1572-648- 553-6671 

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101-105 99-106 9 

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                 .499-521    (494-526 m     1 N&W;     .w-   ,
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250-260 247-263 

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