ORIGINAL (Red) WORK PLAN FOR PHASE I OF EXTENT OF GROUNDWATER CONTAMINATION STUDY AT CHROMATEX, INC., WEST HAZLETON, PA. Prepared for: Chromatex, Inc. INTERNATIONAL EXPLORATION. INC. 577 SACKETTSFOHD ROAD WARMINSTER. PA 18971-1398 (2 IS) 396-7137 February, 1988
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REVISED WORK PLAN FOR PHASE I OF EXTENT OF … · WORK PLAN FOR PHASE I OF EXTENT OF GROUNDWATER CONTAMINATION STUDY AT CHROMATEX, INC., WEST HAZLETON, PA. Prepared for: Chromatex,
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ORIGINAL(Red)
WORK PLAN FOR PHASE I OF EXTENT
OF GROUNDWATER CONTAMINATION STUDY
AT CHROMATEX, INC.,
WEST HAZLETON, PA.
Prepared for:
Chromatex, Inc.
INTERNATIONAL EXPLORATION. INC.577 SACKETTSFOHD ROAD
FIGURE 2: OPEN HOLE CONSTRUCTION FORCONSTRUCTION FOR SHALLOW WELL . . . . . . 7
FIGURE 3: ALTERNATE CONSTRUCTION FOR SHALLOWWELLS IN INCOMPETENT BEDROCK. . . . . . . 9
FIGURE 4: ALTERNATE CONSTRUCTION FOR SHALLOWWELLS IN INCOMPETENT BEDROCK. . . . . . . 10
FIGURE 5: ANTICIPATED CONSTRUCTION OFMID-RANGE AND DEEP WELLS. . . . . . . . . 13
INTRODUCTION
The following outline is intended to describe the plan of
action for the first phase of an investigaton into the
extent of groundwater contamination by volatile organic
chemicals (VOC) in the vicinity of the Chromatex, Inc. Plant
#2 and a number of homes on Bent Pine and Deer Run Roads in
the Borough of West Hazleton and the Township of Hazle,
Luzerne County, Pa.
The investigation will consist of the drilling of 7 wells
into the shallow phreatic zone, and the testing and sampling
of those wells. The sites of 2 of these shallow wells will
each have 2 additional wells drilled into progressively
deeper portions of the phreatic zone, for the purpose of
testing and sampling those zones and determining the actual
head gradients within the aquifer(s) underlying the site.
This phase of the extent of contamination study is intended
to answer the following questions:
What is the direction of groundwater flow in the
shallow phreatic zone beneath Chromatex Plant #2?
Does a groundwater divide exist in the shallow
phreatic zone beneath Chromatex Plant #2?
What is the degree and distribution of VOC contami-
nation in the shallow phreatic zone?
— i _
What is the velocity of groundwater flow in the
shallow phreatic zone?
What head gradients and hydraulic connections exist
between the shallow phreatic zone and deeper zones
from which local residential wells withdraw water?
The answers to these questions should provide enough
information to allow for a determination as to whether or
not the VOC contamination originated on the property of
Chromatex Plant #2. Other questions that should be
answered, in part, by this investigation are:
- What is the vertical distribution of VOC contami-
nation beneath Chromatex Plant #2?
What are the general hydrogeologic conditions of the
deeper phreatic zones beneath the site, with regard
to aquifers and confining layers?
It should be noted that any estimates and assumptions made
in the following outline are for planning purposes, and are
subject to the feasiblity of their implementation in the
field and the actual geologic conditions encountered during
the investigation.
- 2 -
(fled)
WELL LOCATIONS AND
WELL NUMBERING SYSTEM
The approximate locations of the proposed wells are located
on Figure 1. Well numbers followed by the letters A, B, C
indicate the sites of well clusters, where 3 wells of
different depths will be drilled. Well numbers not followed
by letters indicate sites where a single well will be
drilled into the shallow phreatic zone. On January 5, 1988,
the drilling sites were agreed upon and locations approved
by Richard Dulcey of the EPA and Robert Gadinski of the DER.
The well numbering system used is the same as that
originally developed by Mark Tucker of Weston/TAT. This was
felt to be most appropriate since these well numbers and
their associated locations are firmly entrenched in the
minds of all those involved. To renumber the wells so that
they are all consecutive could cause confusion.
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F I 6 U R E 1
AOWITORIN6 UELL LOCATIONS
Veil
- 4 -
(Ret/;
DRILLING METHOD
Wells will be drilled using an air rotary drilling rig. The
bit will be either a down-hole hammer or tricone, whichever
is most efficient in the bedrock encountered. The use of
water as a drilling fluid will be avoided as much as
possible. It may, however, be necessary at times for the
proper completion of the wells.
CONSTRUCTION DETAILS OF SHALLOW WELLS
These wells will penetrate to a depth of approximately 20
feet below the water table. It is anticipated that they
will be of an open-hole type construction, where an inner,
slotted casing will not be needed to protect against
collapse of the borehole.
The determination on whether or not an open hole
construction will be used , will be made at the time of
drilling. This decision will be based upon the competency
of the bedrock by examining cuttings and by repeatedly
lifting the drill bit out of the hole and re-inserting it to
determine if the walls of the well have caved in.
- 5 -
OPEN HOLE CONSTRUCTION
An 8 inch diameter hole will be drilled to a depth of 15
feet, or 5 feet into competent bedrock, whichever is deeper.
A length of standard weight, 6 inch diameter steel casing
will be inserted into the borehole and seated by pushing on
it with the drilling rig. The bottom of the annular space
between the well casing and borehole will be sealed with
bentonite. The remainder of the annulus will be sealed to
the ground surface by pouring a cement mix into the top of
the annulus. A cement apron will be constructed around the
casing. Steel casing will extend at least 2 feet above the
surface.
Once casing and grouting are completed, the grout will be
allowed to set overnight. A 6 inch diameter borehole will
then be drilled to a depth of 20 feet below the water table.
A schematic diagram of this type of construction is
presented in Figure 2.
CONSTRUCTION OF SHALLOW WELLS IN INCOMPETENT BEDROCK
An open hole construction may not be feasible, if bedrock at
a depth of 20 feet below the water table cannot maintain an
open hole. If this is the case, an 8 inch diameter hole
will be drilled to the total depth of the well. Six inch
diameter steel casing, the bottom 20 feet of which will be
S+tckvp
around Surface(Red)
Cem€flt grout
" Jta.m«t«r ftcct casingin co*t«ttvtt t
t«r
<)iameT<fto to+a.1 J«
laorcvJ Op«n \\o)e Construction for'W«H
- 7 -
slotted, will be set in the borehole. The outside annulus
of the casing will be packed with coarse sand or gravel to a
level approximately 2 feet above the top of the slotted
interval.
The remainder of the annulus will be sealed with
approximately 2 feet of bentonite on top of the gravel,
followed by pouring cement to the ground surface. A cement
apron will be constructed around the casing. Steel casing
will extend at least 2 feet above the ground surface. A
schematic diagram of this type of construction is presented
in Figure 3.
An alternative construction method, using an inner casing of
4 inch diameter slotted steel, may also be used, as outlined
in Figure 4.
All three of these methods will provide a satisfactory well.
The actual method will be decided upon in the field by the
site geologist.
Previous work that has been done in the area by Weston/TAT
indicates that the depth to water in area wells is 20 to 30
feet below the ground surface. Based on this data and the
fact that the monitoring wells will penetrate to 20 feet
below the water table, it is anticipated that their depth
will range between 40 and 50 feet.
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(pay)
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ri-i y
benTon'.tc
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3——benton'.lc
STcel -,ha
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ir Ta-ltef h
4 ^ w*-H$ f
- 10 -
CONSTRUCTION DETAILS OF MID-RANGE AND DEEP WELLS
The depths of these two types of wells will not be known
until some exploratory drilling is actually performed. The
existing residential wells in the area range from 85 feet to
400 feet deep. If geologic conditions permit, it is
anticipated that the mid-range wells will be on the order of
100 feet deep and the deep wells will be on the order of 150
feet deep.
The preliminary purpose of the mid-range wells is to study a
zone of weathered/fractured bedrock, which the EPA/Pa.DER
believe to exist beneath the area, from which some of the
nearby residential wells withdraw water. The preliminary
purpose of the deep wells is to study the less
weathered/less fractured bedrock zone believed by EPA/Pa.
DER to exist at a somewhat greater depth.
In order to attempt a determination of the depths of the
weathered bedrock zone and the less weathered bedrock zone,
well #1OC will be drilled first. Well #10C is the deep well
at one of the two well clusters. At well #10C an 8 inch
diameter hole will be drilled to a depth where the field
geologist believes it has penetrated the less weathered
bedrock. At this time, the borehole will be partially
filled with a cement/bentonite slurry. The casing will then
be set to the bottom of the hole. The bottom of the casing
- 11 -
will be sealed with a cap or plug of teflon to avoid having
the grout mixture enter the casing. The steel casing will
displace the grout mixture and force it to rise up in the
outside annulus to some level, The casing will then be
seated into the bedrock by pushing on it with the drilling
string. The upper portion of the annulus will be grouted by
pouring cement in from the surface, if necessary. A cement
apron will be constructed around the casing. Steel casing
will extend at least 2 feet above the ground surface.
Drilling will resume after the grout has set overnight. The
drilling of a 6 inch diameter hole will continue until a
measureable yield is obtained (approx. 3 gpm or more).
It is anticipated that a short length of 8 inch diameter
casing may be used at the outset of drilling prior to
grouting, to protect against collapse of the upper portion
of the borehole, and in certain areas, protect the
groundwater from possible contamination by perched water and
soil water. A schematic diagram of the anticipated well
construction is presented in Figure 5.
After well #10C is drilled, considerably more data will be
available for use in determining how deep to drill the
remaining deep wells and the two mid-range wells, and where
casing should be set to separate specific aquifers or water
bearing zones.
- 12 -
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Tli'ctr»LH
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f
The mid-range and deep wells are planned to be 6 inches in
diameter. However, if incompetent formations are
encountered after 6 inch casing is set, it may be necessary
to set an inner 4 inch casing, and drill a 4 inch diameter
hole below it into competent bedrock.
NOTES ON GROUTING PROCEDURE
The grouting procedure described for the mid-range and deep
wells is designed to provide an efficient seal at the bottom
of the casing, which may be as deep as 100 feet or more. It
is also designed to use a minimum amount of equipment, thus
facilitating low temperature decontamination procedure.
It is anticipated that the casing depth in the shallow wells
will be shallow enough to allow efficient grouting by
pouring bentonite and cement down the annulus from the
surface. If the site geologist and driller decide that the
casing in any individual shallow well is too deep to be
grouted properly from the surface, grouting will be done
using the same method as described for the mid-range and
deep wells.
Another grouting method, using a tremie pipe inserted down
the outside annulus to inject grout, has been discussed with
EPA personnel. However, the tremie method requires the use
of equipment which may freeze or clog in low temperatures.
- 14 -
It also includes the decontamination of additional
equipment, which could be difficult in low temperatures.
Considering the effectiveness of the proposed grouting
methods, and the potential complications of the tremie
method, it is recommended that the tremie not be used on
this project.
WELL LOGGING
An INTEX geologist will be present at the site during the
drilling of each well. The geologist will observe the
drilling of the well and compile a log describing the type
and thickness of rock layers encountered, depth and yield of
water bearing units and measure the specific conductivity of
the water from different aquifer units. Cuttings will be
collected at 5 foot intervals and stored in plastic bags
labeled with the well number and depth of sample collection.
ELEVATIONS OF WELL CASINGS
Upon completion of the drilling of all the wells, the
elevation of the tops of casings will be surveyed to allow
for accurate measurement of the elevation of the water leveli
in each well. Casing elevations will be keyed to mean sea
level.
- 15 -
PRESERVATION REQUIREMENTS
IF A CUSTOMER IS REQUESTING A GROUP OF ANALYSES, SPECIAL SAMPLING CONTAINERS MUSTBE UTILIZED FROM EACH GROUP (UNPRESERVED, ACID, CAUSTIC, ETC). PLEASE REVIEW THEPARAMETERS REQUESTED AND SELECT THE APPROPRIATE SAMPLING CONTAINERS.
EXAMPLE: A CUSTOMER IS REQUESTING AN ANALYSIS FOR PH, CADMIUM, AND AMMONIATHEREFORE, THE FOLLOWING CONTAINERS SHOULD BE COLLECTED:
TABLE 1 SAMPLING AM) PRESERVATIONTECHNIQUES FOR INORGANICS AND ORGANICS
1 PRESERVATIVE
HN03 to pH <2
HN03 to pH <2
HN03 to pH <2
Cool to kC
HN03 to pH <2
HK03 to pH <2
HN03 to pH <2
HN03 to pK <2
HN03 to pH <2
KN03 to pH <2
HK03 to pH <2
KNG3 to pH <2
HN03 to pH <2
HN03 to pH <2
HN03 to ph! <2
KN03 to pH <2HN03 to pH <2HN03 to pH <2HN03 to pH <2
HN03 to pH <2
HNOJ to pH <2HN03 to pH <2
Cool to ^CCool to ^C
Cool to kCP,G
P.G
G only
Cone. HZSOJ4 toPH <2
HN03 to pH <2Cool UCNAOH to
MAXIMUM HOLDING TIME
6 months
6 months
6 months
7 day6
6 months
6 months
6 months
6 months
6 months
6 mon ths
6 months
6 months
6 months
6 months
3? days14 days6 months
6 months6 months
6 months
6 months6 months
6 months2*t hours
7 days
28 days
1*4 days
6 months2^ hoursCool UC NAOH to 2
pH 12 (-65 AscorbicAcid if Residual Chlorine)Cool. kC PO^ to 2k hoursn < -1.0pn
- r- i n
Page 3
CONTAMINANT
TABLE I ( c o n t ' d ) SAMPLING AND PRESERVATIONTECHNIQUES FOR INORGANICS AND ORGANICS
CONTAINER PRESERVATIVE MAXIMUM HOLDING TIME
ALUMINUM
pH
TU7'3IDITY
FREE RESIDUALCHLORINE
CCrOUCTIVITY
TOTAL ORGANICCARBON
CO^OR
HARDNESS
ACIDITY
STLFATE
I'r-'-'N
K,- '-'3ANESE
PVTASSIUK
BROMIDE
CHLORIDE
r;: TRITE
CrlROKIUM(hexavalent)
B'-O
COD
AXMON1A
C1L ANT) GREASE
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
PiG
P,G
P.G
P,G
P,G
P.G
G only
HN03 to pH <2
Cool to ^C
Cool to AC
Cool to AC
Cool to AC
Cool to AC,H2SO^ to pH <2
Cool to AC
Cool to AC,HN03 to pH <2
Cool to AC
Cool to AC
HK03 to pH <2
HH03 to pi: <2
HN03 to pH <2
KN03 to pH <2
Cool to AC
Cool to AC
Cool to AC
Cool to AC
Cool to AC,H SO^ to pH <2
Cool to AC,tLSO^ to pH <2
Cool to AC,
6 months
6 hours
7 days
2^ hours
2A hours
2^4 hours
2A hours
7 days
2^ hours
7 days
6 months
6 months
6 months
6 months
7 days
2k hours
2^4 hourc
6 hours
7 days
2^4 hours
2*4 hoursH BO. to pH <2
P = plastic
TABLE I (cont'd) SAMPLING AND PRESERVATIONTECHNIQUES roil INORGANICS AND ORGANICS '•
CONTAMINANT CONTAINER
DETERGENT (ABS/LAS) P,G
TOTAL KJELDAHL P,GNITROGEN
SILICA P only
HYDROGEN SULFIDE P,G
PETROLIUM G onlyHYDROCARBONS
NON7ILTERABLE RESIDUE P,G(SS)
SULFITE P,G
VOLATILE RESIDUE P,G
PHOSPHOBUS TOTAL P,G
ORTHO PHOSPHATE P,G
E P EXTRACTIOK G only
DISSOLVED OXYGEN (D.O.) G only
ODOR G only
SETTLEABLE SOLIDS P,G
PRESERVATIVE
Cool to 4C
Cool to 4C,H SO. to pH <2
Cool to 4C
Cool to 4C add /AcetateO
MAXIMUM HOLDING TIME
24 hours
7 days
7 days
2^ hours
Cool to 4C,H SO^ to pH <2
Cool to 4C
None
Cool to kC
Cool to kC
Cool to "ItC
Cool to kC
None
Cool to 4C
Cool to *+C
24 hours
7 days
Analyzed on site
7 days
7 days
24 hours
14 days
Analysed on site
24 hours
24 hours
"P = plasticG = glass
Page
TABLE I ( con t 'd ) SAMPLING AND PRESERVATIONTECHNIQUES FOR INORGANICS AND ORGANICS
CONTAMINANT
PESTICIDESPCBs method 608
CHLORO-PiENOXY-HER3ICIDES :
CONTAINER
VOLATILE ORGAN ICSby method 62k
BASE NEUTRALS,ACID EXTRACT-ABLES (includesPESTICIDES andPCBs) by Method 625
TOTAL T2IHALO-KETHAKES (TTHK)
withFoil or Teflonlined cap. Storein dark, at UC.
Glass with Foilor Teflon linedcap. Store indark, at kC.
storeat
Glass with Foilor Teflon linedcap. Store indark, at kC.
Glass'1 ; store indark at kC.
PRESERVATIVE
None
MAXIMUM HOLDING TIKE
None
NaZS203
None
.COS?.' NA2S20?
7 daye1
days
7 days
23 days
stoppered and refrigerated extracts can be held up to >0 days.
ml. vial with Teflon backed rubber septa; See Part I subsection A. on Pageof this manual for sampling instructions.
•'"When the analytes of concern fall within two or more categories, the samplemay be preserved by cooling to ^C, reducing residual chlorine with .OOS fcNa2S203 (only if residual chlorine is present), storing in the dark, andadjusting pH to 6-9.
days after extraction
B. SAMPLING INSTRUCTIONS
Sampling procedurer, are an followr. :
1) Microbiological - The top must be free of oeratorc,strainers, those at tachments and wnter purif icat iondevices. The faucet is flame t rea ted , using a portableburner or pocket lighter. The water is then allowedto flow for 3 to 5 minutes to clear the service line.Samples are then collected in specially prepared, Gter-ilized bottles (120 ml or approx. A o z . ) and are to befilled only 3/^ full (this allows room for mixing thesample when it is run). The bottles are prepared tocontain Na-thiosulfate which neutralizes any chlorinepresent. A chlorine residual test should be run at thispoint, and the results recorded on the Q.C. sample report.
If the faucet is constructed of plastic or containsplastic parts, then the sampler should eliminate the flametreatment. All sampling is done in on aseptic manner. Ifthere is any doubt about the integrity of sample thesampler is obligated to discard the sample and resample.At this point , a sample report and a sample tag are filledout with all relevant data. The tag is then attached tothe sample container. The sample is iced immediately andtransported to the laboratory for analysis.
If a customer conducts his or her own sampling, a copy of"DIRECTIONS FOR TAKING A WATER SAMPLE" is forwarded to himor her along wd th a sterilized sample container. KLease re-fer to Appendix C for the documentation of the Sampling In-structions.
2) Chemical - All chemical sampling that is required can followthe microbiological sampling without any other preparation.If chemical sampling is the only requirement then followthe same procedure used for microbiological sampling exceptflame treatment can be eliminated. Bottles that containpreservatives must be filled to about an inch from the topso that the sample will contain the proper ratio of sample topreservative. Remember Sample bottles that contain pre-servatives must not be prerineed before filling them withthe sample (only pre-rinse sample bottles that contain nopreservatives).
B. SAMPLING INSTRUCTIONS (cont'd)
Note: Samples for volatile organic analyses must bein a special bottle. The bottle has a 4O ml capacity witha rubber teflon backed septucc and a black plastic screw downlid. These bottles are specially prepared in the laboratoryto contain Na-thiosulfate (O.OOSst). Each bottle should befilled just to briming over without prerinsing. The rubberteflon backed septum is slid over the top of the bottle(teflon surface toward the water). The black plastic portionof the lid is then carefully screwed down on the bottle tocomplete the seal. The bottle should then be inverted to checkfor air bubblec. If there are bubbleo present the sample shouldbe discarded and a new one prepared.
C. CHAIN OF CUSTODY
This section lists the procedure that is utilized to maintain theintegrity of all samples, (i.e. the tracking of samples from theirreceipt, through analysis and disposal of finished samples).
Q.C. Laboratory has a two phase system of sample control. The firstis a procedure that is followed when it is known that a particularsarnple might be the basis for enforcement or litigation. The secondis a similar but less stringent procedure that IE followed for fillother samples. The procedure for strict sample control used isbased on the requirements that can be found in the "Manual for theCertification of Laboratories Analyzing Drinking Water", Chain ofCustody, pages
Tne procedure for the strict chain of custody is as follows: Whena sample is collected by a Q.C. Laboratory field representative heor she fills out a Q.C. sample report (see Appendix A). This samplereport serves ae a chain of custody record for bacteriologicalsamples throughout the entire testing procedure from beginning toend. For Chemical samples however the sample report serves as achain of custody record until trie sample reaches the laboratory.There is an additional form that is used ae a record for thesample after it has re-ached the Lab. Thie form is entitled"CHAIN OF CUSTODY RECORD", (see Appendix D).
A laboratory custodian has been designated who will receive samplesfrom a field representative and there—after take full responsi-bility for insuring the integrity of the samples. Nicolette Holthae been designated with this responsibility. Two alternates havebeen designated to assist in her absence; they are Roy Cohen andJuttn Fieeal.
The custodian or the alternate will receive all samples. The cus-todian or the alternate will accept responsibility for the samplesby signing or initialing the field report. The time and date of thetransfer will be recorded. If the person accepting the samples is
Page 8
C. CHAIN OF CUSTODY (cont'd)
not certain of the integrity of a sample he or she will rejectthe sample and schedule a resampling. The custodian is res-ponsible for logging in all of the Eair.plcc. The samples arelogged into a permanently -bound book. The custodian will recordall oertinent information about the eamyle. The custodian willinclude a unique sample number, the dflto the samule is received,the identification of the sample (the name of: company, homeowner, water supplier etc.), and a list of the individual chemicalparameters that are required (space is reserved for the analyticalresults) .
At the same time the cuctodian will fill out the "CHAIN OF CUSTODYRECOKD". This forr; will serve as a written record of the movementsthat the sample will take through the laboratory (in most casessamples will have to be analyzed by several departments and thesamples will be handled by many people). The record will givethe sample identification, the lab. ident. number, a descriptionof the sample, and the signature of the custodian along with thetime and date of accepting the sample custody. The report willalso contain a written record of who removed the sample from thecustody area, when it was renoved, when it.was returned and finallywhen the sample was destroyed. All laboratory personnel who usethe sample will be initialing this form, showing that e transferof custody took place. Laboratory personnel using samples areresponsible for preserving the integrity of all samples when thesamples are in their possession.
The sample custody area in the laboratory is a secured walk-in typerefrigerator, located in the Dairy Micro. Area. All sample dis-tribution from this area is done only be the custodian or thealternate. Samples that are finished and are to be destroyed, arereleased only by the custodian or ajternate (this might includebacteria samples that have exceeded the 30 hour holding time limit).When samples are destroyed the sample tag is saved and retainedas part of Q.C. Laboratory's permanent written record. All recordsare kept for a period of five years.
Routine samples that are not going to be used for litigation pur-poses are handled differently. The samples are written up in aseparate bound book that is kept by the water chemistry department.These samples, unless refrigeration is required, are stored in thewater chemistry lab. Analysts are free to use these samples withoutcustody transfer but they are still responsible for maintainingsample integrity.
Page 9
C. CHAIN OF CUSTODY (cont 'd)
The Q.C. Laboratory sample tag will remain attached to the sampleuntil the sample is destroyed. The tag will act ac the sampletracking form in conjunct ion with the chziin of custody form. Atthe time of disposal of finished suraplec the sample tag is savedand retained as part of Q.C. Laboratory ' 6 permanent records. Therecords are kept for a period that exceeds five (5) years.
PART II INSTRUMENT OPERATION ANT) CALIBRATION1 AND ANALYTICAL PROCEDURES
A. INSTRUMENT OPERATION ANT) CALIBRATION
1) Analytical Balances
Q .C. Laboratory has several analytical balances. For acomplete procedure for the operation of all balances, pleasesee the individual balance operations manual supplied bythe manufacturer of the balance. These manuals are keptin a close proximity to each balance.
Quality assurance requirements for all analytical balancesutilised are as follows:
a. The balances roust have a sensitivity of 0.1 mg.b. The balances must be mounted on a secure tsble.c. The balances are checked and adjusted annually
by a Metier service person and the dates are re-corded in a log book.
d. The balances are checked once a month using atleast two class "S" weights. These weights mustbe detected to the nearest O.I mg. The dates onwhich the checks were performed , the name of theanalyst and other pertinent information is recordedin a log book.
e. All balances shall be kept clean at all times.f. Before the balance is used, the balance level and
the zero adjustment nrost be checked.g. Semi-annually the accuracy of the balances is
checked using a 10O mg weight under a load of lOOg.The procedure is outlined below:
1. Turn pan release to position 1/H and placea lOOg class "S" weight on the balance pan.
2. Set the weight control knob to lOOg andthen turn the pan release to position 1.
3. Optical scale should come' to rest at theexact zero point (if greater or less thanlOOg adjust the scale expansion using theknob adjustment on the top of the balance)
Page 10
A. INSTRUMENT OPERATION ANT) CALIBRATION Analytical Balances ( con t ' d )
*4. Repeat thic procedure two or three timesto check the reproducability of balance.
5. Place a dace "S" 100 mg weight on thebalance pan.
6. Set the weight control knob to O.lg.7. Turn the par. release to position 1 and
set the balance to the zero point withthe optical zero knob.
8. With the balance released, slowly turnthe weight control knob back to zero.The optical scale should come to restexactly at lOOrag.
9- If the reading is greater than or lessthan lOOrog, arrest the balance and ad-just the sensitivity with the knob on thetop of the balance.
10. Repeat step 3, two or three times.11. Place lOCtag and lOOg class "S" weights
on the balance pan.12. Set the weight control knob to 100.Ig.
Release the balance and set the zeropoint with the optical zero knob.
13. With the balance released, slowly turnthe weight control to the lOOg. position.
1^. If the balance does not read lOOg +/-O.lrr.g repeat the procedure 2 or 5 times.
15- If the sensitivity cannot be corrected callKettler repair service.
16. A record of all load tests is placed ina bound book along with the date of the testand the initials of the analyst who performedthe test.
2) Pan Balances
Q.C, Laboratory has several pan balances. For a complete pro-cedure for the operation of all balances, please see the in-dividual balance operations manual supplied by the manufacturerof the balance. These manuals are kept near each balancefor easy reference.
Q.C. Inc. policy requires all pan balances to meet the followingcriteria:
a. Balances are checked once a month using at least twoclass "S" weights (5g ajl(^ 5Og). These weights mustbe detected to the nearest .01 grams. The dates onwhich the checks were performed, the narae of analystand other pertinent information must be recorded in alog book.
Page 11.
A. INSTRUMENT OPERATION1 AND CALIBRATION Pan Balances (cont'd )
b. Balances arc checked and adjusted annually by aMettler service person and the dates are recordedin a log book.
c. Monthly the accuracy of the balances IB checkedunder a load of (ICOg and l^Og); the procedure isoutlined below:
1. Check the level of the balance on the levelgauge .
2. Turn the balance on and check the focusand alignment.
3- Zero the balance with the optical scale usingthe zero knob.
b. Place l^Og of weight (class "S") on the pan.5- The balance should read exactly If&g (if it
is greater or less than 15Qg then adjust thescale expansion ) -
6. Sot the weight control knob to 15Qg.7- The optical scale should come to the exact
zero point.8. Repeat this process 2 or 3 times.y. Place 1 0. Ig of weight (class "S") on the pan.
10. Set the weight control knob to l^O.lg, theoptical scale should come to rest at exactlyzero.
11. Remove 0-lg (1OD nig) and replace several timesto insure sensitivity.
12. Kepeat steps ^ through 11 using ICOg(class "S") weights.
13. If accuracy or eenoi tivity problems are noted ,and they cannot be corrected , then call aMettler service person.
1*4. A record of all load tests is placed in abound book along with the date of analysisand the initials of the analyst.
3) Thermometers
The accuracy of all thermometers is verified by comparing themwith an NBS certified thermometer. The verification is doneyearly and the following [information ie recorded in a bound book:
a. Each thermometer is given a unique identificationnumber that is recorded along v/ith the identificationnumber of the NBS thermometer.
b. Deviations from the KBS thermometer are recorded.c. The dates on which the verifications axe done are recorded,d. The initials of the analyst doing the verification are
aleo recorded.
Page 12
A. Instrument Operation & Calibration (cont'd)
1+) PH Meter (Corning)
Q.C. Laboratory has several different pH meters. The followingdiscussion outlines the calibration of one model and the nextsubsection outlines the calibration of a second model. Referto the specific operations manual for the instrument that youare using for detailed operation instructions. For easy reference,the operations manual for each pH meter is kept in the sameroom as the pH meter.
a. Each pH meter utilized meets the following criteria:
1. The accuracy of the pH meter is within •+/-.05 pH units.
2. The readability of the meter is within +/-0.1 pH units.
b. The protocol for operating the pH neter is listed below
1. The electrodes are rinsed well with laboratorypure water after each reading.
2. The electrodes are dipped several times intothe next sample before the readings are taken.
3. All sampleE are stirred during measurement,using a magnetic stirring plate and a magneticEtir bar.
*r. The electrodes are stored in laboratory purewater or in pH 7-0 buffer solution as suggestedby the manufacturer.
5- The pH meter is not used or stored on a metalsurface.
6. Commercial buffer that are used are dated whenreceived.
7- Quarterly the pH meter is checked with EPAknown standards and/or ERA Aeeoc. known standardsThe data is recorded in a bound book.
o. The pH meter is calibrated before each use with two bufferstandards bracketing the values to be measured, (i.e.U.O and 7-0 buffers).
1. Place the electrodes first in a solution ofbuffer 7-0 and stir gently.
2. Uhen the meter has etabiliz-ed, (meter does notcnange), adjust the reading to read 7-0 usingthe calibrate knob.
13
A. Instrument Operation & Calibration PH Meter (cont'd)
J. Next remove the probe from the buffer, andrinse with distilled water. Carefully dab theprobe dry with a tissue to remove excess waterand place the probe into the next solution pH^.0 buffer.
^. Stir Eently until n constant value is arrived at.5- Adjust the meter to ^.0 using the slope knob.
(Warning if you must adjust the value more than0.2 pH units, there may be a problem with the probeand/or tne pH meter.
d. A daily check is made of the meter after this calibra-tion has taken place- The procedure is as follows:
1. A pH 7-0 buffer is used. The probe and meterare adjusted to this buffer.
2. Next, without further adjustment, a A.O bufferand a 10.0 buffer are measured and the valuesare recorded in a bound book.
5) PH Meter (Radiometer)
The Radiometer pH meter is standardized using the same basicprocedure as vi th the Corning ncter (the same buffer solutionsare used) but the operation of the rr.eter is different. The Radio-meter pH meter is an automated instrument; the r.eter is programmedto calibrate by the press of a button. The procedure is out-lined in the following steps:
a. First place the probe in the pH buffer 7-0.b. Prese the calibrate pH button to start the
calibrate mode function.c. After stirring and stabilization of the pH
meter (a constant value is acheived) press thecalibrate pH button again. This sets the meterto the value of pH 7-0.
d. A prompt or. the pH meter next tells you toplace the p'H probe in second pH buffer solution.(choose a buffer that will enable you to bracketthe pH of the samples that you will be measuring)-
e. As an example, choose a pH *+.0 buffer, and placethe probe in that buffer (take care to rinsethe probe with distilled water between buffersand dab dry with a tissue). Next stir gently untilG constant value is achieved.
Page
A. Instrument Operation R Calibration PH Meter ( c o n t ' d )
f. When the meter ie stable press the cali-brate pH button again. This sets the pH meterto the value of the b u f f e r (in this cese *+.0).
g. Finally press the button labeled pH to go intothe read mode.
h. Place the pH probe into a sample, stir, andwhen a constant value is achieved record that value
i. Always rinse between samples with either lab.pure water or the next sample to be measured.
3. All pH meters are checked monthly using EPAand/or EJiA Assoc. known standards.This data is recorded in a bound book.
6) Conductivity Meter (Radiometer)
a. Maintenance
1. The probe itself ic rinsed with distilled wateronly (use no de te rgen t ) .
2. The instrument is checked with a .01 Molar KC1standard daily (.?^52g KC1 to 1,000 ml). Re-sults must not deviate by more than ICXfc fromthe true value of 1,1+08 mnhos at 25C.
3- The cell, when not in use, is left soaking indistilled water.
Measurement
1. The probe raust be rinsed, with the sample orstandard that is to be read, three times beforea reading is initiated.
2. Place the probe into sample and stir with amagnetic stir bar and a magnetic stir plate.
3- Samples are automatically temperature compensated.**. Once the meter has stabilized take the value on
the meter as your reading.5. The meter is checked monthly with EPA and/or
ERA known reference standards. These results arerecorded in a bound book.
6. Daily the conductivity of the laboratory purewater is checked and recorded in a bound book.
Page 15
A. Instrument Operation & Calibration (cont'd)
?) Refrigerators (walk-in type) and (upright household type)
Q.C. Laboratory har- two walk-in type refrigerotors and severalupright kitchen type domestic refrigerators. Tne walk-inrefrigerators are used for saraple storage and the upright re-frigerators are used for both sample and reagent storage. Allrefrigerators will maintain an internal temperature 01 1-^.^C.A thermometer with at least 1 degree C. increments is used ineach refrigerator. The bulb of the thermometer is kept submergedin a flask of water. Each refrigerator has two temperaturepositions that are monitored, that is, a high and a low position.Q.C. Laboratory has an upright refrigerator that is designed tobe explosion-proof. This refrigerator is used to store reagentsthat are flammable; it sometimes is used to store flammablesamples (i.e. haz-ardous waste samples). This refrigerator main-tains an internal temperature equal to the other refrigeratorsand the temperature is monitored using a thermometer of equalspecifications.
a. Q.A. for all refrigerators consists of the following:
The temperature of all refrigerators ismonitored each day. The results are recordedin a bound book." If the temperature of anyrefrig. is found to be outside of the allow-able limits the analyst will report the con-dition to his supervisor immediately. Thesupervisor will'immediately investigate thediscrepancy and if the problem is not correct-able he or she will report the condition to theQ.A. supervisor. The Q.A. supervisor will takeimmediate steps to correct the problem.
8) Magnetic Stirrers
Q.C. Laboratory has several magnetic stirrers. They are pur-chased from many different manufacturers. All [nagnetic stirrersare variable speed and all stirring bars that are used in con-junction with them are coated with inert teflon.
9) Hot Plates
Q.C. Laboratory has several hot plates all of different manufactureAll hot plates have selectable temperature controls.
10) Drying ovens
Q.C. Laboratory has three mechanical convection ovens. Each ovenhas selectable temperature control from room temp, to l80C. Theovens are predominantly used at one set temperature (i.e. one iskept at 105C, one is kept at 1>OC, and one is kept at l80C).
Page 16
A. INSTRUMENT OPERATION ANT) CALIBRATION Drying ovens Ccont'd)
a. Q.A. for all drying ovens is the following:
The temperature of all drying ovens is monitoredwith thermometers. The thermometers used must becapable of reaching at least l80C, they must begraduated in at least 1 degree C increments, andthey are used with their bulbs submerged in a beakerof sand. The temperatures of the ovens, on the daysthat they are used, are checked and recorded in abound book.
11) Centrifuge
Q.C. Laboratory has two centrifuges. See the manu-facturers operations manual for instructions for usingeach one. All centrifuges are capable of holdingcentrifuge tubes with at least a 15 ml. capacity. Onecentrifuge can hold tubes with a capacity of 1^0 ml.
12) Desic-catorc
Q.C. Laboratory has several portable desicoators aswell two stationary desiccatorB. All desiccators con-tain a moisture absorbing material (desiccant). Thetype of desiccant used must be appropriate for the partic-ular task being performed. See individual methodologiesto determine what absorbant (deniccant) to use.
15) Laboratory Glassware
Q.C. Laboratory uses only borosilicate glass-glassware.This type of glassware is resistant to damage by heat,chemicals and repeated use. All volumetric glasswareused is Class A. Graduated cylinders, beakers, andflasks used are accurate to within +/- 5%. Seriologicalor Mohr-type pipets are not volumetric pipets and arenot to be used in tests or analyses that requirequantitative sample transfer and measurement. Bottlesfor storage of reagents and standard solutions must aleobe of borosilicate glass. Polyethylene bottles may beused for this purpose.
a. Glassware Cleaning Procedure (General)
The cleaning procedure will vary depending onthe specific glassware use. For general app-lications glassware is first cleaned -with detergentQ.C. Laboratories uees Fisherbrand "Sparkleen" ora suitable substitute. Glassware Is next rinsedwith tap water several times, followed by
Page 17
A. INSTRUMENT OPERATION A?H3 CALIBRATION Glassware (cont'd)
rinses with lab. pure water. ^lasswnre thatdoes not come clean after this process iscleaned with chromic acid cleaner and rewashedric above.
b. Glassware Cleaning Procedure (Pipets)
Pipets are washed using the same detergent asgeneral glassware- Pipets are washed howeverin a nalgene auto-p ipet washer. FipetE thatdon ' t come clean after this process are cleanedwith chromic acid clearer and then cleaned againusing the above process.
c. Glassware Cleaning Procedure (Special Purpose-Or gardes)
When the particular analysis required is forsamples containing residues in the parts perbillion range, the preparation of scrupulouslyclean glassware is mandatory. Failure to do socan lead to a myriad of problems in the inter-pretation of the final chromatograms due to thepresence of extraneous peaks resulting fromcontamination, or contamination of the analyteof interest. Particular care must be taken withglassware such ac Kuderna-Danish flasks , evap-orative concentrator tubes, or any other glass-ware coming in contact with an extract that willbe evaporated to a lesser volume. 1'hc processof concentrating the pesticide in this operationmay similarly concentrate the contaminatingsubstance , resulting in extraneous chroma togxaphicpeaks that , in extreme cases , may completely over-lap and mask out the pesticide peak pattern.
Although chemists do not all agree on proceduraldetails in the cleaning of glassware, the majorityare in agreement regarding the basic cleaningsteps. These are :
1. Removal of surface residuals immediatelyafter use. As soon as possible after use ofglassware coming in contact with knownpesticides (i.e., beakers, pipets, flasks orbottles used for standards', the glassware shouldbe acetone flushed before placing in the hotdetergent soak )..
Page 18
A. INSTRUMENT OPERATION AKP CALIBRATION Glassware (cont'd)
2 - Hot soak to loosen and flotate mostof soil. The hot soak consists of abath of detergent (sparkleen) in waterof 5O°C or higher. The .detergent powderor liquid should be entirely syntheticand not a fatty acid base- There arevery few area G of the country "where thewater hardness is sufficiently low toavoid the formation of some hard waterscum resulting from the reaction betweencalcium and magnesium sal ts with a fattyacid soap. This hard water scum or curdwould have an affinity particularly forthe chlorinated pesticides and, beingalmost wholly water insoluble, woulddeposit on all glassware in the bath ina thin film.
Note : Certain detergents, even in tracequantities, may contain organics that willcontribute, significant background contam-ination by electron capture detection.For this reason any detergent selectedshould be carefully checked to ensurefreedom from such contamination. Thefollowing procedure is recommended:
Add 25 ml dist. water, previously checkedfor background contaminants, to a 2^0ml sep funnel . Add 1 drop of the liquiddetergent (50 tug if in powder form),followed by 100 ml hexane. Stopper funneland shake vigorously for 2 minutes. Allowlayer separation, draw off and discardaqueous layer. Add a pinch of anhydrousNa2SO^ to the hexane extract and shake 1minute. Transfer extract to a Kuderna-Danish assembly fitted with a 10 ml eva-porative concentrator tube containing one3 mm glass bead. Reduce extract volumeto ca,3 ml in a hot water bath. Cool,rinse down ground glass joint and aidesof tube with hexane, diluting extract toexactly 5 °J- • Stopper tube and shake onVortex mixer 1 minute. Chroraatograph ofGLC, E.G. and evaluate chronvatogram forcontaminant peaks.
Page 19
A. INSTRUMENT OPERATION AND CALIBRAT1OA Glassware (cont'ri)
. Hot water rinse to flush away flotatedBoil.
4. Soak with deep penetrant or oxidizingagent to destroy traces of organic eoil.The most common and highly effectiveoxidizing agent for removal of traces oforganic soils is the traditional chromicacid solution made up of H jSOi} and pot-assium or sodium dichromate. For maximumefficiency, the soak solution should behot (4O° to 50°C). Safety precautionsmust be rigidly observed in the handlingof this solution. Prescribed safety gearshould include safety goggles, rubbergloves and apron. The bench area wherethis operation is conducted should becovered with lead sheeting as spatteringwill disintegrate the unprotected benchsurface.
The potential hazards of using chromicsulfuric acid mixture are great and havebeen veil publicized . •'•here are nowcommercially available substitutes thatpossess the advantage of safety inhandling. These are biodegradable con-centrates wi th a claimed cleaning strengthequcl to the chromic acid solution. Theyare alkaline, equivalent to ca, O.I N NaOHupon dilution and are claimed to removedried blood, eilicone greases, distillationresidues, insoluble organic residues, etc,They are further claimed to. remove radio-active traces and will not attack glassnor exert a corrosive effect on skin orclothing. One such product is "Chera Solv2157", manufactured by Mallinckrodt andavailable through laboratory supply firms.Another comparable product is "Detex" aproduct of Borer-Chemie, Solothum,Switzerland.
5- Hot water rinse to flush away materialsloosened by deep penetrant BOak.
6. Distilled water rinse to remove metallicdeposits from tap water.
7- Acetone rinse to flush off any final tracesof organic material.
Page 20
A. INSTRUMENT OPERATION AKT? CALIKHA7:! ON Glassware (cont'd)
8, A preliminary1 flush of the glasswarejust before using with the same solventto be used in the analysis. There is al-waye a. possibility that between the timeof washing and the next use, the glasswaremay pick up some contamination from eitherthe air or direct contact. To ensure againstthis, it is good practice to flush theit err. immediately before use with some ofthe same solvent thet will be used in theanalysis.
The drying and storage of the cleaned glass-ware is of critical importance to preventthe beneficial effects of the scrupulouscleaning from being nullified. Pegboarddrying is not recomr-ended as contaminantsmay be introduced to the interior of thecleaned vessels. Neoprene-coated metalracks are suitable for such items as beakers,flasks , cnronatographi c tubes , and anyglassware that can be inverted and suspendedto dry. Small articles like stirring rods,glass stoppers and bottle cape can bewrapped in aluminum foil and oven dxiedo short time if oven space is available.Un_ce_r no cirgujpstance should such jsmalliterss be left in the-open without protectivecovering. The dust cloud raised by thedaily sweeping of the laboratory floorcan nest effectively recontaminate theclean glassware.
d. Glassware Cleaning Procedure (Special PurpOBe-Trace Ketals)
This glassware should first undergo cleaningsuch as in section a. lassware Cleaning Pro-cedure (General). This cleaning should thenbe followed by rinses of 1:1 HNOj, tap water,1:1 Hydro chloric acid and finally lab. purewater. If a piece of glassware is known tobe highly contaminated it must be filledwith 1:1 HHO> and allowed to heat on a steam-bath under a hood for 5-10 minutes. The re-maining rinses can then follow (i.e. tap water,1:1 KC1 and lab. pure water). Caution Whendoing trace metal work metal contamination onglassware is ulwavs a persistent problem.The more percautione you take the better off
21
A. INSTRUMENT OPEKATK'K A1O CALIBRATION Glassware ( c o n t ' d )
you will be. A good plan is to segregateall trace metal glassware from general use.)t is also n good idea TO dedicate glasswarefor e i ther low level work and/or high levelwork (low level samples and low level standardGand high level samples and high level standards)
Spectrophotometer (Turner)
Q.C. Laboratory uses a 'Turner Assoc. Model 35° spectre—photometer for inorganic methodologies. Thic unit iscapable of providing a wave length range between UOO and7OO run. It has a maximum spectral band width of no more than20 nit: and has a wave length accuracy between 0 +/- 2-5 nm-The instrument can accomodr te cells that have path lengthsfrom 1-5 err.. A one Xl) en cell path length is normallyused. All cells are kept clean and free from scratches,finger prints, smudges, and evaporated fi lm residues.For specific instructions in the use and standardization
procedures for the spectrophotor.ieter, see the operationsmanual provided by Turner Assoc. This manual is storedwith the Spectrophotometer.
The Spectrophotometer is checked monthly for properoperation. Quality Control uses Oxford Spectro checksolutions for monitorinr . Two solutions are utilised an'dreadings are taken at ^GO, ^50, 510, 550, 600 run. Resultsare evaluated according to the following guidelines:
a. The wavelength of 5^-0 mm is the peak absorbancefor this reference solution. Any change of .03run or more would indicate a change in bandwidth.
b. The absorbance of solution II should be half ofsolution I if not related, the instrument is riotlinear.
c. At wavelengths ^50 and 550 run, a shift in oppositedirections will indicate a shift in wave!engj.hs.
Also a solution of ,l69g potassium chromate in..05 "NaOH.iemeasured at 37** nm (ideal <2$> T) to check instrument forStray light.
The wavelength calibration is checked monthly by using aHolmiuro Oxide filter etandardiz-ed at 536*9 run. All pertinentdata shall be recorded in lab book.
All spec, tubes arc checked for absorbance uniformity everysix months.
Z2
A. INSTRUMENT OPE-UTTON ANT) CALIBXATlui; Ccont'd)
15) Specific Ion Meter (Radiometer)
Q.C. Laboratory has a ^Radiometer brand specific ionmeter. The meter IE readable and accurate to +/- 1 rav.Q.C. Laboratory has many ion specific probes that are usedin conjunction with the meter (i.e. flouride, chloride,iodide, sliver-sulfide , NT", pH ; and their coorespondingreference electrodes). The probes when in use are leftsoaking in a 10 ppm working standard (the standard thatthe probe is specific for). If there is going; to be alength of time between uses the manufacturer recommendsthe probe to be stored with its own protective cover(supplied with the probe when purchased) in place over thesensing surface of the probe.
Q.A. for the ion nseter and probes is the following:
a. At least a ten fold concentration range of thestandard curve ic run for each group of analysis.The standard curve is run before each set ofsample analysis Is run each day. For the meterand probe to be operating correctly, there mustbe a 57 to 59 raV change per each lOx (10 fold)concentration of the standard. If this conditionis not met, the standard curve is prepared again.The probe meanwhile is left to stir in a beakerof water, to equilibrate further. Finally thestandUxrd curve is rerun. If the results are nobetter or worse than before, the analyst willreport the condition to his or her supervisor.The supervisor will help by replacing or regeneratingthe probe (see procedxire for regenerating probes -if applicable- that are supplied with the probe)
If tumble to correct the problem the supervisorwill inform the Q.A. Supervisor about the situationThe Q.A. Supervisor will expedite a solution tothe problem. A solution might be to assist theabove mentioned personnel to set up an alternateapproved method until the specific ion meter and/or the probe malfunction can be corrected. Note;(See Part III Types of Internal Quality Controlof this manual for more information pertaining toQuality Control for the specific ion meter).
Page 23
A. INSTRUMENT OPERATION ANP CALIBRATION (cont'd)
16) Muffle Furnace
Q.C. has several Muffle furnaces in use. They are allcapable of reaching at least 4OOC. The muffle furnacesare used basically for cleaning glassware (interrae ofdrinking wnter analvsic). The muffle furnaces are usedof course for sample preparations by other departments inQ.C. Laboratory. The accuracy of the ashing provided bythe muffle furnaces ie checked by running controls withsample runs. The results of sample spike recoveriesare monitored for each parameter run. If the resultsare lower than expected, the muffle furnace could bethe cause. An investigation would then be rnade to determineif the muffle furnace is heating too hot. If no otherreason can be determined for low recoveries, the Q.A.Supervisor is notified. He will see to it that a servicecall is made to have the muffle furnace adjusted, orif need be to have it replaced with a new one.
17) Gas Chromatographs (G.C.)
Q.C. Laboratory has four (*0 gas chrorr.atographs. EachG.C. is equipped with a column over, capable of isothermaltemperature control +_ 0.2C to at least 220C. All G.C. Eare capable of temperature programmed operation. TheG.C.s have been outfitted with Various detector systemsdepending on the type of analyses required. Q.C. Laboratoryhas made an attempt to dedicate G.C.s to one or two parti-cular analyses. However, due to sample demands, it some-times becomes necessary to modify G.C. conditions. Whenmodifications are done, careful recalibrations are performedto guarantee against variations in renults. The followingtwo sections will describe; the G.C.s, their detectors systemsand accessories and finally calibration procedures.
a. The four (*0 G.C.s and their detectors andaccessories will be listed below:
1. Varian Assoc. Model 3700 - system I.D.No. 3700-219 . This G.C. is equippedwith an electron capture and a therm-ionic specific detector (nitrogen andphosphorus specific); data aquisitionis accomplished using a Varian 9176 stripchart recorder.
2. Varian Assoc. Model 3700 - system I.D.No. 37OO-13OO. This G.C. is equippedwith four (*O detector systems. Detectorsare used either individually or in somecases simultaneously. The detectors arelisted below.
i. Elect-on capture 63Ni (8mCi).
ft-gc
A. INSTRUMENT OPERATION AND CALIBRATION - G.C. (cont'd)
ii. Flame ioni&ation (F.l.D.)iii. Hall electrolytic conductivit
Data aquisition for this G.C. ip accomplished using aVarian 42?0 integration system and two strip chart recorders(Houston Inst. QmniBcribe and Varian 9176). This G.C. isalso equipped with a Tekmar Assoc. purge and trap systemModel LS-C2 and a ten (10) position auto sampler model(ALS).
3- Varian ARSOC. Model 37 0 - system I.D.No. 37i+C-ll1+12. This G.S. is equipped withan electron capture detector (63Ni-8mCi).Data is acquired using a Varian Model J+2?Dintegration system. This G.C. is alsoequipped with a Varian 80CO - 60 vialposition auto sampler and injector.
*4. Hewlett Packard Inc. Model 330*. ThisG.C. is equipped iwth an electron capturedetector and two flame ionization detectors(F.I.D.). This G.C. is equipped with anH.P. model iSS^OA integration system andan H.P. auto sampler and injector.
Q.A. and calibration procedures for all G.C.s will follow:
b. A record is maintained for each G.C. and it containsthe following information:
1. The date of installation end serial no. ofeach detector installed.
2. Background current profiles obtained at thetime of installation of each detector andsubsequent profiles (column identitynotations are made).
Information for each G.C. column is recorded (i.e. columnident. no., date of packing, liquid phase identity and lotno. of packing material, conditioning temperature, flowrate and no. of hours, length and i.d. (internal diameter)of column, date of silylation of column, and where applicablethe dates of compound conversion monitoring along withpercentages of breakdown).
Carrier gasee for all G.C.e are at least 99-998# pure(aa an added precaution all gases are cleaned by passingthem through a molecular stive). If background problemsare noticed, the molecular seiveB are replaced or re-generated. Two stage regulators are used on gas cylinders.
A. INSTRUMENT OPERATION AND CALIBRATION G.C. (cont'd)
For each dny on which analyses are initiated for pesticides, ,#,..,phenoxy acid herbicides, trihalomethaneB (THH)t volatile />? ^jorganicB (VOC) for example;*! laboratory method blank will */'be prepared and run. This blank is made by analyzinglab. pure water using the same identical procedure that isused to analyze samples,
A minimum of three (3) calibration standards is analyzedeach day to calibrate the system. If the instrumentresponse is linear through the origin one standard perday IB run. The response of that standard is within +__15 percent of previous calibrations or a nev standardcurve is repeated. All chromatagrams are kept on recordfor review.
The following ic o list of additional Q.A. itrims that areadhered to, to calibrate the G.C.s and also to monitor forchanges (drifting).
1. Retention times and/or distances are monitoredand recorded in a log book for THM analysis (timesor distances should not exceed 1O% of the normalvalue during ar. 8 hour period). Any deviationsare reported to the department supervisor.
2. Solvent blanks are made_, for each new lot no, ofsolvents, by concentrating and shooting them tomonitor for irregularities in solvent composition.
3- After shutdown and restart, G.C. columns areprimed by injecting Oul of a priming mixture(Ing/micro liter of each pesticide) using adedicated syringe.
*4. New colunis are silylated to reduce absorption sites.
5- Column inserts with cilylated glass wool are usedand are replaced ofter.
6. Daily a standard containing endrin and p,p'-DIV?is injected to monitor for breakdown of thesecompounds and to act as a column oven check.
For additional information, see Q.C. Laboratory (S.O.P.)Standard Operations Procedural manual for Gas Chromatography,and the specific operations manuals supplied by the instrumentmanufacturers.
Page 26
A. INSTRUMENT OPERATION AND CALIBRATION' (cont'd)
18) G.C./MS (G.C. Mass Spectrophotometer)
a. Q.C. Laboratory has two G.C. Mass SpectropnotometerE(G.C. /MS). Both G.C. /MS meet or exceed EPA .requirements.These requirements are:
i. The G.C. portion is temperature programmable,interfaced with the mass spec, with all-glasstransfer line.
ii . Macs spectral dato are obtained with electron-impact ioni nation at ?OeV. (The spectrum produced ,meets all criteria, that will be listed in thissection for a successful BF3 and/or DFTPP tune) —
iii. Interfaced data system equipped with software toacquire and manipulate data. The data systemscan perform automatic quantitative analysis usingintegrated specific ion abundances with a singleinternal or external standard . The systems canalso provide automatic quantitative analysisusing integrated specific ion abundances andregression analy&is with multiple internal orexternal standards.
b. The two G.C./KT. will be listed below:
1. Pinnigan MAT model 1020 automated quadrupoleG.C. /MS. This instrument is equipped with aPerkin-Elmer sigrna J3 G.C. with capillary andpacked column options. The MS has a range ofU-BOO amu. The instrument has electron ioniz^tion(impact), chemical ionization and solid probecapabilities. The data system is controlled bya 32 Megabyte CMD disk drive. The 1020 is alsoequipped with a Tekraar Aseoc. LS-C2 purge and trapunit. Hard copy of data is provided by an OKI-DATA printer.
Finnigan MAT model 5 -CO automated quadrupoleG.C. /MS. This instrument is equipped with aFinnigan -'G.C. with capillary and packed columnoptions. The MS has a range of 4-800 amu.The mass Bpectrophotometer J,as an electron ionication(impact) detector. The data system is controlledby a 32 Megabyte CMD disk, drive and IB also equippedwith Superlncos and Auto-quan software. The5100 G.C. /MS is also equipped with a Varian ABBOC.model 5000 auto sajnpler-auto injector. Ka_rd copyis provided by a Printronix brand printer.
Page 2?
'%tfA. INSTRUMENT OPERATION AND CALIBRATION G.C./Mii (Cont'd)
c. Each day each G.C./MS must be tuned before any calibrationscan occur. Requirements for the tune will follow:
Method 62*4 the instrument is calibrated with ^^E Bromo-fluorobenzene at least once during each 12 hour shift.Working standards are generated and the linear responseranges for each parameter is verified daily.
Method 625-The instrument is calibrated with 50 mg DFTPPat least once during each 12 hour shift. Working standardsare generated and the linear response ranges for eachparameter is verified daily.
For e tune to be successful with 3FB the following must occur
Mass Ion Abundance Criteria
5O 15 to ItQ* of cvass 9575 3-0 to 6O* of mass 9595 Bass Peak, 100% Bel. Abundance96 5-95 of mass 95
175 " <2*> of mass 17U174 ->50% of mass 95175 5-9# of n^sB 17^176 >95/-' but <101$ of mass177 5-S&>f mass 176
For a tune to be successful with DFTPP the following must occur
Mass Ion Abundance Cri teria
of mass 19868 <~2& of mass 6970 <2^ of mass 69
127 AO-60& of mass 198197 <1# of mass 195198 Base Peak, 10C$ Rel. Abundance199 5-9# of mass 19S275 10-3O^ of mass 198
>\% of mass 198Present but < mass>ltQ/£ of mass 19817-23# of maeE
Page 28
A. INSTRUMENT OPERATION AKP CALIBRATION G.C./KS (cont 'd) i*
Oncc n sat iEfactory tune hnc been achieved, calibration conbegin. (.Jn each analysis day n method blank and o minimum of3 standards ic run. W i t h ench me thod , surrogate compoundsore c piked to mcnnure recovery - The individual surrogatesused, and their acceptable recovery criteria are listed inTable II. A Q.C. check sample is analyzed to monitor recoveriesof contaminant parameters.
The Q.C. check sample is made by dosing water with a Q.C.check sample concentrate. This concentrate contains all ofthe parameters of interest , and is abtained from US EPA.Cinn. Ohio (if available), or is made from the pure reagents.Note: (the source of this Q.C. check sample concentrate isnot the same as that used for the standard calibration curveor any other calibration standards). Recoveries from thisQ.C. check "sample are compared to the acceptance criterialisted in Tables Ha and Jib. If data IE not within accpetablelimits for any parameter, then that parameter must be rechecked.A new Q.C. check sample that contains only that parameter,must then be analyzed. If the parameter still does not pass,then a new calibration for that parameter must be run.
Once a staisfactory tune has been achieved followed by asatisfactory completion of a Q . C . check B ample run, sampleanalyeie can begin.
19) Turbidometer
Instrument: KACH model 21 00 A Turbidometer stock solution: kOOONTU formazin standardizing concentrat ions: 4-0 NTU and b .0 KTU
Dilute 10ml stock forroazin to one CD liter with lab. pure waterand mix well to make a 4-0.- NTU standard. Dilute 10ml of thekQ. NTU standard to 100 ml with Lab', pure water to make a 4.0NTU standard.
To Calibrate me te r :
With range control on ICO, pour 25 ml of the ^0. NTU standardinto a clean glass cell and wipe glass cleaji with a tissue.Insert the cell into the cell holder and cover top with lightshield. Adjus t reading to 40. on meter. Empty the cell, rinseand then pour 25 ml of 4. NTU standard into the cell. Turn therange control to the 10 scale and insert the cell and covertop with l ight shield. . .Ad jue t reading to -4 .0 or. the meter . ABa check, turn range control to 100. The reading should beapproximably ^.0 on this sca'ie as well. If not , check readingon the 10 scale again. When these readings agree, sampleanalysis can begin.
TESTING OF WELLS FOR HYDRAULIC CHARACTERISTICS
Each well will be tested to determine the permeability
and/or transmissivity of the zone that it penetrates. It is
anticipated that the upper portion of the phreatic zone will
have a very low yield, and that bail tests or slug tests wil
be the most appropriate method of testing the shallow wells.
However, the possibility of conducting low rate, short
duration pumping tests on these wells will not be ignored.
The mid-range and deep wells will also be tested using
either slug tests or low rate, short duration pumping tests.
If the yields from these wells are low enough to allow for
accurate falling head and rising head tests by removing and
injecting water. During the falling head portions of the
tests, water removed from a well will be put back into the
same well. If slug tests cannot be used, short duration
(approx. 60 - 100 minutes) low rate pumping tests will be
conducted to avoid causing unnatural warps in groundwater
flow paths.
All of the wells, with the exception of one well in the well
#10 cluster, will be tested in this manner. One of the
wells at #10 will be subjected to a pumping test with a
duration of approximately 4 to 8 hours, if yields permit.
It is anticipated that either the mid-range or deep well
will be tested in this manner. The determination of which
- 16 -
well will be tested will depend not only on its yield, but
the degree of VOC contamination of the zone it penetrates,
since it is the most contaminated zones that are of prime
interest.
During the testing of each well, regardless of method, water
levels in nearby wells will be monitored to obtain
additional data to be used in the determination of hydraulic
characteristics.
- 17 -
COLLECTION OF GROUNDWATER SAMPLES
FOR CHEMICAL ANALYSIS
SAMPLING METHOD
The well #10 cluster will be sampled and analyzed for
trichloroethylene and 1,1,1- trichloroethane immediately
upon completion of drilling and recovery of water levels, so
that data will be available in time to determine which well
in the cluster to conduct the extended duration pumping test
on. Water samples will be collected using a teflon bailer
and immediately transfered into standard airtight VOC vials.
All wells will be sampled at the time of testing, so that
the removal of water for testing purposes will also serve as
part of the purging process. If testing is conducted using
the injection of potable water, groundwater samples will be
collected before any such injection.
The shallow wells will be purged of a minimum of 3 times the
volume of water present in the borehole. Purging will be
done using either a teflon bailer or submersible pump. It
is possible that the recovery rate of the wells will be so
low as to make the removal of 3 times the volume of water in
the borehole impractical. If this is the case, the well
will be purged of 1 borehole volume.
Whichever volume is removed from a well, it will never be
- 18 -
completely emptied, since this can allow the escape of VOC
compounds. Several feet of water will be allowed to remain
at the bottom of the well. Water will be removed from
progressively deeper zones of the shallow wells during
purging, to ensure that all standing water is removed.
After purging, a water sample will be removed from the well
with a teflon bailer and transferred into standard airtight
VOC vials.
The mid-range and deep wells will be purged using a
submersible pump. They will be purged of a minimum of 3
times the volume of water in the borehole, if yields and
recovery rate permits. The pump will be located above the
water bearing zone of the well, to cause water to flow into
the well from the aquifer and up into the pump. The pump
will then be raised up into the casing to remove any
standing water in that portion of the well, if this step is
necessary. It may be possible to cause enough drawdown so
that the water level in the well is just several feet above
the pump. This would eliminate the need for raising the
pump during purging.
After pumping, a sample will be collected from the well
using a teflon bailer and transferred to standard airtight
VOC vials.
All samples will be collected from a depth of approximately
- 19 -
2 feet or more below the water surface in the well, to avoid
collecting near-surface water, which may have lost volatile
compounds. Samples will be collected within 4 hours of
purging. At the time of transfer of water samples from the
bailer to the VOC vial, a field blank of distilled water
will be collected in a VOC vial, and attached to the actual
sample. All sampling will be done by INTEX personnel who
are trained and experienced in sample collection procedures.
SAMPLE PRESERVATION
At the time of collection, each VOC vial will be labeled
with the well number, date and time of collection and
whether it is a groundwater or blank sample. These samples
will be put into an insulated container. Depending on the
weather, these samples may have to be moved to an indoor
location to protect them from freezing.
The samples will be packed in a protective container along
with chain of custody forms listing well number, date and
time of collectors, number and type of container, names of
sample collections, and required analysis. The containers
will be sealed and shipped via overnight courier to Quality
Control, Inc. Laboratories in Southampton, Pa. Quality
Control, Inc. is an independant laboratory certified by the
Pa. DER {#09-131}. All samples will be delivered to the
laboratory within 72 hours after collection.
- 20 -
CHEMICAL ANALYSIS
All water samples will be analyzed using a gas
chromotagraph/mass spectrometer method, with a detection
limit of 1.0 part per billion. The volatile organic
compounds to be analyzed for are as follows:
Chloromethane
Vinyl Chloride
Methylene Chloride
1,1-Dichloroethane
Chloroform
1,1,1-Trichloroethane
Bromodichloromethane
Trans 1,3-Dichloropropane
Dibromochloromethane
Cis 1,3-Dichloropropane
2 Chloroethylvinyl ether
1,1,2,2-Tetrachloroethane
Toluene
Ethvlbenzene
Bromethane
Chloroethane
1.1-Dichloroethylene
Trans 1,2-Dichloroethylene
1.2-Dichloroethane
Carbon Tetrachloride
1,2-Dichloropropane
Trichloroethylene
1,1, 2-Trichloroethane
Benzene
Bromoform
1 , 1 , 2,2-Tetra chloroethylene
Chlorobenzene
A copy of the Quality Control, Inc. r.i
in Appendix A of this work outline.
plan can be found
- 21 -
DECONTAMINATION OF EQUIPMENT
A portion of the Chromatex Plant #2 parking lot will be
designated as a decontamination area, where all equipment
will be transported for decontamination (Figure 1). The
decontamination area is along the southwest wall of Plant
#2. It is paved with asphalt and has water spigots for
attaching hoses. This area is away from the employee
parking lot and is not a thoroughfare for the conducting of
everyday business. The drilling rig will be decontaminated
after the completion of each well and before the drilling of
the next one. This will be done by hosing off the drilling
rods, derrick, bits, drilling table, shovels, deflection and
diversion equipment and any other relevant equipment.
Hosing will be done using potable water. The equipment will
then be steam cleaned and hosed off again.
The submersible pump to be used for testing and purging will
be hosed off, inside and out, with potable water. It will
then be wiped off with isopropyl alcohol, rinsed with
distilled water, wiped with paper towels, and allowed to air
dry for at least one hour before insertion into another
well. Equipment associated with the pump, such as hose,
chain and cable, will be hosed off with potable water, wiped
down with isopropyl alcohol, rinsed with distilled water and
allowed to air dry for at least one hour before insertion
22 -
into another well.
Teflon bailers used for purging will be rinsed with potable
water, wiped down with isopropyl alcohol, rinsed with
distilled water, and allowed to air dry for at least one
hour before insertion into another well. Teflon bailers,
and associated teflon bailing cord, used for collecting
water samples will be rinsed with potable water, wiped down
with isopropyl alcohol, then rinsed with potable water
followed by distilled water. They will be allowed to air
dry for at least one hour before inserting in to another
well. All non-teflon cord and rope used on bailers will
either be saved in a plastic bag for reuse in the same well
or discarded. Water level probes will be rinsed with
potable water followed by distilled water, and allowed to
air dry for one hour.
In addition to the above mentioned procedures, all equipment
will be initially rinsed with potable water before leaving
the well site.
23 -
CONTAINERIZATION OF WELL MATERIAL
The immediate area surrounding the well will be covered with
a plastic tarp, with a hole cut in the middle to accomodate
the drilling string. Cuttings exiting the well will be
directed onto the plastic sheet with a deflection shield.
The cuttings will then be shovelled into 55 gallon drums.
These drums will be of the type 17 H, steel, with 12 mil
plastic liners and lids. If yields from the well are such
that water runs out of the cuttings and off of the plastic,
the material exiting the well will be channelled into a
portable catch basin surrounding the well. It will then be
tranferred into the drums. Some amount of spillage of water
onto the ground is expected. However, it is expected to be
small and to be no more than would occur with any other
alternative method.
Each drum will be labled with the well number and depth
interval from which the cuttings and water in it were
removed.
Water removed from the wells during testing and purging will
be placed in the same type of 55 gallon drums. The drum
will be labelled with the well number. If large volumes of
- 24 -
water must be removed from a well, so that placing it in 55
gallon drums is not practical, it will be put into larger
tank trucks or similar containers. All containers will be
stored at Chromatex Plant #2 until their contents can be
properly disposed of.
25 -
TIME SCHEDULE
An estimated time schedule, assuming fairly rapid progress,
is listed below.
ANTICIPATED COMPLETION TIME
AFTER RECEIVING NOTIFICATION FROM EPA
TASK TO PROCEED (WEEKS)
Mobilization and logistics 2
Drill wells 1 ABC and 10 ABC 6
Drill wells 2, 4, 5 and 11 8
Test and sample all we11s
except 1 well in #10 cluster 10
Extended pumping test on
one well in #10 cluster 10.6
Laboratory Analysis
and QA/QC 12.6
Finished Report 15.6
TOTAL 15.6 (3.90 months)
- 26 -
It is estimated that 3.40 months is the minimum time
required for completion of the project. However, since most
of the fieldwork will take place in January and February,
some delays are expected due to the severe winter weather
that often occurs in the Hazleton area, which can affect
site accessibility, equipment operation, efficiency of
personnel and especially decontamination of equipment.
Delays may also be caused by the necessity to drill and set
casings deeper than anticipated, and to bring in larger
pumping equipment and additional containers if very high
yields are encountered. Equipment failure due to vandalism
is also a possibility.
The timetable estimated by EPA/TAT for an investigation
involving 11 wells at Chromatex was 3 to 6 months.
- 27 -
SAFTEY PRECAUTIONS
All drilling sites will be continuously monitored using a
photoionization vapor detector (h-nu). Respirators with
organic vapor cartridges and safety goggles will be kept on
site for use by all personnel, if appropriate levels are
indicated by the h-nu. Hazardous levels of VOC are not
expected in the groundwater. To date, the highest
concentration of VOC in the groundwater have been found in
the Chromatex well, where TCE was found in a concentration
of 3.3 ppra on October 30, 1987. On November 23, 1987,
levels of TCE in the Chromatex well were measured at 1.5
ppm.
In addition to the safety precautions outlined above, all
INTEX personnel and drilling personnel on-site will follow
the Health and Safety Plan outlined in Appendix B. This
plan will be finalized before drilling commences, and a copy
will be provided to the drilling crew and Chromatex
management. A copy of the plan will be kept on-site at all
times by the site geologist. The site geologist will be the
designated safety coordinator, and will be identified to all
site workers as such.
- 28
APPENDIX A
Quality Control, Inc., QA/QC Plan
INTRODUCTION
Quality Assurance Manual for Quality Control Laboratory12£5 Industrial Highway £outhampton / Pennsylvania 16966
President: Alan Schopbach
Vice President: Thomas Mines
This document contains a list of quality control proceduresthat have been instituted in the laboratory. The object of this planis to provide a listing of quality control measures for thelaboratory to utilize and also to provide a means to ensure that thequality control procedures outlined are followed. The Plan willensure that every check that can be made, will be made, so that dataproduced by Q.C. Laboratory will be precise, accurate andreproducable. The manual is d i v i d e d into two parts. Part I outlinesquality control measures for Chemical Analysis and Part II outlinesquality control measures for Microbiological Analysis.
TABLE OF CONTENTS PAGE No.
PART I SAMPLING ANT) SAM! LE HANDLING 1-9
A. SAMPLING (GENERAL) ' 1B. SAMPLING INSTRUCTIONS 6 + 7C. CHAIN OF CUSTODY 7-9
PART II INSTRUMENT OPERATION ANT) CALIBRATION 9 - 3 7ANT) ANALYTICAL PROCEDURES
A. INSTRUMENT OPERATION AND CALIBRATION 9 - 2 8 and 35~3B. ANALYTICAL PROCEDURES >5
PART III DATA REDUCTION, PREVENTIVE MAINTENANCE, 3>S andTYPES OF INTERNAL QUALITY CONTROL ANDPRECISION AND ACCURACY MONITORING
A. DATA REDUCTION VALIDATING AND REPORTING 33 and3. PREVENTIVE MAINTENANCE ^ - ^C. TYPES OF INTERNAL QUALITY CONTROL ^ - 51D. PRECISION AKD ACCURACY MONITORING ' 5 2 - 5 ^
PART IV CORRECTIVE ACTION 55
A. CONTINGENCY PLANS 55
PART V APPENDIX 56 - 63
A. Q.C. SAMPLE REPORT 56B. Q.C. SAMPLE TAG 57C. DIRECTIONS FOR TAKING A WATER SAMPLE 58-61D. CHAIN OF CUSTODY RECORD 62E. Q.C. SAMPLER INSTRUCTIONS 63
INDEX OF TABLES . PAGE No.
TABLE I - SAMPLING AND PRESERVATION TECHNIQUES FURINORGANICS ANT) ORGANICS 2-5
TABLE II - ACCURACY STATEMENT FOR G.C./MS SURROGATES 29
TABLE I la - PRECISION A NT) ACCURACY LIMITS VOLATILES >0 + 31
TABLE lib - PRECISION AND ACCURACY LIMITS BASE NEUTRALSAND ACID EXTRACTABLES 32 - 3^
TABLE III - ANALYTICAL METHODOLOGY; METALS, ORGANICS,INORGANICS 39 - *tl
All sampling is conducted in accordance with the proceduresoutlined in the EPA "Manual for the Certification ofLaboratories Analyzing Drinking Water", (EPA5701982002),Oct. 198a.
When a Q.C. Laboratory field representative collects a sample,he or she completes a Q.C. sample report (see Appendix A).This report includes the following:
1. The date of collection.2. The time of collection.3- The source (including name, location, and sample type.)U. The preservative used if applicable.5- The analysis required.6. The name or initials of the collector?• Any pertinent field data (pH, D.O., residual Cl, etc.)
A waterproof tag, comrletc with the required information, issecurely attached to the sample bottle (See Appendix B for acopy of a Q.C. sample tag). Microbiological and chemicalsamples are iced during transit and refrigerated at 1-5 Cduring storage in the laboratory.
All QC field representatives are thoroughly trained in correctsampling procedures. No field representatives are authorized tocollect samples until he or she has received training from themanager of field services. /ill sampling procedures used, willbe those from U.S. EPA recommended methods. The specific samplingprocedure will be dictated by the specific analysis to be performed.The type of sample container, the required preservation for eachorganic and inorganic parameter, and maximum holding times arelisted in Table I. See also, Appendix E. for Q.C. Sampler Instructions
Sample bottles will be provided by Q.C. Laboratory. The bottlesused are new (not recycled) to avoid contamination problems.Bottles that contain no preservatives should be rinsed with samplewater once and then filled. Bottles that contain preservativesare not pre-rinsed. The acid that is used as a preservative istrace metal grade. All other reagents that are used as preservativesare either trace quality or ACS quality. As a control an emptysample bottles will be sent back to the Laboratory with each batchof samples. When this bottle is received by the Laboratory itis filled with Lab. pure wnter and run as a bottle control.
r " r
TANDARDS; MJ-ItiQD 6?S £ RkEOVliHY LIMITS 1
- i ( \ r r \ \ r [
SUhKOGATK STANDARDS; METHOD 62^ V R££OV£HY LIMITS
h a5e/'Neu t_r_a 1 Fra_c_t i on)
Aniline - d5
Nitrobenzene - d5
Pyridine - d5
D - 165.8
D - 168 Ji
D - 103.3
(Volatiles)
[iromofluorobenzene
Pentafluorobenzene
I, Jt Di f luorobenzeneKlourobenzene
73-5 - 12*1.366.2 - 12*1.372.8 - 118.73-7 - 116.
(«cid ExtractuLle Fre-ction)
2 - Fluorophenol
Pentafluorophenol
Phenol - d5
D - 180.0
D - 15'u7D -
* «& w i t h other recoveries, a 9!$ compU-teit£ss is exupec ted .
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DI-N-EUTYL PHTHALATE
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1,3 DICHLORO BENZENEl.If DICHLORO BENZENE
3,3* DICHLORO BEHZIDINEDIELDRJN .
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EHDG3ULFAN SULFATE
ENDRIH ALDEHYDE
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EPA 625
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1-EASUREKE1I7 PARAMETER JU'ITERENCE1 PRKCJiilON ItKL. Vi ACCU1UCVJF.E OF ALLC'.VAI-I.E VALUES
a. Q.C. Laboratory has three (5) Atomic .Aboorption (A.A.)units. Two hove graphite furnace and flame measurement,capabilities. One unit ie equipped with graphite furnaceonly. All m.C. Lab. A.A.s meet or exceed EPA requirements(i.e. each is single-channel, single or double beam with agrating monochromator with photomultiplier detector, ad-justable slits, and a wavelength range of at least 190 to800nm).
Single and multielement hollow cathode lamps as well asEDL (electrodeless)discharge lamps. Graphite furnacesare capable of reaching the method specific temperatures.Burner heads for flame analysis are approved typec; toinclude air/acetylene and nitrous oxide when required.All instruments are equipped with Deuterium backgroundcorrectors. Commerical grade actelylene is used. Acetenewhich acetylene is packaged with is eliminated with in linecarbon filters. Air for the acetylene/air flame is suppliedfrom cylinders. Nitrous oxide and Argon are of commericalquality.
b. The following is a list of the A.A.s and their accessories:
1. Varian AEGOC. Spectra *K) A.A. with HgA-95 graphitefurnancc, eight (8) position lamp turret, auto-pipet system,and a D-15 Data system. The D-15Data system is a microproccessor controlled systemthat allows the analyst to set up, through thekey board, unattended sample runs. The A.A. hasthe capability to run a raulti element unattendedprogram. Data is provided via on Etsen FX-80D.H. Printer.
2. Varian Assoc. Model 975 A.A. with HgA-95 graphitefurnace, eight (8) position larap turret, auto-pipet system, flame and direct aspiration capabilitiesusing either air/acetylene or Nitrous oxide, coldvapor mercury and arsine generation capabilities.Tnis instrument is capable of unattended operationin the furnace mode and semi-unattended in theflame mode (Varian direct aspiration auto sampler).Data is provided by an Epsen FX-80 D.M. printer.
A. INSTRUMENT OPERATION AKD CALIBRATION A.A. (contfd)
3- Perkin Elmer model 60J with both furnace and flamecapabilities (air/acetylene and Nitrous oxide). Thisinstrument also has mercury cold -vapor generation capabilities.
All EPA A.A. accessory requirements are met by Q.C. Laboratory.They are the foliowingI
i. Pipet tips for manual pipeting exe free frotr. CdSand range in size from 5 to 100 micro liters.
ii. For cold vapor mercury analysis the absorbtion cellis 1O cm quartz, with end windows. The air pump•used is peristaltic and can be regulated at 1 Literper minute (a flow meter XE included). A watertrap is supplied, in line, and the cell is heatedwith a SCO watt light source to prevent water con-densation.
Calibration for all atomic absorption is done daily. A blank anda minimum of four (A) standards is run with every run. EPA and ERAAssoc. known standards are run with each run. If data is notwithin the required limits given by EPA and/or ERA Assoc. thestandard curve is remade and rerun. * No sample analysis will beginunless this condition is first net. Every precaution to avoidinterferences is taken by Q.C. Laboratory. When interferencesare suspected, samples are run by the method of standard addition.
For details in operation of A.A.s and more on calibration see theoperations manuals supplied by the instrument manufacturers andalso EPA and/or ERA approved methodologies. Also see Q.C. LaboratoryS.O.P. for atomic absorption operation.
21. Lab. pure water
Q.C. Laboratory uses a Marcor Inc. custom designed water purificationsystem to produce its laboratory pure water. The system incorporatesa deionizing unit with a reverse osraosis accessory. The unit isdesigned, through the use of an indicator light, to alert personnelwhen the deionizer cartridges are expired. Two cartridges arekept in series so that at no time will the water being supplied beaffected. The system is checked daily and recorded in a bound book.The water quality meets or exceeds EPA requirements (0.5 megohmsresistivity, 2.0 micromhos conductivity). Regent water blanksare run with every analysis as a Q.A. check on the lab. pure water.A separate in line carbon filtration unit is available to provideultra-high purity organic free water where required.
37
A. INSTRUMENT OPERATION AiCD CALIBRATION Lnb. Water (cont 'd)
22) Reagents, chemicals, standards
II ie Q.C. Lnborntory's policy to purchase only the best qualityreagentc and chemicals thfit arc nvnilnblc. Ajuilysts are instructedto follow methodologies in detail. Analysts will use the gradeof reagents that arc required for e given analysis. The reagentgrade will bo mot or exceeded: as fin example if a procedurerequired the use of ultra-high purity NaCl then the analystwill use ultra-high purity NaCl. The following Q.A. is alsofollowed:
i. Stock and work inc. standard solutions are checkedregular ily for signe of decomposition includingbut not limited to discoloration, formation ofprecipitates, and concentration changes due toevaporation.
ii. All solutions are properly labeled with ident. ofthe compound, concentra t ion, solvent, dste, andthe analysts initials.
iii. All A. A. standards are of ultra-high purity.iv. All chemicals, solutions and standards are dated
when received by the laboratory.v. Special purity standards for organic analysis are
purchased. Any reagent that is heat or lightsensitive and e u V j e c t , t o refrigeration is stored in B.refrigerator et 1-^°C( in explosion proof refrigerator
/ if requ i red) or(frozer: iif- required) .
23) Model 915* Bsctanan TOC (Total Organic Carbon) analyzer
Make up standards fresh daily. 1QDO ppm TOC stock solution^Dissolve 2.125^ B dried Potassium biphthalate in C0£ free waterand dilute to 1060 ml. Voluuietrically prepare 5.0, 10.0,20., 50.and 100. ppm standards.
Turn on CO2 free airflow and adjust pressure to 3-5 psi (flow meterreads 150 cc/rain). Preheat analyzer to 950C using "High" switch.Then switch to "Lo" position. Turn Analyzer trwitch to "Stand by'.1Allow one hour for instrument wannup. See operations manual formore details for the operation of the analyzer.
To calibratc> use a manual syringe. Inject 20 microliter of ablank. When the base line is established inject the standardsfrom low to high concentration. Run replicates until 2 peak heightvalues are the same. Inject a known quality assurance standard toverify the calibration.
36
B- AKALITJCAL
Q.C. Laboratory uses only EPA and/or EPA approved methodologies.Strict adherence to all detailo in each method will be guaranteed.Due to constant Bdvy^cec in tehcnologics and new EPA approvals formethodologies Q.C. Laboratory reserves the right to utilise themost appropriate approved method. All changes in methodology willbe done only at the discrestion of the Q.A. Supervisor (approvalmust come from the President or Vice President of Q.C.).
I>ue to the complexity involved in describing each method or procedureit will not be done here but rather each method will be given byreference. A listing of these methods can be found in Table IIIand Ilia. Hlease refer to the cited references and Q.C. Laboratoryprocedural manuals for details.
PAJ3T III DATA REDUCTION, PREVENTIVE MAINTENANCE, TYPES OF INTERNAL QUALITY CONTROLAND PRECISION AND ACCURACY MONITORING
A. • DATA REDUCTION.VALIDATING ATO REPORTING
1. Raw Data Acquisition
Routine computations to derive the value for a parameterin the units designated by sample instructions will be per-formed by the analyst assigned the sample. Analysts willput all raw data into permanently bound notebooks. All
\ work is to be done in indelible ink. Work is to be neat andorganized. The minimum information requirements to bewritten for a typical analysis is the following:
i. At the top of a page the analyst will recordthe data of analysis.
ii. The name of the analysis is to be recorded*; anexample would.be "Nitrate - Cadmium Reduction".
iii. The raw data will then be recorded.iv. Calculations will then be recorded; if there
are multiple calculations foragiven analysisat least one complete calculation must berecorded. Abbreviated calculations for theother samples are then recorded.
v. Any comments or notes are then recorded.vi. Each analyst keeps his or her own notebook
and therefore he or she need not recordinitials on each page (note: the analyst mustrecord hie or her own name on the front coverof the notebook along with the datethat the book was started).
CONTAMINANT
I f f f f f f I fTABLE III Afiy'TICAL METHODOLOGY; METALS, ORCiAMICii, iNORUAruCS
ME1HOJX3LOGY EPA1
hfege -sy
STD
BABIUH
BOFDN
COBALTFLOURIDE
MAGNESIUM
MOLYBDENUM
TIN
TITA.UUH
ANTIMONY
ARSENIC
BERYLLIUM
CADHUM
CYANIDE (TOT)
COPPER
LEAD
MERCURY
NICKEL
PHENOL (TOT)
SELENIUM
TOALlIUH
ZINC
Atomic absorption; furnanceColorimetric, CurcuminAtomic absorption; furnaceion selectiveAtomic absorption; direct aspiration
289.1l"Methods of Chemical Analysis of Water and Wastes," EPA Environmental Monitoring and SupportCimu, Ohio. i*5268(EPA-600A-79«020)l March 1979-2"Standard Methods for the examination of Water and Woatewate r , " l*»th Edition, American PublicAssociation. 1975«
Atomic absorption; direct aspirationAtomic absorption; direct aspiration
TitrimetricTitrimetric-argentometrie
Spectrophotometrie
218.2
2?2.2
273-1215.1
160.1
353.1202.2
150.1180.1
330-5120.1
110.2
236.1
258.1320.1
1*03208B
505
309B
1 "Metiiods of Chemical Analysis of Water and Wastes," EPA Environmental Monitoring and Support Laboratory,~*nnM Ohio. ^268 (EPA-600A-79-020), March 197).
2 .dard Methods for the examination of Water and V/a .-water," l^th Edition, American Public Health
1 "Methods of Chemical Analysis of Water and Wastes," EPA Environmental Monitoring And Support Laboratory,Cinn., Ohio. ^5263 (EPA-600A-79-020), March 1979-
2 "Standard Methods for the examination of Water and Wastewater," 14th Edition, American Public Health ^^V
A. DATA REDUCTION, VALIDATION AND KEPORTING (cont'd)
vii. Any empty spaces between sample additions inthe notebook are to be voided with long penslaehs.
Any mistakes in the notebook are to be negated by simplycrossing; them out with one pen line, (erasures are notpermitted). Notebooks are to be kept available for reviewby Supervisors and the Q.A. Supervisor.
Calculations for Trace Metals Analyses, and InorganicAnalyses: Calibration curves are prepared to read directlyin mg/1 or ug/1 so it is only necessary to correct forany dilution factor. Solid samples concentrations arereported in mg/kg based on dry or rvct weight of the solid.
Dry solid: metal, rag/kg =
gift (from calibration) x sample volume, ml -x- ____1_____1OOO ml1 x dry weight, g
x 1OOO p
Wet solid: metal, mg/kg =
rug (from calibration)/, s oriole volume, ml x 11 x weight, g x % solids 1000 ml
x 1COO
The method of standard additions is sometimes used. Q.C.Laboratory instrumentation is computer controlled to cal-culate standard additions via linear regression. A manualdetermination is done using the following scheme:
Matrix (i.e. above 1$ solids or viscosity differences) canbe corrected by standard additions:
A. DATA REDUCTION, VALIDATING Aim REPORTING ( con t ' d )
Calculations; for all G.C. and G.C./M.S. procedures aredone in a similar manner. Units are almost always asmeg/liter (PPB). Classical G.C. methods results mustbe calculated by the analyct and recorded in the samplelog in-books. G.C./M.S. results are calculated-by theG.C./M.S. built-in computer. Results are reviewed by theG.C./M.S. operator and then entered in the sample log inbooks.
G.C. and G.C./K3 calculations are the following:
1. Both peak height and area may be used inCalculations,.
2- Internal Standard calculations are usedwherever possible. With this method anothercompound with n retention time close to butnot equal to the parameter in question is addedto standards and samples. This method correctsfor variation in injection size and technique.
Calculation:
Sample (Area or PK. ht) Cone. =£onc.Internal Standard of standard of Sample
Sample (Area or Pk. h t . )Internal Standard
3- External Standard Calculation:
This method is used when internal standard cal-culations are not practical, i.e. in environmentalsamples where an internal standard might interferewith a parameter in the sample.
Calculation:
Samnle (Area or PK. h t . ) Cone, of Stand. = fConc.Standard (Area or Pk. ht.^S Ol SajnPle
All G.C. Chroma tograms will have the following informationrecorded on them.
i. The date and initials of the analyst.ii. The namn of the analysis -(ex. V .O.C. Scan)
iii. Individual parameter identification for all peaks,iv. Standard concentration for comparison.
v. Name of column packing and column ident.vi. Ident of G.C. uned.
vii. Calculations and final answer.
Page 46
A. DATA REDUCTION, VALIDATING AND REPORTING (cont'd)
2) Validation
Raw data is transcribed into bound work bookc by the analysts.Analysts initial these ndditionc indicating that they havedouble checked to prevent transcription errors. Supervisorsare responsible for taking data from bound books and recordingthem on lob. work r-heets. When the lab supervisor in sat-isfied with the accuracy of completed work sheets he initialsthen and sends them to the Vice President lor review.
The Q.A. Supervisor periodically reviews data from all depart-ments. The C^.A. Super, communicates with Supervisors and theVice President any discrepancies that might be found.
After review by management and final approval sample worksheets are sent to Q.C. Laboratory's computer department.Sarnplec results ore then inputted into the computer. Finishedcomputer reports are cent back to the Vice President for finalreview before they are issued to customers and/or Governmentagencies.
3) Reporting (EPA/DEP/DER/o there) '
It is Q.C. Laboratory's policy to expedite all data reporting.Reporting of all EPA/DEP/DER results is to be done usingthe proper applicable forms. The original or true duplicateof results of a test or analysis IE sent promptly to the personrequesting the analysis. The report is signed by the Presidentor the Vice President. If a particular analysis must becontracted to be run by an outside laboratory for one reasonor another; the result is to be reported to the person re-questing the analysis, on the report form of the outside contractlaboratory
Q.C. Laboratory routinely keepn all data (notebooks, boundbooks, copies of reports and forms etc.) for a period thatexceeds five (5) years.
B. PREVENTIVE MAINTENANCE
Detailed coverage of preventive maintenance schedules and proceedurescan be found in y.C. Laboratory S.O.P. and instrument operationsmanuals.
Major instruments and items of equipment are serviced under contractwith the equipment supplier or s qualified agent.
Page
B. PREVENTIVE MAINTENANCE (cont'd)
In addition, critical spore parts arc inventoried. Back-up lampsore maintained for each metal analyzed by atomic absorption to-gether with cpare graphite contact rings and gas cylinders. Ingeneral, tho policy for stocking spares is to recognize the servicevolume, critical nature of the analysis, and the general availabilityof the item. i clow is a listing o_~ G.C./M.S. Maintenance:
1. Daily MaintenanceChange injector septum of G.C.
2. Monthly MaintenanceCheck air filter in card cage. Replace if necessary
3- Quarterly MaintenanceChange oil in vacuum and turbomolecular pumps.
**. Semiannual MaintenanceChange air filter in disc drive.
5- Irregular MaintenanceClean MS source and guardrupoles.Clean jet seperator.Cleoji heads on tape drive.
6. Spare partc in stock/0.1 filters and oilc mentioned above.Complete ion source.Electron Multiplier.Glass jet sepcrator.Various fuses.Extra Filment accemblieE.
A bound book is kept for recordc of all maintenance and repairsthat is done. Each instrument has its own maintenance record book.
C. TYPES OF INTERNAL QUALITY CONTROL
Precision and accuracy of analytical methods wiU be established forall parameters. Precision and accuracy will be monitored throughthe use of routine duplicates* sample spikes and Q.C. check standardsSee Section D. Part III of this manual for details concerningdevelopment of precision and accuracy data and charts. Specificrequirements for quality control measures will be dealt with in thefollowing subsections 1, 2, 3 and k.
Page
C. TYPES OF INTERNAL QUALITY CONTROL (cont'd)
1) Inorganics
This section dcalrr. with internal quality control measuresthat aro utilized for all inorganic and some organic(colorimotric) methods. A standard curve composed of aminimum of five (5) standards covering the concentration rangeof the samples is prepared (at least one of the standards shouldbe at or below the K.C.L.) A reagent blank is prepared daily.For each day on which analyses are performed, the standardcurve needc to verified by use of nt least n laboratory methodblank and ono c; tandnrd within t.hr range of the- ntandrvrd curve.Daily checks chould be within •*•/- 10 percent of original curve.If more thar. 10 sar.ples per day are analysed; the daily standardneed be repeated at a frequency of one standard for each ad-ditional. 10 eamplcc- Each check should be within +/- 10 percentof original curve. Original curves are reproduced at a minimumof once every Quarter. Duplicate samples are run at a frequencyof 10 percent of all samples analyzed. Ten percent of allsamples arc epiked with reagent prade quantities of the para-meter of interest. .Known standards (US EPA Control Samples)are run at least' on a quarterly basis.Values-must be. \rLthia' EPA limitsAll of these data arc recorded in bound books and graphed onchart paper. Limits are +/- 2 standard deviations from themean value. All original standard curves are reproduced at aminimum of once every quarter.
2) Atomic absorption furnace and direct aspiration procedures (Ketals).
A standard curve consisting of a reagent blank and at least ^etandardr, arc run with every analytical run. AE a Q.C. check,an E.P.A. known Control Std. is included in every run. Reagentblanks are included in sample' run at beginning, middle andend of run to monitor for auto sampler cup contamination. lO/ 'of samples arc analyzed in duplicate. 10% of samples are spikedwith reagent grade quantities of the metal of interest. Metalsare spiked at the K.C.L. for each metal, or at the concentrationlevel normally found (when no K.C.L. Value is available'). Datais recorded in a permanently bound book and graphed on controlcharts. Limits are •+•/- 2 standard deviations from the mean value.
Each day in which pesticides analyses are initiated, a laboratorymethod blank is analyzed using the same .procedure used to analyzethe samples. A minimum of three calibration standards is analyzedeach day 'to calibrate the system and check for linearity. Oncethis has beon determined at least one standard is run per day.
Page
C. TYPES OF INTERNAL QUALITY COKTP.OL (cont'd)
The response of thic standard must be within -*/- 15 percentof the previous calibrntion. At least once a quarter an EPAControl Standard is run. Data must not exceed acceptancecriteria supplied by EPA. 10i*> of all samples are done induplicate. '10> of all sampler, are spiked with known quantitiesof each pesticide. Datn is recorded in n bound book and nlsoplotted on Control Chartc. Limits are +/- 2 standard deviationsfrom the mean value.
Q.A. for THK and V.O.C. analysis in the following:
i. A 2 ppb quality check standard is extractednnd analyz.cc each day hofore any Bamples areanalyzed. Instrument status checks and lower
v, limit detection estimations at 5 times the noiselevel are mace from this data.
ii. Each d«y a sample blank is run using dictilledwater. Solvents containing any extraneouspeaks are to bo avoided. Blanks showing anycontamination should be rechecked. Blanksshould have less than 0.4 ppb of individual THM's.
iii. Daily a Q.C. check sample is caadc by dosinglab. water with a check sample concentrate.This concentrate contains all of the parametersof interest and is obtained from USE?A or ism?.de frora the pure reagents. Note: (the sourceof this Q.C. check sample concentrate is not thesame as that used for the standard curve). Re-coveries frorr this Q.C. check cample are com-pared with O.C. lob. established control limitsand/or acceptable recoveries listed in Table Ila.Data for Q.C. check sample must be within acceptablelimits for all sample data on that day to bevalid. Q.C. check samples should be run at a1O# frequency. More precisely, the 10th samplerun on a particular day should be n Q.C. checksample. If lesc than 10 samples are run in aday at least onp Q.C. check sample will be run.
iv. Every tenth G ample is to be analyzed in duplicate.v. Data for recoveries of spikes and ranges for dup-
licates are to be logged into a Precision/Accuracybook. Graphs or photocopies of the spike andeach of the sample duplicates should be fastenedinto this book. A copy of the blk. and std. maybe included. A record of' retention times willbe written on these graphs. This can be in "mm"measured from the injection point. Any changesin flow rate will affcnt thic dato and any physicaladjustments to the flow rate should be recordedon these charts.
Page 50
C. TYPES OF INTERNAL QUALITY CONTROL ( c o n t ' d )
vi. Dntn from all of these mcasurementB is plottedon control charts, (i.e. accuracy control chartsfor recoveries, and precision control chartsfor ranges of duplicates)."
vii. Quarterly EPA-EKSL known control samples shouldbe run. Kesults will not vary by more than theconfidence interval given for each parameter.Results will be tabulated in the Precision/Accuracybook.
viii. Working standards arc generated and the linearresponse range for each parameter IE verified withevery day's run. At least once a month this datais recorded in the Precision/Accuracy data book,
ix. Field blanks axe analyzed along with samples.• x. Samples are collected in duplicate.
*0 G.C./KS Methods 62k and 625
Quality Control checkc and frequencies of checks are the samefor Method 62^ and 625 with few exceptions. Quality Controlchecks and any differences between 62^ and 62p will follow:As listed in Calibration procedures of this manual a satisfactorytune must be accomplished with BF3 for 62*i and DFTPP for 625before sample analyses can begin.
An internal standard method is utilized for both 62^ and 625-All samples, standards and blanks and spikes are dosed at timeof injection with internal standards to aid in quantitation.The following is a list of internal standards used:
Once a satisfactory tune hac been achieved, sample analyses canbegin. On each day of analysis a method blank and a minimumof 3- standards is run. With each method, surrogate compoundsore spiked to measure recovery. The individual surrogates used,and their acceptable recovery criteria arc listed in Table II.A Q.C. check sample is analyzed to monitor recoveries of con-taminant parameters. The Q.C. check sample is made by dosingwater with a Q.C. check sample concentrate.
Page 51
C. TYPES OF INTERNAL QUALITY CONTROL (cont'd)
This concentrate contains all of the parameters of interest,and ie obtained from US EPA. Cinn . Ohio (if available), or IEmade from the pure reagents. Note: (the source of thiB Q.C.check B air. pic concentrate is not the same as that used for thestandard calibration curve or any other calibration standards).Recoveries from thic Q.C. check sample are compared to theacceptance criteria lir>ted in Table Ilaandllb- If data is notwithin acceptable limits for any parameter, then that parametermuDt be rechccked. A new Q.C. check sample that containsonly that parameter, must then be analysed. If the parameterstill docs not pasc, then a new calibration for that parametermust be run.
The laboratory will, on nn ongoing basic, spike and analyzeone sample in every twenty analyzed, or at a mimunim analyzeone per month. One Quality Control check sample will be analyzedfor every twenty samples analyzed. Percent recoveries andstandard deviations will be calculated and limits for acceptableranges arc developed and updated after every 5 samples spiked.Limits are developed equal to •+/- 2 standard deviations fromthe mean value. At no time will these limits exceed the valueslisted in Tables Ha and lib.
For All Procedures:
All control charts arc inspected bi-weekly by the QualityAssurance Officer. The Q.C. Officer has the authority toreject any data that does not meet the control limitsestablished for a given method.
Pa Ec 52
D. PHEC1SION AM) ACCURACY MOKITORlKG
Control limits established for ench analytical procedure vill be used ir.the form of control charts. Limits are based on tvo times the standard devistio:.fro 3 the mean of results on spike and duplicate samples. Data used to establishthe control limits vill be attached to the chart. Specific procedures andtechniques for assessing accuracy and precision of data are as follows:
Precision and encurncv vill be established for all analytical methods.Koutine monitoring of precision and accuracy vill be accomplished throughthe use of control, spikes, duplicates and standards. Data from thesevill be tabulated, and from this dntn control limits vill be calculated,ihe folloving sections vill outline the procedures for: calculating controllimits and preparing control taharts, and routine use of control chartsfor monitoring precision and accuracy.
Precision is a measure of repeatability of a given method. Precision villbe measured as the absolute ran.ge of tvo sanple results. Tne calculationis:
Precision = K = 1st result - 2nd result
Precision Control Charts: At least 20 sets of duplicate results are neededto calculate limits lor the control chart." The control chart is based or.a normal distribution of precision values. Tne chart vill ctart frorr. a"0" Zero deviation base line and vill contcin o varning limit and a controllimit. Tne varning limit is established one standard deviation from themean precision, tlhc- control limit ic tvo standard deviation froffj the mean.
Tne mean precision and standard deviation are calculated as follows:
^_^ Mean Precision - 7. =r £- Xi/n1=1
Where Xi is the range of a duplicate sanple and n is the number of Xi.
Standard Deviation =\ >" Xt — (l
n - ior simplified :
Std. Dcv. =n -i
Example: The following is a set of experimental data that illustratesthese calculations and the construction of e precision control Chart
let 2ndResull Result0.10 .O.1C 0.00.25- O .HC O.CS Mean =o.i? o.io o.or - .0?c.ic- o . i? o.o: stc. DCV. = .0?
53
D. PRECISION AND ACCURACY MONITORING ( c o n t ' d )
The Precision Control Chart (moan = -0?, Std. L»ev. = .02)
.10
.08
.06
.021
0
Control LimitWarning Limit
Zero3 V Time order of results
Once tbe charts are prepared, daily duplicate results are plotted as afunction of time (the date) on the X axic. Results should not exceed thewarning limit and cannot equal or exceed the control limit. The mean, warninglimit, and control limits will be recalculated, everytime the control chart ischanged, but using no less than ?0 resultc.
Accuracy ic a measure of how well an experimental recult compares withthe true value. We will measure accuracy in terms of the % recovery of knowna-nounts of pure reagents that are spiked into real samples or laboratory-water.
Calculate %'> Recovery CLE followc:
5t Recovery = CT-CS
Where CT = the total of sample u'ith cpike addedCSfl= avg. concentration measured in sample before spikeandCSP = concentration of spike added
Accuracy Control Charts: Calculations for preparation of Accuracy Contro3Charts are the eamc as those for precision control Chcrtsexcept that the dis-persion of percent recovery nj ound the mean percent recovery is not calculatedas the absolute value; both positive and negative variations are recorded.Therefore, -there will be an upper and lower warnine limit and an upper and lowe-control limit.
Hxampl e : ' RPSU] tr302? Hean = k^/k
= 103- B ?'
Pape
PRECISION ATTO ACCURACY MONITORING ( con t ' d )
Accuracy Control Churl (Moon
115
100
103-8SJ, eld. Ucv. =r 5-5'':)
____________ U Control Limit
I' Warning Lira4.
Kcar,
1- Warning Ljini 1
L Control Licit
t>eij \ rccoverv values arc then plot ted on" the Accuracy Control Chartas r funct inr , of t ine ( t h e da t e ) . Accuracy control,warninf £^c dear,values are recalculated every time c control chnrt is changed usinc n° lesr-than 20 reeult&.
?or both PreciEion and Accuracy Control Charto: All charts are reviewedand initialed by the Q A officer bi-weekly. The data used to calculate thelimits for each chart vi!3 be at tached to that chart.
Page 55
PART IV CORRECTIVE ACTION
A. CONTINGENCY PLAN'S
Thie section deals with the laboratories response to unacceptableinstrument response and unacceptable internal control checks. Shouldany of the proceeding occur; the Quality Assurance Director isnotified immediately. The Q.A. Director immediately begins an in-vestigation. The first objective of the investigation is to determinewhether or not the discrepancy has affected customer sample results.
If there in any question about the accuracy of sample results, thetesting is stopped and the sample rec.ultn in question are discarded.Samples whose dnto in discarded will be rescheduled for resamplingand rerunning. If any samples previously reported ore in question,the laboratory will notify the customer and all appropriate govern-mental agencies.
The next step in the investigation, should the above occur, is to de-termine specifically what problem occured, determine how to correctit, and determine how any problems discovered can be prevented inthe future. The Q.A. Director at the time of the incident will re-port the event to the Vice-President. Once the problem has beencorrected and the Q.A. Director is certain that the entire systemis back in control, sample testing ie resumed following written,approval fron the Vice President ana President.
The Q.A. Director will prepare o written report that will detailthe event. The report will contain as nruch detail as possibledescribing the time (dates) of the event and the investigation thatfollows. The report will include nil measures taken to get the systemback under control as well oc any new approaches to prevent the pro-blem in the future. This report will be given to both the Vice Presidentand President for their review.
PART V
APFEKT)!):
t f^ \\ \r „ - - • 1 1 1 f I ."•OXa QC Uc ' 1 1 f 1 I
A water sample for bacteriological analysis must be taken in a laboratoryterilized bottle. Water sample for realty transactions, F H A or V }
certifications, U S Public Health or E P A approval, and food and beverageservice to the public must be taken by laboratory personnel or a healthfficer. Samples of streams, ponds sewage or industrial wastes also require
_pecial procedures and equipment, as well as professional observations
"a1 ^r to be tested for potability must be collected in a sterilized container'.\ Inc. will supply you with the necessary containers. samp ling containers
*can be picked up at the main office at 1205 industrial Highway or arrange-ments can be made to mall the containers to you.
*-fake the sample from a faucet that is in regular use, not from a hose or cseldom-used pipe. The tap must be free of aerators, strainers, hose attach-"•-nts and other water purification devices. Flame the rim of the faucet with
*- corch or cigarette lighter for 15 seconds t6 destroy all external bacteria.Let the water run for five minutes, or several hours if there has been nc'ecent use of the system. I£ the faucet is constructed of plastic, the sanp-
_Ler should eliminate the flame treatment step and only flush the water systenA new or repaired well should be disinfected and flushed out before sampling.
Remove the cap from the bottle without touching the glass surfaces at theSneck . Fill leaving a half-inch air space at the top. Replace the cap tighlya place the bottle in its jacket. Write identification on the jacket labelsr^on the tag. Keep the sample refrigerated and deliver it to the lab within
*«30 hours .
If a fecal strep analysis is requested it must be delivered to the laboratory^within 6 hours. If the time constraints are not met, the sample will berejected and a resample requested.
__A11 laboratory sterilized bottles contain sodium thlosulfate, which neutral-izes any residual chlorine that may have been in the water supply, if a sys-tem has been hand chlorinated recently, it MUST be pumped out enoughto eliminate all trace of chlorine otherwise the analysis would be meaning.-
*less. An ortho-tolidine or DPD test should be made to check for residua]chlor ine.
_lf a supply is regularily treated by a mechanical chl'or inator, there should
Page 59
— _ QC IncJAM!* C D M R O i l A B O n A l O " ' f?
e a residual chlorine reading of 0.3 to 0.6 parts per million (ppm) at the_ime of taking the sample. The sodium thlosulfate in the bottle will neutral-ize the chlorine on contact, and bacteriological analysis will show the cond-1 tion of the water at the time o£ sampling. If the supply is treated with Eodinator, there should be an iodine residual of 0.4 to 0.5 ppm. A special
Iodine test kit is required to check for this condition.
k . b o r a t o r y sterilized bottle contains enough water for all bacteriologica)"analyses. A separate bottle must be provided if information on chemical qual-ities is desired, or if pollution is suspected. That bottle should be made)£ clean glass or plastic, not previously used as a container. It need not be
sterile but it should be rinsed thoroughly with the water being sampled, ancit must never have been in contact with soaps or detergents.
rite Identification on the jacket label or on the sample tag. Fold thisH-heet and place it inside the Jacket. See the accompanying sheets forilrections for taking a water sample.
~END REPORT TO: Name __________________________________________________
Adress
Phone
WATER SAMPLE OF: Name
*wrfD COPIES TO:
*'ater sample taken by ____________________________Date taken.
Taken at: source___ pump discharge___ pressure tank ____ faucet
Supply: drilled well ___ dug well ___ spring ___ pond ___ streamL^^ — •"•"'' ' ^ • • ^ ^ ^ ——~
I. » drilled well: year drilled __ feet of casing __ type of pumpX*-"' ————— —————
*-I f a dug well: depth __ type of pump __ type of covering ________
Recent repairs or construction _________________________________
^NFORMATION TO ACCOMPANY A WATER SAMPLE - ( c o n t i n u e d )
r ea tmen t a f t e r point where sample was t a k e n .
Jas the supply hand c h l o r i n a t e d r ecen t ly? ______ If so, was it t h o r o u g h l y
jumped out and tested to make cer ta in there was no res idua l chlorine?____
•% o£ analysis desired: bacteriological ______ domestic chemical _____
other ____________________________________
_In the absence of specific instructions, the laboratory will providea.nalyses and recommendations relative to the background informationorovided above).
VWVjXiOC Inc
V LAB IDsCustomer —————————————— » —————
Aoartss — ———————————————— — — - ——
APPENDIX DPSiO i
PERSON ASSUMING RESPONSIBILITY FOR SAMPLE
•
• -----
SAMPLENUMBER RELINQUISHED BY:
... ... .... . . . . _ . . . ....
a Qf ONTAINERS DESCRIPTION OF SAMPLES
Page 62
TIME DATE
RECEIVED DY:
•
- - -— - - • - - - - -
TIME DATE
^
^4*
REASON FOR CHANGE Or'CUSTODY
£>
q ...ITYI TOT " moj "-RY r1205 Induatrial Highway, P.O.Southampton, Pa. Io9oo r f f
APPENDIX E Qi r t (
SAMPLER INSTRUCTIONS
PRESERVATION
If a customer is requesting a group of analyses, tipecial oumpling containers naiat beutilized from each group (unpreaerved, acid, caustic, e-tc.K Pleaae review theparameters requested and select the appropriate sampling containers.
A customer ia requesting an analysis for pH,Cadmium, and Ammonia, therefore, an unpreservedcontainer und an acid container auat bo utilized.
T£: All aaaples should be transported on ice, upproxitaately >°C,
QUALITY AiinffiAJICE KAKUAL FOR QUALITY CONTROL LABORATORY
120;- INDUSTRIAL HIGHWAY SOUTHAMPTON, FA.
A KATJAL rcn TK£ DIALYSIS C7 DP.IKKING WATER
PAP.T II
MICROBIOLOGY
IKTSOD'JCTIGN
Quality A."-sura,nce Manual for Quality Control Laboratory1C05 Induct rial Highway Sr-utharrt-i:, Penr.cylvania
President: Alan Srh -.-
Vice President: Thomas Kines
This document contain;: n list of quality control y.rocccur?c- thathave been instituted in the laboratory. The object of this t-lanis to --rovicc- a listing of quality control neasurcs for thelaboratory to utilize, and alrc to ^r^vide a means to insure thatthe quality control ^rocedurer outlined are fcll '.-'eri . The Plan willinsure th£i every check that cc-.n b<? rrnce, will be rrace, co thstcats *:r^cucoc bv Q.C. Lnb^rr.torv will be -rreci^c-, accurate anc re-?ro -
» > » * * " *cucaoie. -v e ir.cnual is divided into tv;o rartr. Part I outlines qualitycontrol measurer for Chemical Anslynis and Part II outlines qualitycontrol me-: azure 3 for Micr^bielogi cal Analytic .
FAST I SAILING AI.'D SAMPLE HAJOLIUG 1-2A SAJ-TLINO 1B SAMPLING INSTRUCTIONS 1C CHAIN' CF CUSTODY 2
PART II INSTRUMENT CALIBRATION AKD ANALYTICAL PROCEDURES 3-13A !I-!£T5U1-ENT CALIBRATION 3-£3 AI;ALYTICAL PROCEDURES 9-18
PART III TYPES 0? IKTERjVAL QUALITY CONTROL lS-20A STERILITY CHECKS A3vD OTHER COfiTROLS 18+19B £?!IT SAJ-:PLE PROGRAM 19C DATA REPORTING
A CC.NTIN'GEKCY PLANS 20
PAST V .^PPEN'DIX 21-25
A Q-C. SA>TLE REPORT 21B DIRECTIONS FOR TAKING A WATER SAMPLE 22-?4C Table 905:111 KPN Index and 9^ Confidence
Limitr. fr.r Various Conbinntions of Positive and Negitivc _ r
QC IncDUALITY CONTROL LAQonAionv1205 INDUSTRIAL HIGHWAY • PO D O X ^ l - i • SOUTHAMPTON. HA 1 B 9 G G - O S 1 4 • (?1 5) 355-3900
?AHT I SAILING AND £AKPLS HAJ SLING
All s-r.nr lin<r is concocted in accordance1 with the pr-cer.urcs outlined in theEFA "Manual for the Certification of Laboratories An-lyr,ir.£ Drinking Water",
^-OOZ-)- Oct. 19S2. -
When a QC Laboratory field representative collects a sarrilc, he or she completesa QC sample report. (Sec -Appendix A) This report includer:
1. The date cf collect icrj .5. The time of collection.J>. The source C inclvt'.in£ nanc , loc^tirn, ant1. Eaa;>le ty-es }.^. The preservative u^cd if ?/?.-! i cable .5. The s.naly£ir. recuiroc.j* '6. The ns.r:e "r initials of the collector.7- Ar.y pertinent field cr-ta Cpri, D.C. , Cl residual, etc. ) .
A v.'st c-r :roof t re;, co" -lctc v;ith thn rccuireo in forr.ct ion , is £ ecu rely attachedto the sarr:le brtt t lr- . Ki crobiologicril sample s are iced curing transit andrefrigerated ct 1-^ C during storage in the laboratory.
All QC field representatives are thoroughly trained in correct ssc^ling pro-cecurer. No field representatives are authorised to rrlle^t san-jles untilhe or she hac received training frora the Manager of Field Services.
B- SAJ-IPLIIJG iri57RUCTION£
Scn^lir-2 Procedures are ac follnws:
1. Microbiological - The tap must be free of ac-ratorr, strainers, hoseattachments end water purification devices. The faucet is flar.etreated, us- ing H ^ortablu burner or porket lighter. The water is thenalln-./e-^ i" flor.1 for 3 to 5 minute.- to clear service lino. S,-n.-les arethen collected in specially ;-ire;-.arcd, stc-rili-ed bottles, and are tnbe filler! rnly ~$/k full. If the frucet is constructed of -Ir.sticor contains "lastic -;arts, the 5Dn:')lcr should eliminate th'.? flametreatment, but v;ill flush the system lor 3-5 minutes before cnlloctingn £an--:-lc . Sampling is accomplished in n caroful ascetic manner.If there ir. any doubt about the clmnlinn-s of p. -articular sample,discard thr.t r.arr-lc-, ?nc: then r>ror:ecd to reS'im_.l(.-. At thi:--. %"int ,a sample re-.ort and tnr i^; filled out v;ith ell relevant dnta.
QC IncDUALITY CONTROL LABOn/.TOnv /Al
1305 INDUSTRIAL HIGHWAY • PO BOX SH • SOUTHAMPTON. PA 1QC>6G-OM 4 • (?l 0) 3S5- 3900 fttfls/t
The tag *•'• "C-"1 attached to the sarr-lc cor.tniners. The sar^lcis icet1 irnr-.edintely ant! tr anchor4. PC; to the- lab^rr-.t^ry fr.r analysis.
I f a c ur -t cmor" conduct s hi c. r her <"*v:n S.?.T. •• ling , a c ~vy of "'Di roc 1 1 *~ns-for t akinc o writ or ca^i-lc" i^ frrvardcc; to hin ^r her al^n^r \\ritha st erilizcd sanr-le container. P .cr-.ce re for t r Apr-cr.di>: B f nr thedocur.entatirn of the Sr-r./linc I.- ntr'jcti cnr: .
2. Cheni-al - All chemical sen) ) line thai ic required can foll^v: themicrobiclogical ssnnlir.j; v.'ith ut ar.y other ^reyaratinn . If chemicalssnv.linE is the only requirement, then follow the same -rocecureused for microbiological EEnviiir.c t?xce-t flame treatment car. beeliminatec).
C. CHAIN OF CUSTODY
This section lists. the ~>rocccure that is utilized tr^ r.air.tain the integritynf all £nn :les ,( i.e. the t ra cl-'inr *^f cnrr^lc-c fron their receipt t hrc'jjrhanclyci.'i and cis'-.oKal of f irji"h*rd rn le.-:): The -^rrcecv.re ured ic- b?. £edon the reruirer"ient t~ t hat are found ir. ''Manus.1 f cpr t h? Certification ofLaboratories Analyzing Drinking Water", Chair: of Custody, pg. 5^-55.
The •trcc?cure for strict chairs r f curtsey is as follov.'s : '.vlien 2 rairplcis c'-lloctec by r Q.C. LabTntory field representative he or she fillscut s C.C. Lsb. sample report CSee A^L-endix A). This report contains:
1 . TJie dote of collection.2. The time of collection.3'- The source (including name, location cnc sanr-jlo ty.o).
5» The ar.alycio recuirc-d.6. The rs^rncorinitialsofthccollector.7. Any -ertinent field data (-H, D.O. Cl residual, etc..).
Thir. snn-:le report serves as R chain of custody record for bacteriologicalEanrjlcc.
A Laboratory cuctndian has been designated v:h v;ill receive sarnies fromn field representative and thercnftcr tnk« full resi:onsibility for in-suring the1 integrity of the samples. Nicolo-ttr Holt has- boen designatedwith thij responsibility. Two nltcrnntos have been dcs-igpntcd to os.iir.tin her abrcnco; they are Jl^-j Cohon nnd Juttn Fisr.ol.
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QC IncQUALITY CONTROL LABOPATORV
120S INDUSTRIAL HIGHWAY • PO BOX 0 > - 5 . SOUTHAMPTON.PA 1 G D G G - 0 5 1 4 • (?15) 35&-3900
^-J O'tii.-.-il EC. 'tic should c~me t^ rert r.t tho exact -em'••-«int. (If greater "r l'-rc t h n n ICu (Tin.-., nri jur.t rcaleex" -anri'T. un in r kr.^b ac ju rtr.cn t on t^p r"." sralo ) .
*O Repent steps 1-J , two cr three times to check repro-ducibility of balances.
50 Place a clarr "S" ICO.nc veig-it on balance pan.6) Sot v.-eicht r^r.trol k.nnb t" 0.1 £"•?) Turn - ion rc-I.er.i:.o to po.^it i "n 1 riryj ret :-.cr^ jv^ir.t with
back t c zero . The o->t i cr.l scale should c-~me to restexact ly at 100 me-
o) Tf rer.cinr is crent er t hr.n cr less th?.r. 10': m/r , 21 r?stbslanre e.r.d on j\:rt se^.si t ivit v v.'j th kn^b m tr ; ^f balance
10) K«7e.-t Etejjr J-? two or three tine.*:.11) Piece IGCm-E anci 100^ veirhtr on balrnc^ pan.1Z ) Sc-t veirht control kr^bp. to 100. 1 grr.E.nf lease balance
fine: cet r-ero -j^int wi th ""ticnl zer-^ Vcr.-^b.1~:) V.'ith brlancc- irelcF.^rrd, rlov/l*,* tu rn v/ei r rht control to
1*":O [~rr,?. .1^ } If rc^le doc-s n^t come to IC-'Jfrr.r -f/- 0.1 me, rc-;:er;t .
pr^rc- ' juro two or throe timer:.15 ) » * renr-i t ivit v cnnr. ot be c^rre ct ec call J-'c-t ler • Rr-rjair
Pan Eslnncrc
a. Q.C. Inc. policy requires all par. bslr.ncos to meet thefoll^v/inc criteria :
1) Ealnnces are checked onoe a r.onth urinrj ; t least twoclass "S" veijrhtr; (5% and 50^). T':esc- v/cic'^-tr mu^t bedetec ted to the nearest .01 gro. The dr-tcr, i-vn which thechecks were ">erf--»rmec, the r.arrr <~f analyr.t and other">e r t i n i % n t inf ^rrr.nt i<-n muct be r^c^rcec in a lor b*~>^k .
2) Bnlnnccs srs ..heched and cd . ius ted annu.-lly by n Met ie rService- person and the dnter sro rec"rced in a l^g book
b. Monthly the accuracy nf balances is checked u::inc ? ^00 mg wt .under a load of 100(3 nn° 3-50/r 1 tho r-rocedure ir> out l ined
1) Check l (»vol nf balance ^n l-.-vcl?) Turn bnlonce on - check focur and a l ignment .3) Zi-**o b-'ilnnce v/ i lh optical r-cnle unin^; acre knob.'<) r incc l^'-^G cl3:;r "S" weight on nan .5) Sr.-nlo r-h^ulc! rend exactly l^'-O pmr (if grcat i r r or ler.:;
th.'in 1/0 cnr. ndjur . t r-calr ex;.an;;i<->r. ) .
0) Sot weight cT.tr-1 kn^b to 1^-0 0rr.r.?) Optical r-ale should c^me t^ the exact r.cro j-.^ini .8) P.* >eiit twc or thre^ t i rnor- .9) FIccc 1^-C.l gr.s urine cl-ncr- "S" wcicht on pan
10) Set weight control knobn t^ lf:0.1 gms.11) Optical ccale nh^uld rec'd exactly zero.12) Pcnovc 0.1 pm v:ci^ht and re " lace several times t r insure
sensi t ivi ty.13-) Rc^oat rte^s" 4-12 usinc a 1^0^ class •"£" wcicht .lM If accuracy or sc-r.citivity problem? aro noted ar.c they
c a nn'-t be corrected , ca l lKet lcr Re/.air Service .
a. The nccurEcy of all tr.crm.-.r.et err, is vcrifiec by ccr.parir.r;then v.'ith an Is'BC cc-rt if iec therr.rriet er.
b . The veri f icat ior. is cone yearly sr.d the foll^vinr inforrr.at ion ' "ir recorded .
1) E^oh theiT^rirter ic, riven 2. u n i q u e intier-tificatiT nunberrocnrdc-d alrn^ v.-ith the icc-nt i f ica t ion r.ur:b^r *^f the N5Stherr.-'Deter .
2 } Doviati^r. IT f rom t h(* N'I5c "t h cr jn^rio t CT* sr c r c- c or "; f? d .J) Dates on v.-hi ch veri i"i cat i rr.n s re done arc recorded .") The init ials "f the: *:crc"n dcing; the ver i f ica t ion are
re c^rd PC .
PK Meter CCorr.inc)
a . The ?K He tor utilised meet s the f nll^v/ir.g criteria:
1) Accu racy is within •*•/- . C5 FH uni ts .?) Kr edibili ty IK v.-ithin +/- 0.1 units.
b. The prnt^rol f^r '••jeratinc; the pH 1-jrter is listed br.-lrw;
1) Eloctrr-des ore rinr.ed v/oll wi th laboratrry ;iure v/atera f t e r each rendinc-
2} Electrode.*: arc dipped several times into the next samplebe- fore- readings r rr- ' .nkf.-n.
J) All r.nrnplcn ore r t i r rnc; curijic ncrcurorrcnt .M Electrode." are stored in laboratory pure water or in pH
7«.0 b u f f e r mlutirn r:: r.'jficestert by tlie mnnu. rDct\:rf jr .f>) The PH M ^ t r r ir. n^t r - t ^ r rd ^r uretJ AH a nu:tr l r u r f a r e .C) C^mmcr icn l b u f f ( - r c u.-.nri nro dn tcd when r ece ived .?) '.Junrlorly the PH J-'^ter IF - r h e r k e d w i t h EPA known oH ctandarrt:
nn'i/^r ERA A'T.OT .kjr~v;p. rtf'. . . f inlut i i~ns. The dn tn ir rcrnrdcdi n n bound b -•"!': .
QC IncDUALITY CONTROL LAQOnAIOnv < < , , , , f i j _
1205 INDUSTRIAL HIGHWAY • P.O B O X M * - SOUTHAMPTON. PA 1B9GG-OS) f, • ( 2 i & ) 3M-3900 (Red)
c. pll J-ir-ter is calibrated bnf^rr- each urc with two bufferr tern en roc brri'.-ketinr; the VP.IU-T. t^ be men cured \i . e. ^.0 and 7.0)
1) rln-'_> the elec'.r'xle firrt in a r.olutirr. of buffer (7.0)and G', ir (rcntly.
2) V.'hc-r. the meter h3.r Etabili?cd, (Meter rendinjr doer not, adjust the reading to read 7-0 u^ing the- Cnl
'•) Next remove the probe f r rm the b u f f e r , rinr-e wi thcirtilled v;?ter, careful ly cnb dry wi th a clean ticsuet ^ remnvc exce^r vat cr and pi.?. ce the "robe int^ the- nextb u f f e r ( L . O ) .
M Stir gently ur.til A c^r.stnnt valve is arrived at.5) Adjus t the meter t <•* ^ .0 using the pl^^c control knob.
(V.'arr.inc ,i f 1'°- ur^t adyjr t the value nr-re than 0 . 2 p Hu^itn tiirrc ray be ? problem v.-ith the probe and /or therr.cter ) .
A cnilv chec' ' ir mndc ^f the rreter a f t e r thir cs-libratinr.hac tr-.--.Crr; plr.cc-.
1) A •nii ( 7 .C) b u f f e r ir- usee:. The -or^bo c.nc: r.ctcr are sd-_ *
justed tn this buffer.?) Next v.-ith^ut further re justment a buffer ( .0) and
buffer(lO.C) are measured and the %F?-lues rc-ccrccd in
5. PH Meter - F.
The Haci^metcr Motor is rtan.darriiz.ed in the same fashionBK the C^rninc Meter. Urine tnc same j-H buffer solutions sndthe came procedure. The instrument is programed to operateand calibrate. The instrument' follows throu'rh with- the procedure,utilising prompts" as 2 guide. The procedure is as fcllov.'s:
1) Plnce the probe in th« buffer (7-0)?) Pror..?- th« calibrate p'A butt-n.30 Aft or stirrinc and ctabiliznti^n *^f t h f j meter (a
conr tant value is Achc ived ) rr^r-s calibrate pH again.This setr, the meter tr^ the .pH vnlue 7.0 .
*i ) T!ic- motor next tcllr- ynu t^ "l.?ce tu-.: pH -ircbc ^ n thenext b u f f e r . »ur choice cnulri- b<? ; i .o or 10. C- for
. example .
QC IncDUALITY CONTROL L A B O R A T O R Y , i i1205 INDUSTRIAL HIGHWAY • TO BOX & U • SOUTHAMPTON. PA 1 B9PG-051 -1 • (2151355-3900 (Red)
5*) £tir crrsin , mui vhr-n n c r -n r lnn t . val'.se ir« a t ta ined
6) Finn II:.' v.rcrr. but ter : Ir.boler. •or! t^ £;<•• i n to rend m^de.? ) J'-'inc^: *"H v-r^bc into .~-.rr--.lo , ri i:-, nnd when a c<"*nr.tant
vnluc in achcivod record thnt value .3) When monnur in^ snn-:lc?r o:- rtfindarri.0: alwavr* rinne probe
v:ith water t e twccn urer- nnd fir.nlly rinse with ther^lut i-^n yru arc- ab-~-ut t ^ r^ccicurc next .
9) The meter is checked monthly \irAng EPA and/or EHA ASECC.knrv.r. standard.**.. This data is recorded in a bound bnoV;.
6. Cnnduc t iv i ty Ke tc r ( K a d i r m e t e r )
a. H a ^ " t e P n n c G
1 ) The pr'-oo it self is r»nly rir.sec v:ith distilled v/cit er .2) Tho instrument is checked v.-ith a .01 KC1 standard daily
' -7;O C KC1 t^ 1,000 n u ) % Kc.?i;ltr mu::t nnt dev i a t e byrn^re thr.n lC>o from tho t rue vslue "f l,^0o ir.^h^c at 25 C.
J>} The cell , '-.-hen n^t ir. ^se, i^ lef t s^akir.r in distilled\;at er .
b. 1-icaEMrcmer.t
1) The vrr-be r.urt be ringed v:ith the sample or standardthree tir.eE before ?. reading ir initiated.
2 ) P - s c e T i r o b e i n t o sa^i^le and stir v.-ith magnet i c stirbar.
3) £nr-;:lc£ are automatical ly terser 2 turc; c^r.^enG'-ted .** ) On;e the aeter h.*>.° stabilised take th« value on the
meter as your rending.5) 1-ieter is checked monthly v;ith E?A arO/nr E?.A ta--«''.rn
re f erence r.tandardr . These rerults, are recorded ina bound b'-ek.
6) D^.ily the conductivity of th -v lab^rat^ry *-urc w?.t er ischcci;ed and recorded in a bound brv.Vi.
7. Rcfricirstr-r for r,amp;lc r.tornge
Tlio rofri^c-j-r' .t^r (by P-vcr, m>~del double dr T) v.-ill mnintsin at fcrric rot urc of 1 4:o ^ C. Thorr.omet^rr: ur.cf; (oalibrotod annually)are cr:jcl'J-"t('d in 1- i n c r c m n n t c and bulb.-, arc immernod in liquid.There will be Ivn ten -erotun? stations (h igh and lov.- posit ion) ond they
' ' will bo chocked p.r.'j rf. 'corued /J-! and FH ear:h './orkin dr.y.
QC IncDUALITY CON7ROL L A B O R A T O R Y
1205 INDUSTRIAL HIGHWAY • PO 00X011 • SOUTHAMPTON PA 109fiG-051/. • (21 S) 350-3900
Tn«:ub.Mti ^n Uni t .
Thfr t'.'o inrubr.'.^rs (OCA-ri 'ocic i^n n"dol 6]-') vill m a i n t a i n 3ninterns! t err. -erst -jro ^f 3'^ •+/'- C .? -C,. Each in cubai^r will navetv.-r- thermometers (O.T1 C increments, calibrated annually ,' locatedon. t-"*1: and bo t tom shelves, bulb irmersou liquid! Tempera tu res are
ded both A!'. p.r.ci PK.
9- Hot-Air cvc-n (steri l izinc)
The nvr.-n Oerpnt ch Cvcn, nr-col LH5-1-76) v.-ill be ucod f^r sterilizing•oi set? only. The- thcrn^mr- ter used v.-ill hevc at lep.ct 1C° increments.It «? bulb v;ill bo -.:laco'J in snnd arc: will have a capaci ty , to goto at least Ic-C C. Stcrili ir.ti^n cycle? v.'ill be f r_ - a rain i mum oftwr h^urr . The- hot 2ir rvcriE r.re ecu ivped with chart recorders.fcr t enirerst uro riT.it r ing , sr.O n ft -?r 'jre , the ca" e ET.C t icie i^rec^rd^d on each chart.
10. Autnclavc-E
The au t r claves hsvc o tc m orr. turr- CUT-JTC- v/ith renror or. c-i-i-.eusi ,an r,i-.crot irr.," 1 s r fc - ty vc.lv c u'hich ir ( t C T t o d mrr . th ly) and v;illr.nintnin rtcrilir.atinn te.Trv-crnturo durir.r, o (12-15) minute cycle.IVie da te , tirr.? cr.c tcrr;.jeratur« for each cycle irr recorded on a chart( ch.nrt r, are k^.T-t on f ile ) . A 15 nir.ut c- and 3- minute cycle ischecked, wi-h a ECO :; watch, for each unit each nrnth. Sterilityta ;>e and a maximum rewdinp tl ic-rmnnet er rre ale--, ured for each cycle.A service contract is maintained f <->y each unit .
11. Water Bath."
a . Writer bath. z v.'ill be drained and cleaned v:eekly -b. Terr'.er.'it.urr- checkr v.'ill be nr>de AM and PJ-I . If variation
frr.r. ur:e t nrr;:crature occurs no t i fy Director cf J-:icrcbiol"cyv;hn v.-ill t.^Xo corrective action irrmc-ciately.
c . Check t i m<? cl^cV:.*: monthly to insure T;r<~-'; ^er ctart in^ and
d. Electrical rc-y.airs are r.ndc when nocesrr.ry.
Correct ivo A c t i o n :
1) Roclu.'ck nil SDD;:lo:: involved dur ing .the t im» "f mal-f u n c t i o n
P) Po n^t urc unti l b f t h ic f ixed.3) Rc-.air bo th n>: qu ick ly as ••rsr iblc- .
Pace- 9
C IncOUAUTY CONTROL LABOnAIORV
1?05 INDUSTRIAL HIGHVMV • PQ BOXSl- 1 . • SOUTHAMPTON. PA 109CG-0&1 A . fTl 5) 355-3900
B. Annlvticfil Pro^cdur^::
Erui.*nent znu Ka-c-rialc - I-'"st Probable1 Number (K?N):
stic petri dish or.Pi'-pts 1.1 ml and 11 mlCulture tubes lo y. 1^0 mmCulture tubes 6 y. 50 rcn (insert tube)Flattie cavsl-'etal racV.cInnculating loop 3 -m I.D. Incculatinc noedleAutoclaveIncubator 55 +/- 0.5 C.Leuryl Try/ tree Broth rl: 6.8 (double strength ;--K 6.7)Brilliant Green Lsctone Bile Broth y?H 7-2Er»sin Kethylene Blue Agar pH 7.1E C Kec-iurr. K 6.9Nutrient Agar rH 7.0A"ice D=-xt rocc Broth ^H 7 . i?Ethyl Violet Azide Eroth »-.:-! 7.0Try;;t-ne Broth ;-K 7-0Eir.min's Citrate Ac^r j>n 6.5MRVr (Buffered Glucose Brnth) pH 6.9K^VP.C' s reagentMethyl Red SolutionV--£;es Proskauer Reagont
1. Cnlifn.rn (MPN) Presumtive Test
a. Inoculate a series of ferncntaticn tubes containingLauryl try;-trr.n br^th v;ith 10ml of original sample,or dr-cinal dilution of the orginnl sample if con-tnnir.ation ic expected.
b. Incubate at 55 -«•/- 0.? C for 2-4 hr. +/- 2 hrs.c . Examine for coc production in inverted tubo . Tubes
shov.-ing no gao r.hculd be returned tr. incubator f^r anadditional 2^ hro.
d. Examine again at US +/- 3 lirs. Those tubes shovjingE^s v;ill be confirmed.
?. C^lifnrrn (I-iPlO Confirmed Test
n. After 0oi'.tly shnkinc fermentation tuber-, trnnsfer oneiT/ful v/itli a ctnrilt? Jmm mct.il l^op frori Lr-uryl tryptoseto brilliant crocn lacto:--,c bile brrth.
QC IncDUALITY CONTROL L A B O R A T O R Y
120S INDUSTRIAL. HIGHWAY • PO BOX OK- • SOUTHAMPTON. PA 109GC-051-1 • i?i5l 350-39000;
b.. Incub.-to r.l 30 +/- C.l :Cf^r Jj" +/- ;• I'.rr.. C:-?c'/. at,?-'i hr. Ar.v £/T f rvnc i t i "" ir.dicstos n - j n r i t - v e con-firne'J t'.-rt -
Oliforir. Q-IP::) Crr./lc-tr-d T«r.t
r.. Streak oil -"citive brilliant n rpc" tubf •.'•:- ^ntn eo^ir.mothylT.T.c blx:-:- 2(T.-?r ^Ic-.lc ur-inr r.r. ir inculciinc ncccil?.
b. Invert ar.c incubate plates at y^ +/- 0.5C f'lr 2^ */-2 hr-.
c . From er.ch ••'In t e sVicv.'ir.j1; t ;,••••! en 1 c^l^nicE t r an r fp r nncv:cll is-^lf-t oc: cr-I^Tij' to Lauryl tryptece broth Eir.c; oneto a r.utrient aj;r.r clar.t . Frons a-t^icnl olate^ taket v.'c c^l^nicr cine t r nn r! Tor t li ciT: to LUMITV 1 t ry '" t ^*sc br . hDr.o n nu t r i en t nr r r r lnnt .
d. Incubate at 3-5 +/- 0-5 C for 2^ -*•/- 2 hrs or ^o +/- 3 hrc.if n^ EF-r- -- "roducen in the broth at 2'^ hrs.
e . The f rnat i - r. of gas in a secondary I.suryl t ry~ t *^5e tubennd a E r am -*-"in shov:in£ crsra negative bacilli (ncr. -S7;crefornir.r) nr.y be conr-idcrcd ." yri t ive Completed Test.
1. Where 10 ml of sample is used, Lsuryl tr^-tose broth mustbo dc-uble s-trc-r^th.
2. Uhen g^air. Etainin^ u-o E C-'-li (ATCC 9739) s.c- a positive ccn-N^ /. tr^l and Bacillus Subti3ir (ATCC 6633 2s a ne-rative control.
3- Gram rtair.inr should be d^ne on an lS-2 hrs -culture.^. 1OJS ^f all positive carnal ee froni cor.firmc-cj test should
be run through ccrr/.leted test.
5- Reports, mur.t 'r.tate that results are questionable, if time.limitation?7, are exceeded (i.e. if "the cample is tested between30 and 43 hours frnir. Eam;:lir.£J.
Noto:
Re;?^rtin2 mont probable number, MFII, results (total coliform)
The re^ultr of the confirmed or cor,-;loted tont nny be obtainedfrr-n the 1-IPN tnblt- (Go'-- A-jpendix C) b.-j.-rc-d on t}ie number of positivetube.-, in onch di lu t ion. P.c;^rt ac nur.b^r of total Cr.li
a. Fr~m all ^r^trur.ptivc ;-o^itivc Lauryl try/'orc; tubesinoculate nn £ C tube.
b. Incubate £ C tubor* in water bcth nt U^.5 •+/- 0.2 Cf^r 2^ hrs. Gor. fcrrrr.t icn in ci cater- prnitivc fpcalcrrntnmin-" t i^n .
Note:
1. Tiir.c from inoculation of E C tube? tc placing thorn in a v;aterbath should not exceed "^0 min'jtec (v;ntcr level in bath is above.the broth in the tubcn).
RSPCRTIHG )•?:•: INSULTS (rSC/J. COLZFOFJ-Q
Calculate fecal colif^r^ dor.sities on the basis of the nusiberof positive EC fermentation tubes using the KP!<" table (SeeAi^-er-dix C). Ferort a?. ivjr.ber of fecal Cclifrrnc/lOO ir.l .
5. E. Coli (KPIO
a. Fr"m thp nu t r i on t n f~2 r* slant in th^ c :"cr";lc t ed t e ??t licrht Ivir.cculate 1-P.V? broth, tryotnne broth, and a Sir^n^n'sCitrate slant.
b. Incubate according to chart be lev: :
Indole 2^ hrs. Q 3? CMethyl Ked 5 cays CS 35 CV P i)S hrs <2 35 C
Citrate 9^ hrr S 35 C
?i e a c t ion c :
Indole MK VP Citrate
E. Cell
Citrobactcr Freur.dii
Klcbciella
QC IncQUALITY CONTROL LABORATORY
1205 INDUSTRIAL HIGHWAY • PO. 0 O X 5 1 4 • SOUTHAMPTON. PA 1 8966-051 A • (215)355-3900
6. Fecal Ctrrv-tocorrcur (HPK) Presumptive Tnct
a. Inoculate g series of tubes cmtair.inc ar.ide drxtrcce(AD) broth with rtc-:irc?l dilutionr of the original sanr.-lo( single strength AD for inoculation of 1 ml or loss. Use.double strength AD for 10ml .inoculation).
b. Incubate at 35 +/- O-5 C for 2^ +/- 2 hrs. Check forturbidity. If nr definite turbidity is present, re-ir.cubatcar.d check at ^S +/- 3 hrs.
c. A positive presumptive test shows growth consisting of tur-bidity in the medium or a button of sediment at the bottomof the culture tube, or both.
7. Fecal Streptococcus (KP'O Confirmed Test
a. From positive azide dextrose tubes, transfer three loopfuls(using 3mm loop) ir.tr Ethyl Violet Acide Dextrose (EVAD)tubes (ICnls per tube).
b. Incubate at 53 +/- C.5 C f^r 24 +/- 2 hr£. Check for tur-bidity . If rr- turbidity, repeat transfer from azidedextrose to watching EVAD tube. Peincubate (35 +/- 0.5 C,Zk +/- 2 hr-).
c. A positive c .nfirT.ec test iz the formation of a purple buttonat the bcttoci of the tube, or occasionally dense turbidity.
8. Kftmbrane Filtration Mcthrd (f-iF)
Membrane Filtration Equipment
Six plr.ce Hydrosol Manifold20 liter Stainless Steel Frescure-Vacuum TankVafiuum-Prcccure Pun::Stainless Steel forceps (No ridges on the inside graspi^c surface)Plortic petri diffhcs 60 mn x 1^ mmIncubator 35> +/- G.5 C - 9Cf> humidityPi ;etter. - gl^ro (1.1 ml + 11 ml).Prcr.terili^ed Filters - Golmnn (^7 mm in diameter, C.i*5 mioron
c. The KF unitr, (Hillipore) are r*f rtrinless strel, cl::cc andoutoolavp.bin plastic. They are free from scratches, corrosionana leaks.
b. The glees funnels arc checked ur-ing a graduated cylinder andremarked if the lOOnl lino is incorrect. The funnels arecovered when not in use to prevent dust contamination.
c. Before initial use each day, the whole (MF) unit is autoclaved.The UV steriliser is used to sterilise each funnel (sanrrlecup and glass base) before next series.
c. The funnel:: (sErr'lo cup and base) arc UV sterilised for 3minutes. Uning en Aseptic technique (with stainless steelforceps) place the presterilized filters (cellulose ester,white, A-7 ciri in diameter, 0. 5 raicron pore siz,e and grid marked)onto the glass bcce of sample cup. Place the sanr.:-le cup entop and secure the sample cur .to the base. The assembled unitis placed securely onto tho stainless steel base and used within20 minutes. If the 20 ninute time limit 15 exceeded dis-assemble, sterilise and reassemble the sample cup.
e. The lot nuir.ber and date of receipt of filters and pads are re-corded. The recovery and pcrforr.iar.ce of the new lot V£ theold lot is al.to recorded.
f. The presterilizec plastic KP culTure dishes are placed insidea tight-fitting container and placed in the incubator.
£. A lOx magnification device with floucrescent light is used toaid in counting sheen colonies.
h. A start and finish control is r\in .on the dulution or rinsewater. If any of these show positive results, all samplesfrom that run are discarded and resampled immediately.
The analysts involved in reading results will c-unt the sameV-latos (of certain samples) ond compare rer.ultn (done monthly),recording both in record book.
9. Membrane Filtration (MF) Moth^dology
a. Procedure
1) The number ^f sampler- removed fron rr-fri^ornti'-n v/ill belimited to n ?0 minutes start t^ finish rule.
Pcire
QC IncDUALITY CONTROL LABORATORY1205 INDUSTRIAL HIGHWAY » P.O. BOX 514 . SOUTHAMPTON. PA 18960-0514 • (215) 355-3900
2; The mrr lo shall be rhshen 2? tiracc (the shading i-accomplished within 15 ner^nt's by novinr the bottlewithin a 1 foot arc:). IT an aernbic pl.-te c--unt isrecuir-?d nn aliquot is tnken for that pur;:ose. Next,100 ml of sample is poured into the prccalibratedsample cup. The vacuum pressure valve i.« nr.w openedand the sanr-lc ic allowed tc filter. At thic pointthe next sacrple can be placed in the second sar.ple cupfor filtration. The same procedure is carried throughfor each available sample cup en the manifold. Oncethe sarnie has completely emptied from the funnel, a pre-sterilized squirt rinse battle is used. The funnel isrinsed three separate times (allowing each rinse todrain before the next is begun). The valve is then closedand the- filter remove with flancd forceps (without ridges)and rolled ont^ the ,m-endo !££ agar plate (plate shouldcr.ntain ^nl m-endo UBZ agar). There should be nc air-bubbles under the filter. The dish is placed in a tighlycovered container and incubated at 35 •+/- 0.5 C for 20t-** 22 hrs.
Eeportir.g results
1) Coliforms detected by the KF pr^credure are reported ascolif.~rm density per lOOr.l ..
2) Confluent growth - membrane covered with bacterial growth..3) TNTC - greater than 200 total bacterial colonies.*O If reported as c-nfluent growth or TNTC with, less
than 5 distinguishable sheen, colonies, another sample isrequested fron the sar.e sair;]?ling cite as soon ac passible.
5) If reported as' confluent growth or THTC with 5 ormore distinguishable sheen colonies, this indicates anKCL violation and a rccheck caranle ic r- quested fr^m thesame campling site, as sr.<->n as porsibl-; .
I'ote
1) The tyi-icol coliforn colony has a pin' to dark-red colorwith a metallic nurfacc sheen ( checn aroa my vary frompinpoint to a total r.urface). The 10 x binocular viewingrco-:c with a fluorescent light ir. u. ed to count theKF plater..
H -te'
?."} The idc.-il ;vl:>to bar. botwcen 20 nnJ T,0 colifnrm c^lnnirr,nnd cnr.nnt hnve nnro thnn 20'' coloni'-*." "f nny typo. Ifconfluent nr TIH'C cr~v.-t!i occurs, th^.vc r.ar.-ilen will be re-
When rerunning the np.m-ler-,they will be divided betweenceveml mnmbrr.nrr- (exrinplc 20mls per 5 membranes —lOGnls tested), the total c~liforms or. all vlntec com-puted ac- per 10'> ml. (Standard Methods for the Examin-ation of Water and Waste Water 15th Edition p. 900)
1C. Fecal Coliforn (Mr)
a. Follow the same procedure as for Total Coliform (KF).b. Place filter in petri*' dish containing 2.5 ml of K-FC
^, broth with 1.5# agar added.c. Invert dirh in a water proof plastic bag and incubate sub-
merged for 2^ hrs at kk.$ C.d. Examine filter for developnent of blue colonies. Blue colonies
indicate fecal organisms.
11. Sample Containers
a. Sample bottles, are wide-mouth plastic or non-corrosiveglass, and have a screw cap with a non-toxic liner. Thesebottles car. withstand repeated'sterilization.The screw-cap for non-corrosive glass are used only onceand discarded properly.
b. The sample battles have a capacity of 120nl (k 02.) andars free of chips, crocks or discclorations.
***" 12. Glassware anc Plasticware
a. Glrssv.-are is of borcsilicate glass and free of chips, cracksdiscoloration^ or worn markings.
b. Plastic items are clear and are made of non-toxic materials.c. All graduated cylinders arc accurate to within a 2.?£ tol-
er.ince. Pipets delivering 10 ml or lees must be accurateto within a 2.5# tolerance.
13- Culture Tubes and Closures
a. Tubes are of borosilicate glass and are frse of cracks, chips ,or dircolorationc. Tubes for the presumptive tent procedure(MPH) are of sufficient ci^c (iSx 150mm) to contain the mediumpluc r.nrrnle and be < 3/^ full. The fermentation tubes arc 6 x50mm (inr-ert tubew).
b. T-.ibo closures are clear plactic (In-re fitting) and arc free\1 of crack.': or discoloration."..
QC IncOUAUTV CONTPOL LABOHATORV
1205 INDUSTRIAL HIGHWAY • P.O. BOX 51 A • SOUTHAMPTON. PA 109Gr.-OSU • ( ? 1 5 ) 355-3900
Glace ::i';etr- arc- frtc of chi^i:, cracks, worn r..irkin£i' or dis-colorati-ns and they are stored in stainless rtocl canisters.All ovcneri cDr.istcrs arc reautoclcvec each day and any dis-pocable sterile 7)ipRts ere res-osled between major use periods
Culture Dishes
Frecteriliz,cd plastic culture dishes (loose lid) are used.Opened 'jacks arc reseslod with tare between major uses.
16. Inoculatinc Dqui^rae
Platinum-Hh^ciur. lor*ps with a 3^^ I.D. lor-y are used. These aresterilised by hc-ating in open flarr.c to "red hot".
17. Media
The cnnrr.ericolly ^re-arec dehydrated nedia is stored in acod dry location. Each container will be dated u;:cn arrivaland upon opening. The records will show date of preparation,ty?e of medium, Irt number, sterilization time and temperatureal^o recorded en autoclave charts), final -oH and thetechnicians initials.Prey>curc-d plates v;ill be used within nne week (m-endo LE3platen are refripcrnted and used within 2 ve-skr).N»_/ -
c. Broths shall be ucon vithin oned. Standard Methods Agcr will be remclted (in flowing steam)
only or.c?. It will be held at h**-'-6c until it ic used forpouring. It will be held for no more than 3 hcurs at **-—^6C,
e. Membranco Filter Kcdin - H-Endc agnr LSS v.-ill have a final;p!! r,f 7.2 +/- 0.2. Direct heat is used for nrevnrption andonly pure ethanol Cpurchnscci from a Pa. Strte Store) is added.Th? -poured *;lntec are rtcrc- in a ti^rht covoreu container andrefritferntod (storage not to cxcocd 2 week;}.
f. 1-1PN Media - The modio i:: di(;-:en^od in voluncc rf not less then10ml per tube, they liavo l ose-:itt-ir.(- \-lt?stic closures nndarc stored at room temperature in a dark cabinet end ore usedwithin on« wc'.:k.
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QC IncGUAUTV coNinoi lAOOru.'tonY1?OS INDUSTRIAL HIGHWAY • PO. BOX 514 . SOUTHAMPTON. PA i SPGC-OI l l 4 - (?1 5) 30C'-3
After notifying tho '..-atr-r ru ^ vlirr by phone, of a viol~^ion, the?Q.C. re :rcrontst iv*' will next ivruo a ;-<-rtcnr:: notifying: the r.up-lierby moil. All OTT 'let oo anri initialed final roportr «"?.rc- nnxt senttn the -~cr:v.utor ro^ f^r entry i:v:<-. tho corrr-rter. After procethe computer gcnerntnc re' :'t i:-, sent ba'-k to thr Vice Presidentfor final revi-?-..-. At thir- tine = ~r'.''y ^- the result r- ir. sent toK.J. ^DP ^r. forn UAQC 02. l-'.rnthly, n" c^rr._-u4-er tr./c "file" cf allrari.?lc results ir, .v.er.t to Pn. DEP ir.rtcac! of ircuing re.->rrt frrmas with KJ DEF-
Part IV COPPXCTIVE ACTION
A. Contingency Flanr;
Thi " sect ion dor.l MT with t ho Inborn t ori cr ror^onsc- t c unc cce'.,1* nbloir.ctruner.t rer^or.cc and unnr c?":tr.'cle internal control chc-cks . Shouldany nf the ^roccodir.;:; occui-; t'.;c O^ality Accurr.ncc- Director i"notified ir.rr:ediat elv . T:"e C.A. Director immediately begins aninvert ig^-ti in. The first objective of thn invent igr-ticn is tc deterir.ir.ev:hcther cr not the circro^nr.cy h~,s a f feet eo custcrsor sarr/;le results .
If there is s,ny question about the accuracy of sample results, thetn^tinjr is ctop'-'ec: and tho naci^le results in ouectirri arc discarded.Sarn^les v.'hcso cnt a is discarccc v:ill be recchodul? d for resamlingand rerunning. If any 5F.ra:.'lcs ::reviounly reported are ir. question,the laboratory will notify the curt cnicr and nil a-:-ir"*?riat c -govern-mental agencies.
The next st e^ in tho i nvect i^at ion , should the ab^ve occur, is to de-termine specifically v/hat problem oc cured, determine hov? to correctit, and determine ho .- any nr obi err..? diocovered , can be prevented inthe future. Tho C.A. Director .it the tine of the incident willreoort the event to the Vicc-Precident . Once the pr'-blen has beencorrected and the Q.A. Dire^.tor i.^ certain that the er.tire rystemis bncl-: in control , r-on:.'lc tertinc i- rcruned f^llov;inc v/rit t en
from the Vice President and President .
The Q.A. Director will prepare a written report thr-t v;ill detail theevent. Thf: report will certain ar, rruch detail as possible describingthe time (datcc)of the event and the invest icat~- n that fc-llr.v.'t*-.The report vjill include all r-r-nruros taken to cct the system backum^er control nr veil a:-; any n^v: a •; rnachcs to prevent the omoleinin the future, This report will bo giver, to both tho Vi^c Presidentnnd Prcridont for their re'-'icv.'.
A water sample for bacteriological analysis must be taken in a laboratorysterilized bottle. Water samples for realty transactions, F H A or V Acertifications, U S Public Health or E P A approval, ahd food and beverage serviceto the public must be taken by laboratory personnel or a health officer. Samplesof streams, ponds sewage or industrials wastes also require special proceduresand equipment, as well as professional observations.
Water to be tested for potability must be collected in a sterilized container.Q C Inc. will supply you with the necessary containers. Sampling containerscan be picked up at the main office at 1205 Industrial Highway or arrangementscan be made to mail the containers to you.
Take the sarrnle from a faucet that is in regvular use, not from a hose or aseldom-used pipe. The tsp must be free of aerators, strainers, hose attachmentsand other water purification devices. .Flame the rim of the faucet with a torchor cigarette lighter for 15 seconds to destroy all external bactetia. Let the waterrun for five minutes, or severe! h-urs if there has been no recent use of the system.If the faucet is constructed of plastic, the sar-.ler should elisir^.te the flametreatment ste^ and only fluch the water system.A nev: or repaired veil should bedisinfected ar.d flushed out before sampling.
e the ca;; from the bottl- without touching the glass surfaces at the neck.Fill leaving a half-inch air space at the top.. Replace the cap tightly and placethe bottle in its jacket. Write identification p.p. the jacket label or or. the tag.Keep the sanr/lc refrigerated r.nd deliver to the Ip.b-vithin 3O hours.
If a fecal ctrc^ analysis ic requested it must bo delivered to the laboratorywithin 6 hours. If the tine cnnstrsintc ere not met, the sem.;le will be rejectedand a ressnr-.le requested.
All laboratory sterilized bottles contain thiosulfate, which neutralizes anyresidual chlorine that may have been in the water supply. If a system has beenhard chlorinated recently, it MUC7 be vumpec out cnourh tn elimirjctc- all trace ofchlorin* otherwise the analysis would be meaningless. An ortho-tolid ine or DPD testshould bo made to check for residual chlorine.
If a supply is regularly treated by a mechanical chlnrinator, there should be nresidual chlorine reading of 0,3 tn 0.6 nart.*? r^er million ot the time of talcingtho snm-ile. Th<; thin-vulfoto in thu bottle v:ill neutralise thi^ chlorine uponf.-ontact, .'.-nd bacteriological r::nlycif will chrw ihc condition of the water nt thetime of sDmj'.lir. . If treated ly on iouinator, thor3 chnuld be an iodine residualnf 0. ' to O.J>. A special iodine test kit is needed to rhrv-k for thir. condition.
AFEENDIM B
DIRECTIONS FOR TAKING A WATS?. SAISPLS ( crnt in
A laboratory sterilised bottle c^ntainr enruch water for all baanalyses:. A cc_>sr.ite battle rrrurt be provided if infonn^tirn on chemicalqualities if. desired, ^r if ;j^llutirn ic cun;:ecteri. That bcttle shnuld be-clean glaze cr r.laistic, nr^t 7,-rovinucly uced as a container. It need net besterile, but chruld be rinsed thoroughly v;ith the water being san^led, androust never have been in contact- with scavis or determents.
APPENDIX 3
-**INFORMATION TO ACCOMPANY A WATER SAMPIS
Write identification on the jacket label or on the tag. Fold this sheet andplace it inside the jacket. See other side for directions in taking a sample,for volume of water required and for testing supplies that were chlorinated.
SEND REPORT TO: Name
Address
Phone _
WATER SAMPLE OF: Name __
SEND COPEES TO:
Water sanple taken by ________________________ Date taken
Taken at: source ___ pump discharge ___ pressure tank ___ faucet
Supply: drilled well ___ dug well ___ spring ____ pond ___ stream
If a drilled well: year drilled ___ feet of casing ___ type of pump __
If a dug well: depth ___ type of pump ___ type of covering _________
Treatment after point where sample was taken ____________ ____
Was the supply hand-chlorinated recently? __• If so, was it thoroughly pumpedout and tested to make certain there was no residual chlorine? _________________
Type of analysis desired: bacteriological ______ domestic chemical _______other
(In the absence of specific instructions, the laboratory will provide analysesand recommendations relative to the background information provided above.)
111 Mrs; 1-smr.xLD.OTI FOR VAJUOIA
or POMTTVT A>T> NEOATTVIWHEN Frvi 10-uL foano** AJU
USED
No. ofTobaOfTI&l rOBIQVC
KJQMCOOB Out 01Sof IDmLEacb
01i345
MPNiBdu/100 mL
< r22.23.19.2
16.0> 16.0
93% Cooftdenc*Lumo
(AppnuinuLir)
Lowej Upper
0 6.00.1 1160.5 19.21.6 29.43.3 52.9S.O Infinite
APPENDIX C
Most Probable Number Indox and 95% Conf ldunco Limits for Five Tube, Three Di lu t ion Series (8.9)
No. of Tubes Giving} 'outlive H cue lion out of
s or 10ml Each
0000
11JJ1333333
3333333444444
5 uf 1ml Each
0012
00112
00I123
0011223001112
S of 0. 1nil l£ach
0100
01010
0J0100
0J01010010120
Miaa.Indexper
100 ml
<2224
244e6
S71e0
12
B1111M141717131717212022
B5^ ConfidenceLimits
Lover
<o.s<0.5<0 .5
< 0 . 5<0.5< O . S<0.i<O.S
<0.511223
12244Sb3!>S7u7
Upp«r
77
11
711111515
13171721212B
IB252531344G4C3I<.°46£378C7
No. of TuLtei GivingPoaUlvc Reaction out of
5 of 10ml Each
4444
AS&555
&5&fi5&555&555t55&5
5 of 1ml Ettct
2334
0001I12223333444445bb55i
5 of 0. 1rn] Ench
1010
012012
01201230123401
'234b
MPNTmjfx
per100 ml
2fi2T333<
233143334fl63
4D700470
110MO100130170220280350240350MOD 2 U
1000> 2400
057. ConfidenceLlmlti
Lower
D9
1112
71115111621
17232825313744354357BO
12060
120100300040
Upper
7880D363
7080
110S3
120150
1301702201BO250340500300400700B50
1, 000750
1. 0001, 4003.2005, BOO
APPENDIX B
Health and Safety Plan
•HEALTH AND SAFETY PLAN
CHROMATEX, INC.PHASE I - EXTENT OF GROUNDWATER CONTAMINATION STUDY
TABLE OF CONTENTS
PAGEA. INTRODUCTION 1B. RESPONSIBILITIES 1C. SPECIFIC POTENTIAL SITE HEALTH AND SAFETY HAZARDS 2D. SITE ACCESS RESTRICTIONS 8E. NOTIFICATION PROCEDURES 8
ATTACHMENTS* EMERGENCY PHONE NUMBERS 9* DIRECTIONS TO HOSPITAL 10* MAP TO HOSPITAL 11* LISTING OF HAZARDOUS MATERIALS / MSDS 12
Prepared By:
INTEX, Inc.Warminster, PA 1897k
215-598-7137
December 18, 1987
HASP-CRX-P1
HEALTH AND SAFETY PLAN
DRILLING, TESTING AND SAMPLING PROJECT
A. INTRODUCTION /fc '' V3* i ??/•/_:
It is the sole intent and purpose of this Health and Safety Plan (HASP) to
provide involved personnel with guidelines regarding some health and safety
issues for the DRILLING, TESTING AND SAMPLING PROJECT. This HASP is oriented
towards the protection of all project personnel and authorised visitors to the
project site. This document and the project specifications should be consulted
for guidance in preventing, and quickly abating, any threat to human safety or
the environment. Resonable precautions will be taken to prevent unauthorized
access to the project work site. The provisions of the HASP do not replace or
supersede any regulatory requirements of USEPA, PADER, OSHA, NIOSH. or any
other regulatory body.
B. RESPONSIBILITIES
This Health and Safety Plan presents proposed guidelines to minimize the
risk of injury to on-site authorized personnel and to provide rapid response in
the event of injury. The provisions of this Health and Safety Plan shall be
implemented by INTEX's Project Supervision for the duration of this project.
The Client may instruct INTEX's Project Supervision to improve or modify health
and safety measures at the project site.
HASP-CRX-P2
C. SPECIFIC POTENTIAL SITE HEALTH AND SAFETY HAZARDS G <
The following list contains some potential health and safety hazards
expected to be encountered at the project site and some actions to be
implemented by the involved personnel to minimize the associated risk to health
and safety. This is not intended to be a complete listing of any and all
potential health and safety hazards, and it should not be interpreted as such.
The suggested actions to be taken under this HASP are not to be substituted for
good judgement on the part of the involved personnel and INTEX's Project
Supervision.
(1) Head and Body Injury
Potential Hazard
* Due to the need for well drilling, lifting, materials handling and
other construction equipment at the project site, head and body
injuries are possible due to falling objects or related causes.
Protective Action
* All persons on-site will be required to wear hard hats at all times.
(2) Injury due to Falls
Potential Hazard
* Slippery ground and uneven terrain are potential sources of injury due
to falls.
Protective Action
* All persons on-site will be required to wear appropriate foot apparel
for construction site activities which, at a minimum, will include
leather boots with tread soles or equivalent.
HASP-CRX-P3
* All persons on-site will be cautioned by INTEX's Project Supervision •
to avoid approching openings and excavated areas.
(3) Injury due to Fire or Explosion
Potential Hazard
* Injury could be caused by open burning, flammable liquids explosions
or fires, or unexpected disruption of above- or underground utility
lines.
Protective Actions
* INTEX's Project Supervision will provide and properly maintain at
least one 20-pound ABC fire extinguisher on site at all times such
that they are readily obtainable if needed.
* Open burning is strictly prohibited.
* Smoking is strictly prohibited at all times by persons within the
designated project areas.
* All liquids with a flash point of 1^0 F or below shall be confined to
UL and DOT approved safety containers. INTEX's Project Supervision
shall provide NO SMOKING signs where flammable liquids are stored.
* INTEX's Project Supervision shall remove from the project site litter
and debris at least once per day and more often if the debris presents
a fire hazard.
(i*) Injury due to Dust Inhalation
Potential Hazard
* Dust particles may produce irritation, or other injuries, during
certain weather conditions and tank cleaning activities.
HASP-CRX-P^t
Protective Actions
Should conditions become such that dust is a problem in the judgmtmigw.
of INTEX's Project Supervision shall spray the dust producing areas
with water only as necessary to eliminate the dust problem to the
satisfaction of the Client or require involved personnel to wear dust
filtration repirators.
* All project personnel working in dusty areas shall wear appropriate
dust masks. Goggles or safety glasses with sideshields will be
protective eye equipment to be provided for all involved personnel.
(5) Injury due to Organic Vapors
Potential Hazard
* Organic vapors are not expected to be encountered at levels
anticipated to present hazards to on-site personnel should the safety
precautions described herein be followed.
Protective Actions
* If a release of organic vapors is suspected or detected, INTEX's
Project Supervision will conduct an investigation while using Level C
protection (full- or half-face respirator with organic chemical
cartridge, tyvek suit and gloves). The investigation should be
conducted with a photo-ionization detector (h-nu) to confirm vapor
levels in the work area.
HASP-CfcX-Pf;
An area of approximately a 20 foot radius from the well itself will be
designated as the work site. This entire area will be periodically
monitored by the site geologist using the h-nu. Monitoring will be
concentrated at head level at a distance of 4 to 6 feet from the well
itself. If vapor levels in excess of 20 ppm are detected in this
space, drilling will be halted and all personell will be retreat from
the site to equip themselves with half-face resporators with organic
vapor cartridges, tyveck suits and gloves. Drilling will commence
when all personell are properly equipped. The site supervisor will
not allow any person onto the work site without proper apparell for
the existing situation. Proper saftey attire for site workers will be
kept in the cab of the drilling truck.
HASF-CRX-P6
( 6 ) In jury due to Weather Exposure
Potential Hazard
* The work site is open and workers will be exposed to the weather.
Since work operations will occur during winter months, there is a
potential for frostbite, hypothermia, or other cold weather exposure
related injuries.
Protective Actions
* INTEX's Project Supervision will be responsible for insuring that
workers are properly clothed for the weather conditions.
* Heated buildings are located a short distance from the work site, and
access will be provided by the Client.
* If weather conditions become such that worker safety is questionable
in the judgment of INTEX's Project Supervision and/or the Client, then
work will cease until safe weather conditions return. In judging the
weather condition, INTEX's Project Supervision will consider such
factors as temperature, wind chill factor, worker exposure to drilling
and decontamination water, precipitation, wind velocity, and any other
appropriate weather factors.
(7) Injury from Contaminated Groundwater, Soil and Rock Cuttings
Potential Hazard
* Drill wastes generated during work operations may contain materials
which could cause dermal reactions or injury to mucous membranes if
directly exposed.
HASP-CRX-P7
Protective Actions
* INTEX's Project Supervision will make sure that all persons
protective goggles and/or safety glasses with splash shields and
chemical resistant gloves during any wastewater handling operations in
addition to protective clothing such as boots, coveralls, chemical
resistant coveralls, and long sleeved shirt or acid resistant apparel,
as required.
* Eye-wash kits will be provided and properly maintained on-site by
INTEX's Project Supervision.
(8) Other Health and Safety Issues
INTEX's Project Supervision will be responsible for providing and properly
maintaining adequate first-aid equipment on-site to treat minor injuries.
Furthermore, INTEX's Project Supervision will be responsible for arranging
transportation of any injured authorized on-site person to medical
facilities should more serious injury occur. INTEX's Project Supervision
will be responsible for providing administration of first-aid.
HASP-CRX-P8
D. SITE ACCESS RESTRICTIONS
~~ Access to the project work site will be limited to authorized personnel
including INTEX, Inc., Subcontractors, Client personnel, and authorized
visitors. The Client shall be responsible for authorizing all visitors. All
^_ visitors must coordinate with INTEX's Project Supervision prior to project site
entry. INTEX's Project Supervision shall ensure that all visitors abide by the
— provisions of the Health and Safety Plan. The Client will, if able, accompany
all authorized visitors while they are on the site. Should the Client be<»_-
unable to accompany an authorized site visitor, the Client will inform INTEX's
Project Supervision and INTEX's Project Supervision will accompany the site
visitor or inform the visitor that the visitor shall not enter the project site
"*- until an accompanying party can be provided.
*" E. NOTIFICATION PROCEDURES
In the event of incident or injury, INTEX's Project Supervision will notify*umthe Client Project Supervision who will then notify the facility Security
— and/or First Aid office, unless in the judgment of INTEX's Project Supervision,
^_^ there is clear reason to do otherwise to protect health and safety.w
Emergency phone numbers are provided as an Attachment to this HASP.>—However, additional parties may be contacted if there is clear reason to do so
_ to protect health and safety. Directions and a map to the nearest Hospital are
provided as an Attachment to this HASP.
EMERGENCY PHONE NUMBERS
KASP-CRX-P9
ATTACHMENT
SJTE EMERGENCY SERVICES_________
Police Dept. West HazletonState Police
Fire Department/AmbulanceSt Joseph Hospital Main
EmergencyChromatex Doctor, Dr. Eugene StishPADERUSEPA HOTLINEPA)
INTEX EMERGENCY COORDINATORS
Primary Coordinator:
*
**
Joseph Jacobsen - President.Horsham, PAJohn Walker - V.P...........Doylestown, PA
* Julie Vann - Site Geologists..........West Chester, PA
** Richard Oki - Alternate Site GeologistWillingboro, NJ
.HOME:
HOME:
(215) 436-8125
(609) 877-2371
HASP-CRX-P10
ATTACHMENT"7^
DIRECTIONS TO ST. JOSEPH'S HOSPITALFROM PLANT 2
TURN RIGHT EXITING FROM PLANT 2 (JAYCEE DRIVE)
BEAR RIGHT AT TRIANGLE (DEER RUN ROAD)
CONTINUE ON DEER RUN ROAD TO STOP SIGN (INTERSECTION RT 93) TURNRIGHT AND PROCEED SOUTH TOWARDS WEST HAZLETON FOR APPROX. 1.25MILES
TURN LEFT ONTO 15TH STREET AT TRAFFIC LIGHT IMMEDIATELEY AFTERPASSING BURGER KING
CONTINUE EAST ON 15TH STREET APPROX. 2 MILES TO INTERSECTION OFRT. 309 (TRAFFIC LIGHT)
TURN SOUTH AND PROCEED UP HILL (7 BLOCKS)
TURN LEFT IN FRONT OF ST. JOSEPH'S MEDICAL CENTER (8TH STREET)
WATCH FOR SIGN ON LEFT
EMERGENCY ENTRANCE IS IN ALLEY BEHIND HOSPITAL WATCH FOREMERGENCY ENTRANCE SIGN.
HASF'-CRX-Pll
ATTACHMENT
MAP TO ST. JOSEPH'S HOSPITAL
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7 A STATS VSV-2&1O
ATTACHMENT
LISTING OF HAZARDOUS MATERIALSHSDS « MATERIAL SAFETY DATA SHEETS
The following listing indicates the hazardous materials that will behandled at the project site. Additions and deletions of hazardous materialswill be coordinated by INTEX's Project Supervision. The foregoing list isclassified by compatibility groups inorder to reinforce that handling, storageand safety procedures should generally the same within the same group.Material Safety Data Sheets (MSDS) for hazardous materials will be available atINTEX Field Office.
Floata on •**- Flammafiia. mttang vapor « produMd.
Slop dracnarg* * paaima. Kaw PMPW •*•*.Snirl on qman tomvi and can lira oapanmanlSUy uD«nd and ua* want way M "«WC« Oowi" vtpor.larxala and rvnov* diacMrgM malarial.NoMy kx* n*am ano poNuHon osrffol *g«iOH
Fire
Exposure
WaterPollution
FLAMMABLE.FlaafiMcK along, vtpor nt mo|> ooax.Vapor mat aivuo* t igraMd n an an elan a araaiEnmgwO «•*• *V enanneal. to*". or caroon OcmO**alar may M pnanottva on In.Coot aipoaod contavwi vtm «*Mr.
CALL FOB MEDICAL AiO.
VAPONirnuang to vya*. ROM end mm.ii innaMd. <rtt cau** ottanma. naaoacna. (Mftcun tx«uv"j
or KM* ol oonaoouanaaa.Wov* 10 fr«*n Ifn oroamng naa HoooM. 9~« arWoai 'iuwiuonii tx»itr»ng * armcun on* twyaanLKXHOimta»ng la Mm an) ayaa,It HMEOnaa. nMfccuM rmaj«a. v vomrano,S«mov« oontaminaiM cxMNnq ana txj*iciutn ait*eiad V*M wnn p««ntir c< -il*r
.F SWALLOWED ana ••ew •« CCSSCOUS
3f mut3O SOT iMDOCE vaw.T'NG
HABMFUL TO AQUATIC LIFE IN VEBY LOW CONCENTRATIONS
I. RESPONSE TO OrSCKAKE
IMU* •Hmog-n«X1 "wrvnibiMrEvKulM MM
UX] flutfl
1. CHEMICAL DESICCATIONSCO CompcUMWr OMC Mue«««r«om
Hyarocwoon Manuf*«formutf |Mmn of rryOrocwtarn]IMO/UN DMtgMMon 11/1203DOT ID Ma^ 1203CAS t*gMtr¥ Mo^ D*U no)
1 LABELLI CftfQarr- FI*mmioM WMd
4. OBSERVABLE CHARACTERISTICS
SUM (HCoMr Cdortni 10 Crown
HEALTH HAZARDS
Symptom* Following ExaoHn: Vnubon of "xxou* nwnbfWM* uM lUnuinon fo*ow«0 6yo*pr*uan a* cwww rwrvou* «r»t*m SrHDwg of vipor nwy MO CIUM aa&rwu. n«M*cn«.mo ncoorOiUDon o>, in mot* iwcri rim vmihMHi. comi. tna r«o«»Mxy vrnt If Mud•nl«rt king*, ii wilt UUM Mv*n muaon. cougnxg. B*OD(ig. punwwf dMnu. »"J- lii*r.ugra of broncnoMWJinoni •"> CnoumontM. Snnlow^g mtr UUM T*«JU'* nwvtDMt.
TrMMMM of Eipown: INHALADOrt: muniMi nnntan ana Mffwniw oi fgvn: «nforc« Mdrru H MJIH] 4 « lung*. 1NOESTTON- oo NOT mdua vonntng; womccn tfwuM b* ln*gM (byooctoi) if iptKvcutiM auwwiir i twoiowM. EYES. *un wnn cooout ouacMy of w*i*r. SKIN:<np« off and oun untt *ow> and wow.
TVMfM4d LVM Value 300 ppmShort T»rm InMMtofl UMta: 300 ppm for M imToUcltr By lnfl*aBon: GrtO* Z: LD.. . O.S » S g/Hg.LJI* ToiMtty: Non*Va«or (CM) trfttfni CrMnctwMttGK Vapon caua* a MgW imatmg of tr* *T" or rMpratory
lyiUfn if 0r*MM in rign conocnomiont. Th* «rtaa * iwnoorary.UOUM) or SMM IrniaiM CfivacterMUcc Mmrnum nuard. If «**1 on cloifwig am >ikw«o 10
nmwi. FTWT c*** vnarang and ifOOffn) ol <M nun.Odor TTirMnaM 0 24 ppmIOUH Valu*: Data not «vnl«j4«
PlaMi Patnfe —M'F C.CUMM In Am 1 4%-7 4*
ng Aaiintai Fovn. ewtran
i.4 Fir. f xttngutoMng Ao*nM Hot Hi M
M •linear IB *Mc Vapor * tMavw ih*nand may nv«l oomidvMM iMunc*
of ignMn aM «aan bacK.: »S3'F
M Da«MoM Mvur« Oa« I. Crouo D
ltd laiibmc Flam* Tin+ntur*Dale no) avaMoM
(.11 Ha4eh>oin«li'M Air to Futf Matta:DM not ivaiIMM
1.11 Hano T«np«nrlur«: 0*ta not
7. CHEMICAL REACTIVITY
7.1 Baatflrtty WWi WIMR Na raacnon7 J HucHYity urttfi Commoo MMartMv Mo
r*acnon7J at**l»t| Ounn« rranaaore SIMM7.4 NMrtraNMng AoMiM for Aefcta aM
CauBUCK NOI portrwnt
J.t InrHMIor of Pofynwluaon;
7.7 l«ola> IU«)e (R**ctant loPraducf£ Out not avaiicox
nil or (pron loi Wun p(pi»ct>oor•nd tte. innofifitn* i
U iymptom* FoDowttig lipto tot* of conuowwM: Ngh cofle*ntoition nn t» '*'•! * * lo tvr&f
nrnbkwd mm tow ol oorHoouwWH MGESTION. produc*1 flfKtl timlw tomn.i*tion ind miff emit* torn* iMtng ol mm»« EYES iNo»th> (rrniting «nd Iw^vvmciorySKIN dotinna KIton rr»y cawM d«nwMI*
Tr*«m»nt of CipOoun: Q*» m#dk*C ilMnton for M "Y* «-jxnw« tn] >><i otrn »fxxi» ov*-•ipotu*! Oo MOT Ktmortt* i»ir«»n or »<*» *>*i>. oltwM*.. bf*v-*ir* M (ymptornthcHWALATKM' Finny, vtetm u tinh MIL * n»cMMrf, M>Phr i»fic«i rvw 'ilK" *n)/or