John E. Regnier John W. Gable, Jr. Joe L. Marsh Departt?ient of Public Health Montgotwr}’,Ala. 36 I30
In 1974. the Congress passed P.L. 93-523, “The Safe Drinking Water Act of 1974.” Section 1401 ( 1 ) of this Act discusses quality control and testing procedures to ensure compliance with Maximum Contaminant Levels ( M C L ) . T h e associated N a tional Interim Primary Drinking Water Regulations, 40 C F R 141 and 142, require that, for compliance purposes. analyses must be performed by a laboratory approved by the state. However, analyses for turbidity and free chlorine residual may be performed by a person acceptable to the stat e. States must establish and maintain a prograni for certification of laboratories conducting measurements of drinking water contaminants. T h e regulations further require that any state accepting primacy under the Act must designate a principal state laboratory or laboratories to be responsible for administering this certification program. Within this broad mandate, the general protocol adopted was for EPA to approve and then certify the principal state laboratories and the state, in turn, to approve and certify local laboratories. T h e concept involved interim approval granted on the basis of administrative review; whereas certification, either interim or final, would require site evaluation, and analysis of performance samples. T h e approval/certification process was to be implemented by June 24, 1977, which corresponds with the effective data of the Interim Regulations. Final certification of all laboratories is to be completed by 1980, which is the expected effective date of the National Revised Primary Drinking Water Regulations. Alabama accepted primacy under the Act, and designated two principal state laboratories-the Environmental Health Administration Laboratory (EHAL) for chemical and radiological parameters, and the Clinical Laboratory Administration for microbiolog40
Environmental Science & Technology
ical determinations. T h e EFIAL. which is a multidisciplinary laboratory serving all environmental prograins under the Department of Public Health, elected to implement a full certi ficat ion program involving site eva I ua t i o n and perform an ce sa in p I e testing immediately, rather than begin with a n administrative approval approach. The aim, here, is to describe that program, particulnrly as it iipplies to chemical determinations, and to present the results obtained during the first year of operation, from June 24. 1977 to June 24. 1978. Hopefully, this information may be helpful to states which may not have accepted primacy, or have not been able to implement a ce r t i f i ca t i on p r og r a ni .
Alabama’s certification program Within A I a ba ni a, respo n s i bi 1it y for implementing t h e S a f e Drinking Water Act is delegated to the Division of Public Water Supplies of the Alabama Department of Public Health, which is established as the focal point for all certification requests. An application for certification, i n letter format, is sent to the Director of the Division of Public Water Supplies, and identifies the laboratory and the parameters of interest. The Director then forwards the request to thc E H A L , clinical laboratory, or both, depending on the parameters for which certification is requested. No fees are charged for in-state laboratories. When a certification request is received by the E H A L , the laboratory certification officer makes telephone contact with the requesting laboratory, and arranges for a mutually convenient time for a site visit and evaluation, During this visit, the certification officer obtains information on the laboratory personnel, facilities, equipment, analytical methodologies, and quality control. This is done according to checklists included in EPA’s Manual for the Interim Certification of Laboratories Involved in Analyzing Public Drinking W a t e r Supplies. Particular attention is given to quality control practices, and to whatever documented evidence of satisfactory analysis of performance samples, supplied through a recognized program such as that of the EPA or the USGS, the laboratory can furnish. These data may be accepted in lieu of
LABORATORY CERTF IC I ATO IN
0013-936X/79/0913-0040$01 .OO/O
@ 1979 American Chemical Society
analysis of E H A L performance samples. If no such data are available, a set of E H A L performance samples for the parameters in question is left with t h e laboratory manager, and any other questions or problems a r e discussed with him prior to conclusions of the site visit. T h e certification officer documents this site visit, in memorandum form, to the Director, Division of Public W a t e r Supplies, with a copy to the laboratory manager.
Here’s how it’s done in Alabama, to ensure that testing methods vi11 be in compliance with the Yafe Drinking Water Act
Performance samples Satisfactor), analysis of performance samples is considered to be the foundation of the Alabama certification program for chemical and radiological parameters. At the inception of the program. capability did not exist for preparation of all radiological performance samples, but samples were prepared for the sixteen inorganic and organic parameters required under the Act. It was felt that if radiological samples \ v u e needed, they could be obtained from EPA, until such time as internal capability u a s developed. Detailed procedures used in the preparation and distribution of these samples are available from the authors on request. Briefly, the procedures involve preparation of stock solutions from EPA-supplied standards for organic samples, and A C S reagent grade chemicals for inorganic samples. Special precautions are followed in the cleaning of all glassware, and cartridge-purified water with a n in-line resistance of 18 megohms is used for all aqueous dilutions. Solvents and prcscrvation techniques a r e chosen to avoid interferences such a s precipitation. Consequently, two solvents in different ampoules a r e required for inorganic and three for organic samples. Appropriate aliquots of these samples a r e dispensed by buret into glass ampoules, which are flame-sealed and blotter-tested for leakage. Initially, the samples wcre prepared in the approximate range of the M C L specified in the Act, rather than higher concentrations, in order to identify any problems which might be encountered with required sensitivity as well a s accuracy, a s soon as possible. Laboratories are given sixty days to complete performance sample analy-
ses. I f they have not responded in this time period, they must reapply for certification, and analyze another set of performance samples. I n the event that any of their results a r e outside acceptance limits, they a r e provided with a second set of samples, and instructed to reanalyze them for the questionable parameters. Results of the second set of tests must be returned within thirty days. If those results a r e still outside the limits, a recommendation is made to the Director, Division of Public Water Supplies, that the laboratory be certified only for the parameters for which it obtained satisfactory results. However, the E H A L will work with that laboratory, if desired, to determine the cause of the unsatisfactory results. Acceptability To be acceptable, results must fall ifithin the range defined by plus or minus three standard deviations of the known value. However, no laboratory will be denied certification because of performance, unless a t least one peer laboratory can produce results within the acceptance limits. Standard deviations on which t o base the limits are derived in two ways. As the performance samples were prepared, the E H A L ran five replicate determinations, and calculated the standard deviations for each parameter. T h e acceptable ranges for the organics and inorganics, except nitrate and fluoride, are based on these values. Standard deviations for nitrate and fluoride results, thus calculated, a r e essentially zero. Consequently, standard deviations based on historical d a t a from EHAL‘s in-house quality control program are used to define the acceptable ranges for these two parameters. Because of the few replicates analyzed, and EHAL’s relative inexperience in organic analyses, resultant acceptance ranges have been rather large in some cases. However, time was not available to permit more replication and meet the mandated June 24, 1977 inception deadline. Out-of-state laboratory requests for Alabama certification a r e dealt with similarly to in-state requests, except that site visits a r e avoided, if possible. I f site visits a r e required, the laboratory must agree to pay expenses inciVolume 13, Number 1, January 1979
41
TABLE 1
In-state applications Bank for
cerllcatbn Laboratories
Parameter
As Ag Ba Cd Cr Hg Pb Se N03-N
F Endrin Lindane Methoxychlor Toxaphene 2,443 2,4,5-TP Gross ct Gross p Tritium E9Sr 22sRa 228Ra 134cs 1311
U Photon emitters a
apptylng for CertiHcatlon
Past
Rrst analy-
analy-
14 15 15 15 15 14 15 14 15 15 10 10 10
10 10 10 2 2 2 1 1 1 1 1 1 1 1
1 1 1 1
1
1 1 1
Includes laboratories that have reapplied for certification.
TABLE 2
Out-of -state-appliiaths Basis for
Se
Lindane Methoxychlor Toxaphene 2,4,5-TP Tritium
Photon emitters 42
Second
Environmental Science & Technology
dent to the visit. Upon receipt of an out-of-state request, the laboratory is contacted to determine if it has been certified by EPA, or by its home state. If so, and such certification includes performance sample analysis requirements as stringent as Alabama's, and copies of pertinent data are submitted, reciprocal certification is recommended. If not, the laboratory is asked to provide E H A L with all of the information normally obtained on a site visit, and is sent a set of E H A L performance samples for analysis. In addition, the appropriate agency in the home state is contacted to obtain any additional information concerning the laboratory which may be available. I f necessary, arrangements for a site visit a r e made at this time. Subsequent to the foregoing contacts and actions, the out-of-state requests are processed in the same manner as an in-state request. N o fees are charged, unless it is deemed necessary to perform a site visit.
How the program worked During the first year of the program, 16 in-state and 8 out-of-state laboratories applied for certification for one or more of the parameters involved. Tables 1 and 2 present summaries of these certification requests for the two laboratory categories according to parameters requested, basis for certification, reasons for non-certification, and numbers of pending and approved requests as of June 24, 1978. Although not noted in the tables, the 16 in-state requests represented 1 federal, 1 state, and 14 commercial laboratories, but no municipal laboratories. The commercial laboratories range in size from a three-man staff to one that employs over 600 people. Eight of the laboratories are associated with consulting engineering firms; the others range from a utility in-house environmental laboratory to a research center associated with a university. N o single in-state laboratory requested certification for all parameters, and one laboratory requested certification for only the radiological parameters. From the tables, it can be seen that only this laboratory and one other in-state laboratory had sufficient existing performance data to be certified, whereas two out-of-state laboratories fell into this category. For those analyzing E H A L performance samples, a majority of the certified in-state laboratories obtained acceptable results on the first attempt for most parameters. However, significant numbers of laboratories did not complete the analyses within 60 days, even though this reporting time
FIGURE 1
Performance sample results inorganic parameters and reported results Chromium
Silver
0.
c 0 .c
0.06
Upper limit
0
i
c
Cadmium
0, 0
Barium
o,'l
0.012
0
0°
Upper limit
1
Known
0 40 0 005
0 36
0 Arsenic
1-1 0.25
0.032 0.030 0.028
Fluoride Upper limit
0 20 0 15
iI. Nitrate nitrogen
Selenium
0
Upper limit
0.80
0.007
0 60
Upper limit
0 005
0 70
. F
0 003
-
L
0
c 0 .c
Lead
Mercury 0 (0.009)
I 0.022 0.020 0.018
0
-
-0
0
Upper limit
I
0.001 1 0 0010 0 0009
Upper limit
Volume 13, Number 1, January 1979
43
FIGURE 2
Performance sample results organic parameters and reported values 2,4-D
Endrin Upper limit Upper limit
0.00015 0 00010 0.08
0.00005
; ;
F c 9
.4-
+ 2 c
0
2r
Lindane
Toxaphene
0.0017
2,4,5-TP
Methoxychlor
0.0215
Upper limit
i Upper limit
0.0050
0 0150
was thought to be quite liberal. Predictably, organic analysis capability was less prevalent than inorganic, and i t can be inferred from Table 1 that of the inorganic parameters, arsenic, barium and selenium proved to be the most troublesome. Notwithstanding the difficulty of organic analyses, only one of the certified laboratories in this area required a sample rerun, and for only one parameter-endrin. The results obtained by in-state laboratories for analysis of some inorganic parameters a r e presented graphically in Figure 1 . A normal distribution of results produces a sigmoid curve similar to that for nitratenitrogen. Lead, barium, and possibly fluoride data also seem to follow this pattern. Data for other inorganic parameters appear skewed in some fashion, although, with the limited number of data points, any firm conclusions would be of dubious value. However, the plots for silver and cadmium do indicate that the acceptance limits are unrealistically large; conversely, those for chromium and arsenic are possibly too restrictive. N o explanation is available for the unusual consistency of mercury results, other than that it is probably an anomaly attributable to limited data. Too few organic data were available to evaluate, so Figure 2 is presented only to indicate the relation of the reported values to the limits established. It is expected that these limits will be tightened as experience is gained in this area. As of August, no performance data had been received from out-of-state laboratories, although two had been certified on the basis of EPA, or home-state evaluation. However, a number of these laboratories are currently analyzing EHAL performance samples, and should be reporting data soon.
0 0095 0
0
Lower limit
A surprising finding The first year of this program has been enlightening in several ways. Perhaps most notable was the number of laboratories, particularly commercial in-state laboratories, which applied for certification. It was expected that only a few laboratories in a largely agricultural state such as Alabama would have the necessary equipment and capabilities for the required analyses. However, the site evaluation program has revealed the existence of a surprising number of well-equipped and staffed laboratories, rather than the “garage” laboratories it was feared might spring up in response to the monitoring requirements of the Safe Drinking Water Act. 44
Environmental Science & Technology
The performance of the laboratories has been better than might be expected: the major difficulty was slowness in analyzing performance samples and reporting data. The cooperation of the laboratories has otherwise been quite good. Parenthetically, it should be mentioned that a n Association of Laboratory Analysts has been formed in Alabama, and has provided a n excellcnt forum for disseminating information about the certification prog r a m . Any state beginning a certification effort would be well advised to work closely with a professional laboratory association. if one exists or can be formed. As previously mentioned, the d a t a collected to date have indicated the need for modification of acceptance criteria for several parameters. These modifications a r e currently under evaluation, on the basis of data collected in Alabama. and a recently conducted E P A performance evaluation of state primary laboratories. Table 3 presents a comparison of the acceptance limits used by EPA and the E H A L , and further illustrates the need for adjustment o f some E H A L values. Because these deficiencies were realized, the acceptance criteria were not
rigidly enforced in certification decisions.
would go far t o b a r d minimizing difficulties with such requests.
costs During the first year of operation, the Alabama certification program has required approximately one man-year of effort a t a total cost of $18 950. These costs a r e listed a s follows: Personnel Travel Supplies Samples analysis
$17 000 750 200
1000
T h e average cost for the 23 laboratories which have applied, and have been certified, or are in some stage of processing, was $824 per laboratory. As this program moves into its second year of operation, t u o areas will receive increased attention. These a r e reappraisal of performance sample acceptance limits, and reevaluation of the reciprocity policy for processing requests from out-of-state laboratories. Although this latter area has not caused any significant problems to date, it is felt that as these requests increase, the effort and costs involved in processing them may become prohibitive. T h e authors feel that a consistent reciprocity policy by EPA
John E. .Regnier is a L ' S . Public Health Sercice cormiissioned officer on lociti froni E P A to Alahatira as Director o f t h e Encirontiieiital Health Adi>riiiistratioriLahoratorv. He has been incolued iti direction of radiologicnl rind encirontwntal laborator!' acticitiesjor the past ? I ],ears.
John W. Gable, Jr. ( I ) has h,orked'in enrironniental health f o r I O years. He has been sercitig as the laboratory certification inspector f o r 2 )$ears. J o e L. M a r s h ( r ) is the deputj,director of the Alabania Encironniental Health A d ministration Laboratory. He has been incolred in water and wastewater analysis f o r 8 years. Coordinated by J J
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