WQ0002702_Regional Office Historical File Pre 2018 (20)

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5474
Mr. Wayne Drye
ALCHEM, Inc.
8135 Red Road
Rockwell, NC 28138-
Michael F Easley, Governor
William G Ross Jr., Secretary
North Carolina Department of Environment and Natural Resources
May 17, 2006
SUBJECT: Initial Wastewater/Groundwater Laboratory Certification
FIELD PARAMETERS ONLY
Dear Mr. Drye:
.Alan W Klimek, P E Director
Division of Water Quality
The Department of Environment and Natural Resources, in accordance with the provisions of NC GS 143-
215.3(a) (10), 15 NCAC 2H .0800, is pleased to certify your laboratory to perform specified environmental
analysis required by EMC monitoring and reporting regulations 15 NCAC 2B .0500 and 2H .0900 and 2L
.0100, .0200, ,0300, and 2N .0100 through .0800.
A certificate acknowledging the certification of your laboratory is enclosed for your use. The certificate
describes the requirements and limits of your certification. Please review this certificate to insure that _your
laboratory is certified for all parameters required to properly meet your certification needs..
Please contact us at 919-733-3908 if you have questions or need additional information.
Sincerely,
?James W, Meyer
boratory Section
Enclosure
cc: Chet Whiting
No ° Car
Atra'u
Laboratory Section 1623 Mail Service Ccnter, Raleigh, NC 27699-1623
4405 Reedy Creek Road; Raleigh, NC 27607
Phone [phone] / FAX [phone] / Internet www.dwglab.org
An Equal Opportunity/Affirmative Action Employer- 50% Recycled/10% Post Consumer Paper

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4
STATE OF NORTH CAROLINA DEPARTMENT OF THE
ENVIRONMENT AND NATURAL RESOURCES
DIVISION OF WATER QUALITY
LABORATORY CERTIFICATION PROGRAM
In accordance with the provisions of N.C.G.S. 143-215.3 (a) (1), 143-215.3 (a)(10) and NCAC 2H.0800.
Field Parameter Only
Mry za t7yr O
r
t� -IPRmI rm-
QUAM
•
ALCHEM, INC.
Is hereby certified to perform environmental analysis as listed on Attachment I and report monitoring data to DWQ for
compliance with NPDES effluent, surface water, groundwater, and pretreatment regulations.
By reference 15A NCAC 2H .0800 is made a part of this certificate.
This certificate does not guarantee validity of data generated, but indicates the methodology, equipment, quality control procedures,
records, and proficiency of the laboratory have been examined and found to be acceptable.
This certificate shall be valid until December 31, 2006
Certificate No. 5474
r�rrn.Q-1LG'C.�
James W. Meyer
i

Lab Name: ALCHEM, Inc.
Address: 8135 Red Road
Rockwell, NC 28138-
Attachment
North Carolina Wastewater/Groundwater Laboratory Certification
Certified Parameters Listing
FIELD PARAMETERS ONLY
Certificate Number:
5474
Effective Date:
05/17/2006
Expiration Date:
12/31/2006
Date of Last Amendment:
05/17/2006
The above named laboratory, having duly met the requirements of 15A NCAC 2H Oe00, Is hereby certified for the measurement of the parameters listed below
CERTIFIED PARAMETERS
INORGANICS
PH
Std Method 4500 H B
This certification requires maintance of an acceptable quality assurance program, use of approved methodology, and satisfactory performance on evaluation samples Laboratories are
subject to civil penalties andlor decertification for Infractions as set forth In 15A NCAC 2H 0807.

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
Laboratory Name:
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor:
Date Received:
Date Forwarded to Alberta:
Date Mailed:
5474
ALCHEM
Maintenance
Chet Whiting
October 14, 2008
November 3. 2008
November 3, 2008
Insp. Initial X Insp. Reg. _ Insp. No Finding _ Insp. CP
Gary Francies

LABORATORY NAME:
CERTIFICATE #:
ADDRESS:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
INTRODUCTION:
On -Site Inspection Report
ALCHEM, Inc
5474
8135 Red Road Rockwell N.C. 28138
October 14, 2008
Maintenance
Chet Whiting
Robert Wolcott
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
II. GENERAL COMMENTS:
The laboratory has had significant changes in overall management and personnel. As a result a good
deal of documentation was lost in the transition. Also previous management had not responded to the
prior inspection report. The physical state of the analytical lab was much improved especially the overall
cleanliness of the work area. Of serious concern was the overall lack of documentation. In this area the
lab has regressed rather than improved. A sampling event was observed from sample collection through
analysis. Supporting information for the analysis was documented on an envelope that was not retained.
The lack of supporting records renders such data indefensible. A follow up inspection will be conducted to
verify that the requirements specifed in this report are implemented.
Please be advised that a laboratory may be decertified for failing to respond to an inspection report.
Recommendation: A copy of the laboratory certification rules were given to personnel at the time the
time of the inspection. It is recommended that these be carefully reviewed and that this office be
contacted should there be any questions.
Recommendation: A copy of Technical Assistance for the Field. Analysis of pH was also given to
personnel at the time of the inspection. We also recommend that it be carefully reviewed.
Recommendation: Personnel were also advised that the certification web site at (dwqlab.org) was a
valuable informational asset and should be periodically reviewed for new and/or updated technical
assistance.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
A. Finding: The laboratory has not submitted an application amendment updating changes in
management and analytical personnel.

Page 2
Requirement: The laboratory must submit an application amendment no later then 30 day from
receipt of this. report. Ref: 15 A NCAC 2H .0807 (a) (11)
Comment: A copy of this document was given to personnel at the time of the inspection.
pH.. Standard Methods 4500 H+B
B. Finding: Supporting record for collection and analysis of compliance samples are not maintained.
Requirement: Data pertinent to each analysis must be maintained for five years. Certified Data
must consist of date collected, time collected, sample site, sample collector, and sample
analysis time. The field benchsheets must provide a space for the signature or initials of the
analyst, and proper units of measure for all analyses. A record of instrument calibration where
applicable, must be filed in an orderly manner so as to be readily available for inspection upon
request.
Comment: An example sheet was custom made for the facility at the last inspection. This was
provided as technical assistance for guidance as to general requirements for field analysis. This
document could have been copied and used for analytical documentation (that option was
discussed during the previous inspection). The example document meets the current requirements
for filed testing for pH.
C. Finding: The Automatic Temperature Compensator (ATC) has not been verified annually (due
March 2008).
Requirement: The ATC must be verified annually (i.e., every twelve months) by analyzing a
buffer at 25' C (the temperature that pH values are compensated to) and a temperature(s) that
bracket the temperature ranges of the samples to be analyzed. This may require the analysis of
a third temperature reading that is > 25' C. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) Policy Statement 09/2007.
D. Finding: The temperature sensing device on the pH meter has not been calibrated against an
NIST certified or traceable thermometer annually (every 12 months).
Requirement: All temperature sensing devices on meters must be calibrated against a NIST
certified or NIST traceable thermometer annually (every 12 months) and proper corrections
made and documented. The meter reading must be less than 1°C from the NIST certified
reading to be acceptable. Document the serial number and manufacturer of the MIST
thermometer that was used in the comparison. Document any correction that applies (even if
zero) on both the meter and on a separate sheet to be filed. Ref: Ref: Technical Assistance for
Field Analysis of pH, Rev. 10/2008
Comment: The sensor check was due in March 2008.
pH: EPA SW-846 Edition 9045 D
Comment: There appeared to be some confusion among staff as to the nature of samples matrices
analyzed. The sample collection observed was liquid. Analytical personnel stated that on occasion
samples consisting mostly of sand were collected. According to analytical personnel these samples
were analyzed correctly. A copy of the method was on -site. The laboratory is not currently certified for
SW-846 9045 D and must obtain certification for the analysis of solid samples.

Page 3
Recommendation: It was recommended that a request for 9045 D certification be added to the
certification amendment that must be submitted to update personnel records. There is currently no
charge for the addition.
Recommendation: The laboratory had not ordered a performance evaluation sample at the time of the
inspection. It was recommended that a "quick turn around" type sample be ordered immediately. The
laboratory was directed to our web site for a list of vendors.
IV. PAPER TRAIL INVESTIGATION:
No paper trail was conducted.
V. CONCLUSIONS:
Correcting the above -cited findings and implementing the recommendations will help this lab to
produce quality data and meet certification requirements. The inspector would like to thank the staff for
its assistance during the inspection and data review process. Please respond to all findings.
Report prepared by: Date:
Report reviewed by: Date:

Technical Assistance
Automatic Temperature Compensator (ATC) Check Procedure for pH meter:
The following must be performed on an annual (i.e., 12 month) basis:
1. Pour an adequate amount of buffer into a beaker or other container and analyze at 25° C.
Document the temperature and pH value.
2. Lower the temperature of the buffer by placing the container in cool water or a refrigerator
to less than the lowest anticipated sample temperature and analyze. Document the
temperature and pH value.
3. If samples greater than 250 C are to be analyzed, perform the following additional step:
Place the container in warm water, or a water bath and raise the temperature above 250 C
to greater than the highest anticipated sample temperature and analyze. Document the
temperature and pH value.
As the temperature increases or decreases, the value of the buffer must be within ± 0.1 S.U. of
the true value of the buffer.
Comment: Anticipated temperatures can be obtained from a review of the Discharge Monitoring
Reports (DMRs) from the peak summer and winter months. Historical data should provide a
reasonably accurate estimation of ranges that will bracket the expected sample temperatures.

On -Site Inspection Report
LABORATORY NAME:.
ADDRESS:
CERTIFICATE NO:
DATE OF INSPECTION:
TYPE OF INSPECTION:
EVALUATOR:
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
ALCHEM
8135 Red Road, Rockwell NC 28138
None
February 20, 2007
Initial
Chet Whiting
Mr. Wayne.Drye
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H
.0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
The facility needs to improve documentation. A copy of an example field sheet was sent with
initial certification materials that also included the program rules. An example field sheet specific
to the types of items needed was given to the facility on February 21, 2007. Please be reminded
of the importance of properly documenting information related to compliance testing. Proper
documentation validates that required methods and procedures were followed. Without this
documentation the validity of testing is in doubt. Further proper documentation is a condition of
field parameter certification. Also pH by method 9045 C must be requested. Procedures are on -
site. An application amendment was sent under separate cover.
III. DEFICIENCIES, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
C;FNFRAI
A. COMMENT (new policy): Verification of the temperature compensator function was not
performed/documented.
REQUIREMENT: Check and document the meter ATC function annually (every 12 months).
(NCLC Policy)
This may be accomplished as follows:
1) Pour an adequate amount of buffer into a beaker or other container and analyze at 250 C.
2) Raise or lower the temperature of the buffer by:
a) Placing the container in warm water or a water bath to raise .the temperature
(anticipated highest sample temperature), then analyze.
b) Placing the container in cool water or a refrigerator to lower the temperature
(lowest anticipated sample temperature) and analyze.

V Belmont Textile Machinery Field Lab. Inspection Page 2
There should not be a significant difference in the readings if the temperature compensation
devices are working properly. The buffer must read within ± 0.1 pH units of the true value of the
buffer.
B. COMMENT (new policy): The temperature at which pH is measured is not documented.
REQUIREMENT: Document the temperature at which the pH sample(s) are analyzed. Ref: EPA
150.1-4.4, Standard Methods 18th Edition Method 4500H+ B.1b.
1 DEFICIENCY: The annual temperature check of laboratory thermometers vs. an
NIST Traceable Thermometer/thermocouple was not documented for the following
for: pH meter .
REQUIREMENT: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked against an NIST traceable thermometer and
proper corrections made. Check laboratory thermometers vs. an NIST thermometer and post
any required corrections. Ref: 15A NCAC 2H .0805 (a) (7) (0)
2 DEFICIENCY: Required supporting information not documented (Analysts name
or initials, units of measure, analysis time).
REQUIREMENT: Document Analysts name or initials, units of measure, analysis time on work
sheets. 15 A NCAC (a) (8) (g) (1)
C. COMMENT: expired reagent: pH 10 buffer 3/2006
NOTE: The pH 7 Buffer expires in March of this year.
REQUIREMENT: Replace this reagent immediately. Ref: 15 A NCAC (a) (8) (g) (4)
3 DEFICIENCY: The pH calibration log could not be located at the time of the
inspection.
REQUIREMENT: Instrument calibration documents must be available for review upon request.
15 A NCAC (a) (8) (g) (2)
IV. PAPER TRAIL INVESTIGATION:
A general documentation review was conducted.
V. CONCLUSIONS:
Correcting the above -cited comments and implementing the recommendations will help this
lab to produce quality data and. meet certification, requirements. Please respond to all
numbered deficiencies lettered comments.
Report prepared by: Chet Whiting Date: February 21, 2007

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
5474
Laboratory Name:
ALCHEM
Inspector Name:
Chet Whiting
Inspection Date:
February 20, 2007
Date Report Completed:
February 21, 2007
Reviewed by:
Date Reviewed:
Manager:
Date Received:
Date Mailed:
cc: Section Chief (Routing Sheet only)
INSP-RTE.DOC
5221

• oF w A 7-
7
O 'S
January 26, 2006
Mr. Wayne Drye
ALCHEM
8135 Red Road
Rockwell, NC 28138
SUBJECT: Initial Laboratory Certification Inspection
Dear Drye:
Michael P Easley, Governor
William G Ross Jr., Secretary
Norili Carolina Department of Environment and Natural Resources
Alan W Klimek, P E Director
Division of Water Quality
Enclosed is a report for the inspection performed on January 13, 2006 by Mr. Chet Whiting.
Where deficiencies are cited in this report, a response is required as well as for all lettered comments
and/or recommendations. Within 30 days of receipt, please supply this office with a written item for
item description of how these deficiencies, comments and/or recommendations were corrected. For
certification maintenance, your laboratory must continue to carry out the requirements set forth in 15A
NCAC 2H .0800.
Copies of the checklists completed during the inspection may be requested from this office.
Thank you for your cooperation during the inspection. If you wish to obtain an electronic copy of this
report by email, or if you have questions or need additional information please contact us at 919-733-
3908.
Sincerely,
IrJames W. Meyer
Laboratory Section
Enclosure
cc: Chet Whiting
Mooresville Regional Office
No di Carolina
,Na1 l -a11!f
Laboratory Section 1623 Mail Service Center, Raleigh, NC 27699-1623
4,105 Reedy Creek Road; Raleigh, NC 27607
Plionc [phone] / FAX [phone] / Inlemel: www dwglab org
An Equal Opporfunily/Aff rmative Action Employer— 50% Recycled/10% Post Consumer Paper

On -Site Inspection Report
LABORATORY NAME:
ADDRESS:
CERTIFICATE NO:
DATE OF INSPECTION:
TYPE OF INSPECTION:
EVALUATOR:
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
ALCHEM
8135 Red Road, Rockwell NC 28138
None
January 13, 2006
Initial
Chet Whiting, Ellen Huffman (DWQ)
Mr. Wayne Drye
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H
.0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
This is the facility's initial on -site inspection in preparation for Wastewater Field Parameter
Certification related to the facilities Land Application Permit. A number of items need to be
addressed in order to meet certification requirements. Since this was only an initial visit the
laboratory needs to start the process by submitting an application to this unit. These items will be
provided under separate cover. Also a technical assistance document and a copy of the
Laboratory certification rules will be provided. Please review these items and contact us for
assistance if you have any questions. There may be specifics as to documentation where our
assistance would be useful. The facility has a copy of SW-846 Method 9045 on sire. Mr. Drye's
cooperation was greatly appreciated.
DEFICIENCIES REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
GENERAL:
A. COMMENT: The calibration range for the pH meter does not bracket the sample range.
REQUIREMENT: The meter is calibrated with pH 4, 7, and 10 buffers however it is very likely
that reported values will be below pH 4 and seldom exceed pH 7. This was verified by on -site
testing. The facility has a pH 2 buffer on site and will simply need to change the calibration
range to 2, 4, and T.
COMMENT: The facility will need a worksheet document that records all items related to
compliance testing.. This will include the time the meter is calibrated, the calibration buffers,
the check buffer result, analyst initials, analytical results, time and data of testing and location
for the sample. We have a series of generic forms that may prove suitable and useful and
would be happy to provide examples upon request.

_ aV: PAPER TRAIL INVESTIGATION:
-t•
Since this was an initial review a paper trail was not conducted at this time.
V. CONCLUSIONS:
Correcting the above -cited comments and implementing the recommendations will help this
lab to produce quality data and meet certification requirements. Please respond to all
lettered comments.
Report prepared by: Chet Whiting Date: January 26, 2006

0
NCDENR
North Carolina Department of
Environment and Natural Resources
FAX Mooresville Regional Office
919 North Main Street
Mooresville, North Carolina 28115
Phone; 704/663-1699
Fax; 704/663-6040
Date:/-023— e►-2
i o:
ax Number 70 /,2%q- 4 �( 1
Messaae: 417c,� C/,, a-- &,.; ,
rom: -fli, .��
Div/sectiom. , ) Q
Number of pages (Incl. cvr) -I-)

i
CONTACT SHEET
Lab Contact Sheet pgl
LAB#
LAB NAME
Contact
Phone
012
1
Pace
Mavis Jones
704-875-9092
020
2
PAR Labs
Chris Tita
704-588-8333
365
26
AquaSource
Samantha Austin
704-788-9497
402
27
Prism Labs
Helmuth Janssen
704-529-6364
559
39
K & W Labs
Gosia Graska
704-569-1800
440
29
Statesville Analytical
Dena Myers
704-872-4697

METHOD 9040E
off ELECTROMETRIC MEASUREMENT
1.0 SCOPE AND APPLICATION
1.1 Method 9040 is used to measure the pH of aqueous wastes and those
multiphase wastes where the aqueous phase constitutes at least 20% of the total
volume of the waste.
1.2 The corrosivity of concentrated acids and bases, or of concentrated
acids and bases mixed with inert substances, cannot be measured. The pH
measurement requires some water content.
2.0 SUMMARY
2.1 The pH of the sample is determined electrometrically using either
a glass electrode in combination with a reference potential or a combination
electrode. The measuring device is calibrated using a series of standard
solutions of known pH.
3.0 INTERFERENCES
3.1 The glass electrode, in general, is not subject to solution
interferences from color, turbidity, colloidal matter, oxidants, reductants, or
moderate (<O.1 molar solution) salinity.
3.2 Sodium error at pH levels >10 can be reduced or eliminated by using
a low -sodium -error electrode.
3.3 Coatings of oily material or particulate matter can impair
electrode response. These coatings can usually be removed by gentle wiping or
detergent washing, followed by rinsing with distilled water. An additional
treatment with hydrochloric acid (1:10) may be necessary to remove any remaining
film.
3.4 Temperature effects on the electrometric determination of pH arise
from two sources. The first is caused by the change in electrode output at
various temperatures. This interference should be controlled with instruments
having temperature compensation or by calibrating the electrode -instrument system
at the temperature of the samples. The second source of temperature effects is
the change of pH due to changes in the sample as the temperature changes. This
error is sample -dependent; and cannot be controlled. It should, therefore, be
noted by reporting both the pH and temperature at the time of analysis.
4.0 APPARATUS AND MATERIALS
4.1 pH meter: Laboratory or field model. Many instruments are commer-
cially available with various specifications and optional equipment.
4.2 Glass electrode.
CD-ROM 9040B - 1 Revision 2
January 1995

4.3 Reference electrode: A silver -silver chloride or other reference
electrode of constant potential may be used.
NOTE: Combination electrodes incorporating both measuring and
referenced functions are convenient to use and are available with
solid, gel -type filling materials that require minimal maintenance.
4.4 Magnetic stirrer and Teflon -coated stirring bar.
4.5 Thermometer and/or temperature sensor for automatic compensation.
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless
otherwise indicated, it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the American Chemical
Society, where such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Primary standard buffer salts are available from the National
Institute of Standards and Technology (NIST) and should be used in situations
where extreme accuracy is necessary. Preparation of reference solutions from
these salts requires some special precautions and handling, such as low -
conductivity dilution water, drying ovens, and carbon -dioxide -free purge gas.
These solutions should be replaced at least once each month.
5.3 Secondary standard buffers may be prepared from NIST salts or
purchased as solutions from commercial vendors. These commercially available
solutions have been validated by comparison with NIST standards and are
recommended for routine use.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1 All samples must be collected using a sampling plan that addresses
the considerations discussed in Chapter Nine of this manual.
6.2 Samples should be analyzed as soon as possible.
7.0 PROCEDURE
7.1 Calibration:
7.1.1 Because of the wide variety of pH meters and accessories,
detailed operating procedures cannot be incorporated into this method.
Each analyst must be acquainted with the operation of each system and
familiar with all instrument functions. Special attention to care of the
electrodes is recommended.
7.1.2 Each instrument/electrode system must be calibrated at a
minimum of two points that bracket the expected pH of the samples and are
approximately three pH units or more apart. (For corrosivity characteri-
zation, the calibration of the pH meter should include a buffer of pH 2
CD-ROM 9040B - 2 Revision 2
January 1995

for acidic wastes and a pH 12 buffer for caustic wastes; also, for
corrosivity characterization, the sample must be measured at 25±1°C if the
pH of the waste is above 12.0.) Various instrument designs may involve
use of a dial (to "balance" or "standardize") or a slope adjustment, as
outlined in the manufacturer's instructions. Repeat adjustments on
successive portions of the two buffer solutions until readings are within
0.05 pH units of the buffer solution value.
7.2 Place the sample or buffer solution in a clean glass beaker using
a sufficient volume to cover the sensing elements of the electrodes and to give
adequate clearance for the magnetic stirring bar. If field measurements are
being made, the electrodes may be immersed directly into the sample stream to an
adequate depth and moved in a manner to ensure sufficient sample movement across
the electrode -sensing element as indicated by drift -free readings (<O.1 pH).
7.3 If the sample temperature differs by more than 2°C from the buffer
solution, the measured pH values must be corrected. Instruments are equipped
with automatic or manual compensators that electronically adjust for temperature
differences. Refer to manufacturer's instructions.
7.4 Thoroughly rinse and gently wipe the electrodes prior to measuring
pH of samples. Immerse the electrodes into the sample beaker or sample stream
and gently stir at a constant rate to provide homogeneity and suspension of
solids. Note and record sample pH and temperature. Repeat measurement on
successive aliquots of sample until values differ by <0.1 pH units. Two or three
volume changes are usually sufficient.
8.0 QUALITY CONTROL
8.1 Refer to Chapter One for the appropriate QC protocols.
8.2 Electrodes must be thoroughly rinsed between samples.
9.0 METHOD PERFORMANCE
9.1 Forty-four analysts in twenty laboratories analyzed six synthetic
water samples containing exact increments of hydrogen -hydroxyl ions, with the
following results:
Accuracy as
Standard Deviation Bias Bias
pH Units pH Units % pH Units
3.5
0.10
-0.29
-0.01
3.5
0.11
-0.00
7.1
0.20
+1.01
+0.07
7.2
0.18
-0.03
-0.002
8.0
0.13
-0.12
-0.01
8.0
0.12
+0.16
+0.01
10.0 REFERENCES
CD-ROM 9040B - 3 Revision 2
January 1995

National Bureau of Standards, Standard Reference Material Catalog 1986-87,
Special Publication 260.
CD-ROM 9040B - 4 Revision 2
January 1995

METHOD 9040B
pH ELECTROMETRIC MEASUREMENT
Start
7.1 Calibrate pH
meter.
7.2 Place sample
or buffer solution
in glass beaker.
/ 7.3 Does
temperature
differ by more
than 2C from
1. buffer? i
No
7.4 Immerce
electrodes and
measure pH of
sample.
7.4 Note and record
pH and temperature;
repeat 2 or 3 times
with different
aliquots.
Stop
Yes
7.3 Correct
measured pH
values.
CD-ROM 9040B - 5 Revision 2
January 1995

METHOD 9045D
SOIL AND WASTE pH
1.0 SCOPE AND APPLICATION
1.1 This method is an electrometric procedure for measuring pH in soils and waste
samples. Wastes may be solids, sludges, or non -aqueous liquids. If water is present, it must
constitute less than 20% of the total volume of the sample.
2.0 SUMMARY OF METHOD
2.1 The sample is mixed with reagent water, and the pH of the resulting aqueous
solution is measured.
3.0 INTERFERENCES
3.1 Samples with very low or very high pH may give incorrect readings on the meter.
For samples with a true pH of >10, the measured pH may be incorrectly low. This error can be
minimized by using a low -sodium -error electrode. Strong acid solutions, with a true pH of <1,
may give incorrectly high pH measurements.
3.2 Temperature fluctuations will cause measurement errors.
3.3 Errors will occur when the electrodes become coated. If an electrode becomes
coated with an oily material that will not rinse free, the electrode can (1) be cleaned with an
ultrasonic bath, or (2) be washed with detergent, rinsed several times with water, placed in 1:10
HCI so that the lower third of the electrode is submerged, and then thoroughly rinsed with water,
or (3) be cleaned per the manufacturer's instructions.
4.0 APPARATUS AND MATERIALS
4.1 pH meter with means for temperature compensation.
4.2 Glass electrode.
4.3 Reference electrode — A silver -silver chloride or other reference electrode of
constant potential may be used.
NOTE: Combination electrodes incorporating both measuring and referenced functions are
convenient to use and are available with solid, gel -type filling materials that require
minimal maintenance.
4.4 Beaker — 50-mL.
4.5 Thermometer and/or temperature sensor for automatic compensation.
4.6 Analytical balance — capable of weighing 0.1 g.
9045D - 1 Revision 4
November 2004

5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it
is intended that all reagents shall conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are available. Other
grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Reagent water. All references to water in this method refer to reagent water, as
defined in Chapter One.
5.3 Primary standard buffer salts are available from the National Institute of Standards
and Technology (NIST) and should be used in situations where extreme accuracy is necessary.
Preparation of reference solutions from these salts requires some special precautions and
handling, such as low -conductivity dilution water, drying ovens, and carbon -dioxide -free purge
gas. These solutions should be replaced at least once each month.
5.4 Secondary standard buffers may be prepared from NIST salts or purchased as
solutions from commercial vendors. These commercially available solutions, which have been
validated by comparison with NIST standards, are recommended for routine use.
6.0 SAMPLE PRESERVATION AND HANDLING
Samples should be analyzed as soon as possible.
7.0 PROCEDURE
7.1 Calibration
7.1.1 Because of the wide variety of pH meters and accessories, detailed
operating procedures cannot be incorporated into this method. Each analyst must be
acquainted with the operation of each system and familiar with all instrument functions.
Special attention to care of the electrodes is recommended.
7.1.2 Each instrument/electrode system must be calibrated at a minimum of
two points that bracket the expected pH of the samples and are approximately three pH
units or more apart. Repeat adjustments on successive portions of the two buffer
solutions until readings are within 0.05 pH units of the buffer solution value. If an
accurate pH reading based on the conventional pH scale [0 to 14 at 25 • C] is required,
the analyst should control sample temperature at 25 t 1 • C when sample pH approaches
the alkaline end of the scale (e.g., a pH of 11 or above).
7.2 Sample preparation and pH measurement of soils:
7.2.1 To 20 g of soil in a 50-mL beaker, add 20 mL of reagent water, cover, and
continuously stir the suspension for 5 min. Additional dilutions are allowed if working with
hygroscopic soils and salts or other problematic matrices.
7.2.2 Let the soil suspension stand for about 1 hr to allow most of the
suspended clay to settle out from the suspension or filter or centrifuge off the aqueous
phase for pH measurement.
9045D - 2 Revision 4
November 2004

7.2.3 Adjust the electrodes in the clamps of the electrode holder so that, upon
lowering the electrodes into the beaker, the glass electrode will be immersed just deep
enough into the clear supernatant solution to establish a good electrical contact through
the ground -glass joint or the fiber -capillary hole. Insert the electrodes into the sample
solution in this manner. For combination electrodes, immerse just below the suspension.
7.2.4 If the sample temperature differs by more than 2 • C from the buffer
solution, the measured pH values must be corrected.
7.2.5 Report the results as "soil pH measured in water at _ C" where "_• C" is
the temperature at which the test was conducted.
7.3 Sample preparation and pH measurement of waste materials
7.3.1 To 20 g of waste sample in a 50-mL beaker, add 20 mL of reagent water,
cover, and continuously stir the suspension for 5 min. Additional dilutions are allowed if
working with hygroscopic wastes and salts or other problematic matrices.
7.3.2 Let the waste suspension stand for about 15 min to allow most of the
suspended waste to settle out from the suspension or filter or centrifuge off aqueous
phase for pH measurement.
NOTE: If the waste is hygroscopic and absorbs all the reagent water, begin the
experiment again using 20 g of waste and 40 mL of reagent water.
NOTE: If the supernatant is multiphasic, decant the oily phase and measure the pH of
the aqueous phase. The electrode may need to be cleaned (Step 3.3) if it
becomes coated with an oily material.
7.3.3 Adjust the electrodes in the clamps of the electrode holder so that, upon
lowering the electrodes into the beaker, the glass electrode will be immersed just deep
enough into the clear supernatant to establish good electrical contact through the ground -
glass joint or the fiber -capillary hole. Insert the electrode into the sample solution in this
manner. For combination electrodes, immerse just below the suspension.
7.3.4 If the sample temperature differs by more than 2 •C from the buffer
solution, the measured pH values must be corrected.
7.3.5 Report the results as "waste pH measured in water at _• C" where "_• C"
is the temperature at which the test was conducted.
8.0 QUALITY CONTROL
8.1 Refer to Chapter One for the appropriate QC protocols.
8.2 Electrodes must be thoroughly rinsed between samples.
9.0 METHOD PERFORMANCE
9.1 No data provided.
9045D - 3 Revision 4
November 2004

10.0 REFERENCES
1. Black, Charles Allen; Methods of Soil Analysis; American Society of Agronomy:
Madison, WI, 1973.
2. National Bureau of Standards, Standard Reference Material Catalog, 1986-87, Special
Publication 260.
9045D - 4 Revision 4
November 2004

7.2.1 Add 20 mL
water to 20 g soil;
stir continuously
for 5 minutes.
7.2.2 Let soil
suspension
stand for 1
hour or filter.
Correct
measured pH
values.
METHOD 9045D
SOIL AND WASTE pH
Start
7.1 Calibrate
each instrument/
electrode
system.
Is the 7.3.1 Add 20 mL
Soil sample soil water to 20 g waste;
or waste, stir continuously
for 5 minutes.
7.3.2 Let waste
suspension
stand for 15
minutes or filter.
Is waste yes
Repeat experiment
hydroscopic7
with 20 g waste
and 40 ml- water.
No
Insert
eleos
Is
No su ernatant Yee
�—
Decent oily
phase;
into male
p
m l iphasic7
measure 'pH of
solution,
aqueous phase.
Aqueous
Phase
Yeser
ps
*Report
dlre
Stop-
9045D - 5
Revision 4
November 2004

METHOD 9045C
SOIL AND WASTE pH
1.0 SCOPE AND APPLICATION
1.1 Method 9045 is an electrometric procedure for measuring pH in
soils and waste samples. Wastes may be solids, sludges, or non -aqueous
liquids. If water is present, it must constitute less than 20% of the total
volume of the sample.
2.0 SUMMARY OF METHOD
2.1 The sample is mixed with reagent water, and the pH of the
resulting aqueous solution is measured.
3.0 INTERFERENCES
3.1 Samples with very low or very high pH may give incorrect
readings on the meter. For samples with a true pH of >10, the measured pH may
be incorrectly low. This error can be minimized by using a low -sodium -error
electrode. Strong acid solutions, with a true pH of <l, may give incorrectly
high pH measurements.
3.2 Temperature fluctuations will cause measurement errors.
3.3 Errors will occur when the electrodes become coated. If an
electrode becomes coated with an oily material that will not rinse free, the
electrode can 0 )-be cleaned with an ultrasonic bath, or (2) be washed with
detergent, rinsed several times with water, placed in 1:10 HC1 so that the
lower third of the electrode is submerged, and then thoroughly rinsed with
water, or (3) be cleaned per the manufacturer's instructions.
4.0 APPARATUS AND MATERIALS
4.1 pH Meter with means for temperature compensation.
4.2 Glass Electrode.
4.3 Reference electrode: A silver -silver chloride or other
reference electrode of constant potential may be used.
NOTE: Combination electrodes incorporating both measuring and
referenced functions are convenient to use and are available
with solid, gel -type filling materials that require minimal
maintenance.
4.4 Beaker: 50-mL.
4.5 Thermometer and/or temperature sensor for automatic
compensation.
CD-ROM 9045C - 1 Revision 3
January 1995

4.6 Analytical balance: capable of weighing 0.1 g.
5.0 REAGENTS
5.1 - Reagent grade chemicals shall be used in all tests. Unless
otherwise indicated, it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the American
Chemical Society, where such specifications are available. Other grades may
be used, provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the
determination.
5.2 Reagent water. All references to water in this method refer to
reagent water, as defined in Chapter One.
5.3 Primary standard buffer salts are available from the National
Institute of Standards and Technology (NIST) and should be used in situations
where extreme accuracy is necessary. Preparation of reference solutions from
these salts requires some special precautions and handling, such as low -
conductivity dilution water, drying ovens, and carbon -dioxide -free purge gas.
These solutions should be replaced at least once each month.
5.4 Secondary standard buffers may be prepared from NIST salts or
purchased as solutions from commercial vendors. These commercially available
solutions, which have been validated by comparison with NIST standards, are
recommended for routine use.
6.0 SAMPLE PRESERVATION AND HANDLING
6.-1 All samples must be collected using a sampling plan that
addresses the considerations discussed in Chapter Nine of this manual.
6.2 Samples should be analyzed as soon as possible.
7.0 PROCEDURE
CD-ROM
7.1 Calibration:
7.1.1 Because of the wide variety of pH meters and
accessories, detailed operating procedures cannot be incorporated into
this method. Each analyst must be acquainted with the operation of each
system and familiar with all instrument functions. Special attention to
care of the electrodes is recommended.
7.1.2 Each instrument/electrode system must be calibrated at a
minimum of two points that bracket the expected pH of the samples and
are approximately three pH units or more apart. Repeat adjustments on
successive portions of the two buffer solutions until readings are
within 0.05 pH units of the buffer solution value. If an accurate pH
reading based on the conventional pH scale [0 to 14 at 25°C] is
required, the analyst should control sample temperature at 25±1°C when
9045C - 2 Revision 3
January 1995

sample pH approaches the alkaline end of the scale (e.g., a pH of 11 or
above).
�7 `'a11p11+' ,II, I,naratinn and rsH mPasuremPnf ref s�olMls�'
CD-ROM
7.2.1 To 20 g of soil in a 50-mL beaker,, add 20 mL of reagent
water, cover, and continuously stir the suspension for 5 minutes. .
Additional dilutions are allowed if working with hygroscopic soils and
salts or other problematic matrices.
7.2.2 Let the soil suspension stand for about 1 hour to allow
most of the suspended clay to settle out from the suspension or filter
or centrifuge off the aqueous phase for pH measurement.
7.2.3 Adjust the electrodes in the clamps of the electrode
holder so that, upon lowering the electrodes into the beaker, the glass
electrode will be immersed just deep enough into the clear supernatant
solution to establish a good electrical contact through the ground -glass
joint or the fiber -capillary hole. Insert the electrodes into the
sample solution -in this manner. For combination electrodes, immerse
just below the suspension.
7.2.4 If the sample temperature differs by more than 2°C from
the buffer solution, the measured pH values must be corrected.
7.2.5 Report the results as "soil pH measured in water at
°C" where "_°C" is the temperature at which the test was conducted.
7.3 Sample preparation and pH measurement of waste materials:
7.3.1 To 20 g of waste sample in a 50-mL beaker, add 20 mL of
reagent water, cover, and continuously stir the suspension for 5
minutes. . Additional dilutions are allowed if working with hygroscopic
wastes and salts or other problematic matrices.
7.3.2 Let the waste suspension stand for about 15 minutes to
allow most of the suspended waste to settle out from the suspension or
filter or centrifuge off aqueous phase for pH measurement.
NOTE: If the waste is hygroscopic and absorbs all the reagent
water, begin the experiment again using 20 g of waste and 40 mL
of reagent water.
NOTE: If the supernatant is multiphasic, decant the oily phase
and measure the pH .of the aqueous phase. The electrode may need
to be cleaned (Step 3.3) if it becomes coated with an oily
material.
7.3.3 Adjust the electrodes in the clamps of the electrode
holder so that, upon lowering the electrodes into the beaker, the glass
electrode will be immersed just deep enough into the clear supernatant
to establish good electrical contact through the ground -glass joint or
the fiber -capillary hole. Insert the electrode into the sample solution
9045C - 3 Revision 3
January 1995

J
in this manner. For combination electrodes, immerse just below the
suspension.
7.3.4 If the sample temperature differs by more than 2°C from
the buffer solution, the measured pH values must be corrected.
7.3.5 Report the results as "waste pH measured in water at _
°C" where "°C" is the temperature at which the test was conducted.
8.0 QUALITY CONTROL
8.1 Refer to Chapter One for the appropriate QC protocols.
8.2 Electrodes must be thoroughly rinsed between samples.
9.0 METHOD PERFORMANCE
9.1 No data provided.
10.0 REFERENCES
1. Black, Charles Allen; Methods of Soil Analysis; American Society of
Agronomy: Madison, WI, 1973.
2. National Bureau of Standards, Standard Reference Material Catalog, 1986-
87, Special Publication 260.
CD-ROM 9045C - 4 Revision 3
January 1995

7.2.1 Add 20 mL
water to 20 g soil
stir continuously
for 5 minutes.
7.2.2 Let soil
suspension
stand for 1
hour or filter.
Correct
measured pH
values.
CD-ROM
METHOD 9045C
SOIL AND WASTE pH
Start
7.1 Calibrate
each instrument/
electrode
system.
Is the 7.3.1 Add 20 mL
Soil sample soil water to 20 g waste;
or wast
e? stir continuously
for 5 minutes.
7.3.2 Let waste
suspension
stand for 15
minutes or filter.
Is waste Yes
Repeat experiment
hydroscopic?
with 20 g waste
and 40 mL water.
No
Insert
electrodes
Is
No supernatant Yes
Decant oily
into sample
�— multiphasic7
phase;
measure pH of
solution.
aqueous phase.
Aqueous
Phase
Do
sample
Yes and buffer
sol'n temps
vary by
2C?
No
Report
results and
temperature
Stop
9045C - 5
Revision 3
January 1995

aou pn values
Subject: Soil pH values
From: "Larry Ausley" <[e-mail]>
Date: Wed, 24 Aug 2005 10:21:50 -0400
To: <[e-mail]>
Ellen, per our discussion yesterday, I performed an ad hoc experiment as below:
For the soil samples:
5G2220- "Lagoon 3"
5G2221- "Residuals Fill Area"
5G2222- "Lagoon 2"
I placed 50ml volume of the sample in a 100ml graduated cylinder and diluted to 100ml with laboratory
deionized water. Each sample was slurried by shaking and once slurried was mixed by inverting 10 times.
Each cylinder was allowed to sit for 30 minutes. pH was then measured in the overlying water in each
cylinder.
The results are as follow:
Initial pH of laboratory deionized water= 5.3
Slurry of sample 5G2220=3.7
Slurry of sample 5G2221=3.5
Slurry of sample 5G2222=3.0
To reiterate our discussion, these values should not be construed to represent in situ pH as allowable
holding time for pH under 40CFR part 136 is 15 minutes, in addition to the fact that these results
represent an artificial in vitro modification of the samples. If you should have any questions, please give
me a call.
Larry Ausley, CPM
Microbiology & Inorganic Chemistry Branch Manager
NC Div. of Water Quality Laboratory Section
1623 Mail Service Center
Raleigh, NC 27699-1623
(t) 919.733.3908 x 222
(f) 919.733.6241
http://www.dwglab.org
1 of 1 1/6/2006 10:54 AM

31'` yy
Report to:�i�"i 1,1 WATER QUALITY SECTION Page of )
CHAIN OF CUSTODY (COC) RECORD
NC DENRIDWQ LABORATORY (check one): I�/NTRAL I J ARO I J WaRO
For Investigation of:
Sample collector (print name)
and DM-1 forms completed by.
r ,�j�!
• Ptlt 1• 2n Sample collector's signature:
Field storage conditions and location (when applicable):
A S i9 br�C 1. t
IAb Use Only
LAB NO.
STATION NO.
STATION LOCATION
DATE
SAMPLED
TIME
SAMPLED
NUMBER
OF
CONTAINERS
.3
I
Relinquished by (si ature)
Dale
Time
Received by (signature):
Date
Time
Relinquished by (signature): I
Date
Time
Received by (signature):
Date
Time
Relinquished by (signature):
Date
Time
Received by (signature):
Date
Time
Method of Shipment circle one)-
State Courier Hand -delivered Federal Ex ress UPS Other.
7 lGt,+ � ,
Security'Pype a�d Conditions:
ea e y:
�� /•tG1 /�!�'
Broken by:
INTRALABORATORY CHAIN OF CUSTODY - Lab Use Onlv
LAB NUMBERS
FROM THROUGH
NUMBER
BOTTLES
ANALYSES
REQUESTED
RELINQUISHED
BY:
RECEIVED `.
BY:
DATE
TIME
QA\Forms\Sample Receiving\COC form WQ 4110101 dns

nonn uaronna
GROUNDWATER FIELD/LAB FORM Department of Environment and Natural Resources
DIVISION OF WATER QUALITY -GROUNDWATER SECTION
SAMPLE TYPE SAMPLE PRIORITY
County ROWAN ❑ Water ErRoutine Lab Number
Quad No Serial No. Soil ❑ Emergency 3 Date Received Time:
Lat. Long. ❑ Oth_er/ Rec'd By: From:Bus, Courier, Hand Del.,
Chain of Custody Other:
Report To: ARO, FR , NIFrR-s't,RCe'ntra1
OWaRO, WiRO, Data Entry By: Ck:
WSRO, Kinston F Off., Other: Date Reported:
Shipped by: B , Courie , Hand Del., Other. Purpose:
Collector(s): Date_8 23-05 Time1L: /,2am ✓ Baseline, Complaint, Compliance, LUST, Pesticide Study, Federal Trust, Other:
FIELD ANALYSES Owner_ALCHEM (circle one)
pH 400 Spec. Cond.94 at 250C Location or Site Lagoon 2
Temp.lo °C Odor Description of sampling point residuals collected out of lagoon 2
Appearance Sampling Method grab Sample Interval
Field Analysis By Remarks um baner. etc.i
ARr1RATr1RY ANAI YSF.q (Pumping time, air temp., etc.)
BOD 310 mg/L
COD High 340 mg/L
COD Low 335 mg/L
Coliform: MF Fecal 31616 /loom]
Coliform: MF Total 31504 /100ml
TOC 680 mg/L
Turbidity 76 NTU
Residue, Suspended 530 mg/L
units
Alkalinity to pH 4.5 410 mg/L
Alkalinity to pH 8.3 415 mg/L
Carbonate 445 mg/L
Bicarbonate 440 mg/L
Carbon dioxide 405 mg/L
Chloride 940 mg/L
Chromium: Hex 1032 uglL
Color: True 80 CU
Cyanide 720 mg/L
Lab comments
Diss. Solids 70300 mg/L
Fluoride 951 mg/L
Hardness: Total 900 mg/L
Hardness (non-carb) 902 mg/L
Phenols 32730 ug/I
Specific Cond. 95 uMhos/cm
Sulfate 945 mg/L
Sulfide 745 mg/L
Oil and Grease mg/L
NH3 as N 610 mg/L
TKN as N 625 mg/L
NO2 + NO3 as N 630 mg/L
P: Total as P 665 mg/L
Nitrate (NO3 as N) 620 mg/L
Nitrite (NO2 as N) 615 mg/L
GW-54 REV. 7/03 For Dissolved Analysis -submit filtered sample and write "DIS" in block.
Ag-Sliver 46566
u /L
X
AI -Aluminum 46557
u /L
X
As -Arsenic 46551
u /L
Ba-Barium 46658
u /L
Ca-Calclum 46552
m /L
X
Cd-Cadmium 46559
u /L
X
Cr-Chromium 46559
u /L
X
Cu-Copper 46562
u /L
X
Fe -Iron 46563
u /L
X
Hg-Mercury 71900
u /L
K-Potassium 46555
m /L
Mg -Magnesium 46554
m /L
Mn-Manganese 46565
u /L
Na-Sodium 46556
m /L
X
Ni-Nickel
u /L
X
Pb-Lead 46564
u /L
X
se -Selenium
u /L
X
Zn-Zinc 46567
u L

GROUNDWATER FIELD/LAB FORM
SAMPLE TYPE SAMPLE PRIORITY
County ROWAN ❑ Water Routine
Quad No Serial No. esoil ❑ Emergency
Lat. Long. ❑ Other/
Nonn uarouna
Department of Environment and Natural Resources
DIVISION OF WATER QUALITY -GROUNDWATER SECTION
Lab Number
Date Received Time:
Rec'd By: From:Bus, Courier, Hand Del.,
Chain of Custody Other:
Report To: AROSF.
FIRRO, WaRO, WIRO, Data Entry By: Ck:
WSRO, Kinston Central Off., Other: Date Reported:
Shipped by: Bud Del., Other: ,Purpose:
Collector(s): Date_8-23-05 Time,: rams Baseline, Complaint, Compliance, LUST, Pesticide Study, Federal Trust, Other:
FIELD ANALYSES Owner _ALCHEM (circle one)
pH 400 Spec. Cond.94at 250C Location or Site Residuals fill area
Temp.lo °C Odor Description of sampling point residuals collected out of residuals fill area
Appearance Sampling Method grab Sample Interval
Field Analysis By Remarks um aier. e�.
LABORATORY ANALYSES (Pumping time, air temp., etc.)
BOD 310 mg/L
COD High 340 mg/L
COD Low 335 mg/L
Coliform: MF Fecal 31616 /100ml
Coliform: MF Total 31504 /100ml
TOG 680 mg/L
Turbidity 76 NTU
Residue, Suspended 530 mg/L
units
Alkalinity to pH 4.5410 mg/L
Alkalinityto pH 8.3 415 mg/L
Carbonate 445 mg/L
Bicarbonate 440 mg/L
Carbon dioxide 405 mg/L
Chloride 940 mg/L
Chromium: Hex 1032 ug/L
Color: True 80 Cu
Cyanide 720 mg/L
Lab Comments
Diss. Solids 70300 mg/L
Fluoride 951 mg/L
Hardness: Total 900 mg/L
Hardness (non-carb) 902 mg/L
Phenols 32730 ug/I
Specific Cond. 95 uMhos/cm
Sulfate 945 mg/L
Sulfide 745 mg/L
Oil and Grease mg/L
NH3 as N 610 mg/L
TKN as N 625 mg/L
NO2 + NO3 as N 630 mg/L
P: Total as P 665 mg/L
Nitrate (NO3 as N) 620 mg/L
Nitrite (NO2 as N) 615 mg1L
GW-54 REV. 7/03 For Dissolved Analysis -submit filtered sample and write "DIS° in block.
Ag-Silver 46566
u /L
X
AI -Aluminum 46557
u /L
X
As -Arsenic 46661
u /L
Ba-Barium 46658
u /L
Ca -Calcium 46552
m /L
X
Cd-Cadmium 46559
u /L
X
Cr-Chromium 46559
u /L
X
Cu-Copper 46562
u /L
X
Fe -Iron 46563
u /L
X
Hg-Mercury 71900
u /L
K-Potassium 46555
m /L
Mg -Magnesium 46554
m /L
Mn-Manganese 46565
u /L
Na-Sodium 46556
m IL
X
Ni-Nickel
u /L
X
Pb-Lead 46564
u /L
X
Se -Selenium
u /L
X
Zn-Zinc 46567
u /L

North Carolina
GROUNDWATER FIELD/LAB FORM Department of Environment and Natural Resources
DIVISION OF WATER QUALITY -GROUNDWATER SECTION
SAMPLE TYPE SAMPLE PRIORITY
County ROWAN ❑ Water 9"-Routine Lab Number
Quad No -Serial No. Moil ❑ Emergency Date Received Time:
Lat. Long. ❑ Oth__e,,,,r' Rec'd By: From:Bus, Courier, Hand Del.,
L�Chain of Custody Other:
Report To: ARO, FRO, ffZO, O, WaRO, WiRO, Data Entry By: Ck:
WSRO, Kinston F rust, Central Off., Other: Date Reported:
Shipped by: Bu Courier Hand Del., Other: Purpose:
Collector(s): S. Date_8-23-05 Time_.01'am ✓ Baseline, Complaint, Compliance, LUST, Pesticide Study, Federal Trust, Other:
FIELD ANALYSES Owner_ALCHEM (circle one)
pH 400 Spec. Cond.94 at 250C Location or Site Lagoon 3
Temp.lo eC Odor Description of sampling point residuals collected out of lagoon 3
Appearance Sampling Method grab Sample Interval
Field Analysis By Remarks um Wier. etc.
ARr1RATr1RV AMAI VCFC (Pumping time, air temp., etc.)
BOD 310 mg/L
COD High 340 mg/L
COD Low 335 mg/L
Coliform: MF Fecal 31616 /looml
Coliform: MF Total 31504 /loom]
TOC 680 mg/L
Turbidity 76 NTU
Residue, Suspended 530 mg/L
units
Alkalinity to pH 4.5 410 mg/L
Alkalinity to pH 8.3 415 mg/L
Carbonate 445 mg/L
Bicarbonate 440 mg/L
Carbon dioxide 405 mg/L
Chloride 940 mg1L
Chromium: Hex 1032 ug/L
Color: True 80 CU
Cyanide 720 mg/L
Lab Comments S
Diss. Solids 70300 mg/L
Fluoride 951 mg/L
Hardness: Total 900 mg/L
Hardness (non-carb) 902 mg/L
Phenols 32730 ug/I
Specific Cond. 95 uMhos/cm
Sulfate 945 mg/L
Sulfide 745 mg/L
Oil and Grease mg/L
NH3 as N 610 mg/L
TKN as N 625 mg/L
NO2 + NO3 as N 630 mg/L
P: Total as P 665 mg/L
Nitrate (NO3as N) 620 mg/L
Nitrite (NO2as N) 615 mg/L
GW-54 REV. 7103 For Dissolved Analysis -submit filtered sample and write "DIS' in block.
Ag-Silver 46566
u /L
X
AI -Aluminum 46557
u /L
X
As -Arsenic 46551
u /L
Ba-Barium 46558
u /L
Ca -Calcium 46552
m /L
X
Cd-Cadmium 46559
u /L
X
Cr-Chromium 46559
u /L
X
Cu-Copper 46562
u /L
X
Fe -Iron 46563
u /L
X
Hg-Mercury 71900
u /L
K-Potassium 46555
m /L
Mg -Magnesium 46554
m /L
Mn-Manganese 46565
u /L
Na-Sodium 46556
m /L
X
Ni-Nickel
u /L
X
Pb-Lead 46564
u /L
X
Se -Selenium
u /L
X
Zn-Zinc 46567
u IL

9104e,-Y� M/W�ff ar(-*
pH
Al
Date
MW-1
MW-2
MW-1
MW-2
Office
Stream
7/18/2002
5.70000
5.30000
0.88000
0.13700 replacement wells installed
2/25/2003
5.85000
5.10000
0.03400
0.34000
7/17/2003
5.80000
5.60000
0.28100
0.17800
2/5/2004
6.50000
5.20000
0.06200
0.20700
7/30/2004
6.00000
5.20000
0.12500
0.59600
2/15/2005
5.75000
4.80000
0.05100
0.18400
2/15/2005
5.30000
4.60000
0.16000
0.43000 MRO sampling
7/13/2005
5.80000
5.50000
0.72000
0.82000
7.01000
0.27000
12/1/2005
5.45000
5.50000
0.90000
3.24000
12.70000
2/22/2006
5.74000
4.81000
0.31800
0.81000
5.88000
0.65600
6/15/2006
5.96000
5.20000
0.30000
2.34000
2.93000
11 /6/2006
5.63000
4.35000
0.43000
4.76000
0.61500
12/5/2007
5.70000
4.90000
0.79000
4.20000 MRO sampling
12/5/2007
0.55000 Alchem sampling
2/27/2007
4.75000
4.70000
2.29000
0.76300
0.24000
0.84500
3/23/2007

7RVATIONTECHNIQ
BLE 2-36
CONTAINERS, PREU-S, ANDHOLDING TIMES
OUS ICES
Name
Inorganic Tests:
Container' Preservation Maximum holding time
Chloride
P, G
None required
28 days
Cyanide, total and
P, G
Cool to 4°C; if oxidizing
14 days
amenable
agents present add 5 mL
to chlorination
0.1 N NaAsO2 per L or
0.06 g of ascorbic acid
per L; adjust pH>12 with
50% NaOH.
See Method 9010 for
other interferences.
Hydrogen ion (pH)..m-a-
P, G
None required
24 hours
Nitrate
P, G
Cool to 4°C
48 hours
Sulfate
P, G
Cool to 40C
28 days
Sulfide
P, G
Cool to 4°C, add zinc
7 days
acetate
Metals:
Chromium VI
P, G
Cool to 4°C
24 hours
Mercury
P, G
HNO3 to pH<2
28 days
Metals, except chromium VI
P, G
HNO3 to pH<2
6 months
and mercury
Organic Tests:
Acrolein and acrylonitrile
G, PTFE-lined
Cool to 4°C,
14 days
septum
0.008% Na2S2O3a,
Adjust pH to 4-5
Benzidines
G, PTFE-lined
Cool to 4°C,
7 days until extraction,
cap
0.008% Na2S2O33
40 days after extraction
Chlorinated hydrocarbons
G, PTFE-lined
Cool to 4°C,
7 days until extraction,
cap
0.008% Na2S2O33
40 days after extraction
Dioxins and Furans
G, PTFE-lined
Cool to 4°C,
30 days until extraction,
cap
0.008% Na2S2O33
45 days after extraction
Haloethers
G, PTFE-lined
Cool to 4°C,
7 days until extraction,
cap
0.008% Na2S2O33
40 days after extraction
Nitroaromatics and
G, PTFE-lined
Cool to 4°C,
7 days until extraction,
cyclic ketones
cap
0.008% Na2S2O33,
40 days after extraction
store in dark
Nitrosamines
G, PTFE-lined
Cool to 4°C,
7 days until extraction,
cap
0.008% Na2S2O33,
40 days after extraction
store in dark
(continued on next page)
CD-ROM TWO - 48 Revision 3
December 1996

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NCDENR
North Carolina Department of Environment and Natural Resources
Michael F. Easley, Governor William G. Ross Jr., Secretary
January 27, 2006
Mr. Wayne Drye
ALCHEM, INC.
8135 Red Road
Rockwell, NC 28138
Subject: Field Parameter Certification
Dear Mr. Drye:
Enclosed please find the following items: Application for Field Parameter
Certification, Instructions for filling out the application, A copy of the Laboratory
Certification Rules, an example field analytical sheet and a copy of the pH Technical
Assistance Document.
If you have any questions, or we can be of assistance please do not hesitate to
contact us at 704 663-1699.
Sincerely
3
Chester E. Whiting
Lab Certification
cc: James Meyer
610 East Center Avenue, Suite 301, Mooresville, North Carolina 28115 One
Phone: [phone] FAX: [phone] l Internet: www.enr.state.nc.us NorthCarohna
Aatmrally

ALCHEM August 20, 2007 ® lab