MBMG ANALYTICAL LABORATORY

QUALITY ASSURANCE MANUAL

Jacqueline Timmer

Montana Bureau of Mines and Geology Open-File Report 729

June 2020
Jacqueline Timmer

Cover photo: Instruments in the MBMG Analytical Laboratory in 2020. Top row: Thermo iCAP 6000 ICP-OES, Picarro
G2131-I 13C High-Precision Isotopic carbon dioxide (CO2) analyzer. Middle row: Picarro L2130-I Isotopic Water
Analyzer, Thermo iCAP Q ICP-MS, and HIDEX 300SL Auto TDCR Radon Analyzer. Bottom row: Metrohm 882 IC Plus
Anion Chro- matograph, Metrohm 855 Robotic Titrator. Photos by Jacqueline Timmer.

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 MBMG Open-File Report 729: Analytical Lab QA
Manual
TABLE OF CONTENTS

List of Acronyms.......................................................................................................................................v
Introduction...............................................................................................................................................1
Sample Handling.......................................................................................................................................1
Sample Handling for Inorganic Constituents......................................................................................1
Sample Handling for Organic (Inorganic) Carbon.............................................................................3
Sample Handling for Radon................................................................................................................3
Sample Handling for Semi-Volatile Organic Constituents.................................................................3
Sample Acceptance...................................................................................................................................3
Sample Login............................................................................................................................................4
Inorganic.............................................................................................................................................4
Organic................................................................................................................................................4
Sample Preparation...................................................................................................................................4
Inorganic.............................................................................................................................................4
Organic................................................................................................................................................5
Short-Term Sample Storage......................................................................................................................5
Inorganic.............................................................................................................................................5
Organic................................................................................................................................................5
Long-Term Storage...................................................................................................................................5
Sample Analysis........................................................................................................................................5
Data Acquisition and Reporting................................................................................................................5
Outside Evaluation Programs....................................................................................................................5
Preventive Maintenance............................................................................................................................5
Waste Disposal....................................................................................................................................6
Chemical Inventory.............................................................................................................................6
Certified Analytes................................................................................................................................6
Quality Control Protocol.....................................................................................................................6

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 FIGURES
Figure 1. Sample bottle label....................................................................................................................1

TABLES

Table 1. Sample container, preservation, and hold time..........................................................................2

Table 2. Equipment routinely used by MBMG Laboratory......................................................................6
Table 3. Analyte parameters and associated methods...............................................................................7
Table 4. Quality control check samples for analytical work.....................................................................8
 MBMG Open-File Report 729: Analytical Lab QA
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LIST OF ACRONYMS

‰ per mille
CCV Continuing calibration verification
COC Chain of custody
CRDS Cavity ring-down spectroscopy
DIC Dissolved inorganic carbon
DOC Dissolved organic carbon
DOT Department of Transportation
EPA Environmental Protection Agency
ERA Environmental Resource Associates
FA Filtered Acidified
FU Filtered Unpreserved
GCMS Gas chromatograph mass spectroscopy
GWIC Groundwater Information Center
H2SO4 Sulfuric acid
HCl Hydrochloric acid
HDPE High-density polyethylene
HNO3 Nitric acid
IC Ion chromatograph
ICP-MS Inductively coupled plasma mass spectroscopy
ICP-OES/AES Inductively coupled plasma-optical/atomic emission spectroscopy
ICV Initial calibration verification
ID Identification
LCS Laboratory control sample
LIMS Laboratory Information Management System
LSC Liquid scintillation counter
MBMG Montana Bureau of Mines and Geology
MDL Method detection limit
mg/L milligrams per liter (parts per million)
MRL Method reporting limit
MTDPHHS Montana Department of Public Health and Human Services
MUS Montana University System
pCi/L picocuries per liter
QA/QC Quality assurance/quality control
RA Raw Acidified
RPD Relative percent difference
RU Raw Unpreserved
SAP Sampling and analysis plan
SOP Standard operating procedure
SPE Solid phase extraction
SRS Standard resource sample
SVOC Semi-volatile organic compounds
TOC Total organic carbon
USGS United States Geological Survey
VOA Volatile organic analysis
μg/L micrograms per liter (parts per billion)

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INTRODUCTION source.

The Montana Bureau of Mines and Geology

(MBMG) Analytical Laboratory is located on the
first floor of the Natural Resources Building (NRB)
on the Montana Tech campus (1300 West Park
Street)
in Butte, MT. The MBMG Analytical Lab provides a
wide array of analytical support to MBMG
profession- als and their projects, as well as to
research from pro- fessors and graduate and
undergraduate students from Montana Tech and other
Montana University System (MUS) schools.
The MBMG analytical lab is committed to quality
assurance and strives to ensure all data produced by
the lab is high quality and meets or exceeds minimum
QA/QC standards. The laboratory is currently
certified by the Montana Department of Public Health
and Hu- man Services (MTDPHHS) Laboratory
Certification Program and is licensed to analyze
public drinking water supplies.
This Quality Assurance Manual is intended to
meet the requirement of a QA plan outlined in the
MTDPHHS Laboratory Certification Program, as
well as be useful as a training tool to laboratory
personnel. It should also be useful to field
personnel/samplers within the MBMG.
In addition to analyzing for pH, conductivity,
alkalinity, major anions (ion chromatograph, IC), and
cations (inductively coupled plasma-optical/atomic
emission spectroscopy, ICP-OES/AES), the MBMG
Analytical Lab also has the capability of analyzing
water samples for trace elements, including some
rare earth elements (inductively coupled plasma mass
spectroscopy, ICP-MS), organic and inorganic
carbon
(TOC analyzer), 222Radon (liquid scintillation
count- er, LSC), stable water isotopes and carbonate-
carbon isotopes (cavity ring-down spectroscopy,
CRDS), and project-specific organic compounds (gas
chromato- gram mass spectroscopy, GCMS).

SAMPLE HANDLING
Sample Handling for Inorganic Constituents
The adherence to sampling protocols greatly
contributes to data quality. As outlined below, these
procedures are meant to ensure that data from sample
analyses reflect the actual composition of the water
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 Jacqueline
Timmer
Samples should be taken using project-specific
standard operating procedures (SOP). All inorganic
samples that will be submitted to the MBMG Lab-
oratory are collected in high-density polyethylene
(HDPE) bottles obtained from the laboratory. If
sam- plers are planning on collecting 20 or more
samples, it is important they let the lab know as
soon as possible (at least 7 to 10 days before
needed). This not only gives the lab time to get
bottles and acid ready, but also ensures there are
enough bottles available. Labels are supplied with
the bottles and have spaces for the appropriate
information concerning the sample (i.e., sample ID,
date, time, filtration, preservation, etc.; see fig. 1).
All bottles should be filled to a zero headspace
capacity when possible. NOTE: When acid is being
added for preservation, some headspace is needed
to allow for mixing of the acid.

Figure 1. Sample bottle label.

Filtration and preservation of samples will

depend on what analyses are needed (table 1). The
samples collected for the MBMG suite of inorganic
parameters are:
Raw Unpreserved (RU):
An unfiltered, unpreserved 500 mL aliquot of
the sample, used for the determination of
specific conductance, pH, and alkalinity in the
laboratory.
Circle UNTREATED (RAW) on the label.
Samples should be kept at or below 4°C and
submitted to the laboratory as soon as
possible. While alkalinity and specific
conductance have a holding time of 14 to 28
days, respectively, pH needs to be analyzed
as soon as possible.
Filtered Acidified (FA):
1. A 500 mL aliquot of sample filtered
through a 0.45 μm pore diameter membrane
filter and preserved with 5 mL of nitric acid
(HNO3) to

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Table 1. Sample container, preservation, and hold time.

Volume Holding
Parameter
(mL) Container Preservation Time
Filter (Days)
Method GENERAL
CHEMISTRY
Acidity EPA 305.1 500 HDPE Cool, 4°C N RU 14
Alkalinity EPA 310.1 500 HDPE Cool, 4°C N RU 14
Chloride EPA 300 250 HDPE Cool, 4°C Y FU 28
Conductivity EPA 120.1 500 HDPE Cool, 4°C N RU 28
Fluoride EPA 300 250 HDPE Cool, 4°C Y FU 28
Nitrate-N (IC) EPA 300 250 HDPE Cool, 4°C Y FU 28
Nitrite-N (IC) EPA 300 250 HDPE Cool, 4°C Y FU 48 hours
Nitrate/Nitrite-N
HACH 250 HDPE
(nutrient) Y FU 28
H2SO4,Cool,
pH EPA 150.1 500 HDPE Cool, 4°C N RU ASAP
Ortho-Phosphate-P EPA 300 250 HDPE Cool, 4°C Y FU 28
4°
EPA C
Radon
913.0
125 Glass Cool, 4°C N RU ASAP
Mo
Sulfate EPA
d 300 250 HDPE Cool, 4°C Y FU 28
Water Isotopes Picarro 25 HDPE Y FU NONE
METALS/TRACE METALS
MS- EPA 200.7/
ICP-OES/ICP- 500 HDPE HNO3 Y FA 180
Dissolved 200.8
MS- EPA 200.7/
ICP-OES/ICP- 500 HDPE HNO3 N RA 180
Total 200.8
Recoverable
ORGANICS
Pentachlorophenol EPA 528.0 14 to extract
1000 Glass HCl, 4°C N RA 14 to
Mod
Carbon analysis
Organic EPA 415.3 40 Glass H2SO4, 4°C FA/
Y/N 28
FU
Dissolved / Total

a pH <2. This is used for the determination Filtered Unpreserved (FU):

of major metals and trace elements by
EPA A 250 mL aliquot of sample filtered through
Methods 200.7 (ICP-OES) and 200.8 (ICP-MS). a 0.45 μm pore diameter membrane filter.
No
Circle FILTERED + 1% HNO3 on the label. preservative is added. Samples are used for the
Once filtered and preserved, samples have a determination of anions by EPA Method 300.0
holding time of 6 months. (IC).
2. A 250 mL sample aliquot filtered Circle FILTERED on the label. Samples should
through a 0.45 μm pore diameter membrane be kept at or below 4°C. Once filtered and
filter and preserved with 2.5 mL of 5% preserved, samples have a holding time of 28
sulfuric acid days.
(H SO ) to a pH <2. These are used for the
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determination of nitrite plus nitrate (and total 10242, respectively.
nitrogen, when requested), often referred to
as ‘Nutrients’ by HACH Methods 10206 and Circle FILTERED + 0.5% H2SO4 on the label.
Samples should be kept at or below 4°C. Once
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Jacqueline
Timmer
filteredand preserved, samples have a holding Water Isotope:
time of 28 days.
25 mL of filtered, unpreserved sample is also
needed for water isotopes. Samples are collected
in 25 mL plastic vials with caps that have conical
inserts to ensure no headspace. There is no
holding time for water isotopes.

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 MBMG Open-File Report 729: Analytical Lab QA
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Raw Acidified (RA):
come from a source under laminar flow conditions.
A 500 mL aliquot of unfiltered sample preserved It is important to ensure there are no air bubbles in
with 5 mL of nitric acid for the determination of the sample bottle. The sample must be labeled
total recoverable metals and trace elements by with the date and time of collection. Because of
EPA Methods 200.7 (ICP-OES) and 200.8 (ICP- radon’s
MS). short half-life (3.8 days), it is imperative to submit the
sample to the laboratory as soon as possible, but no
Circle RAW + 1% HNO3 on the label. Once longer than 48 hours after sampling. Samples need to
preserved, samples have a holding time of 6 be kept on ice until they are submitted to the laborato-
months. ry. Radon is analyzed by EPA Method 913.0 modified
(LSC).
Sample Handling for Organic (Inorganic) Carbon
See project-specific SOP for proper sample collec- Sample Handling for Semi-Volatile
tion and filtration. Field filtration of the sample, per- Organic Constituents
formed by the sampler, will depend upon the Collect sample as outlined by the project-
sampler’s request for total organic carbon (TOC) or specific SOP. One liter amber bottles are used to
dissolved organic carbon (DOC). TOC samples do not collect sam- ples from the field. The sample is
require filtration, whereas DOC samples do. NOTE: If preserved by acid- ification to pH <2 with 6N
filtra- tion is required, ensure filters used are 0.45 m hydrochloric acid (HCl).
and appropriate for organic carbon (example: After preservation, the samples should be stored at
polyether- sulfone filter). Organic carbon samples are a temperature between 6oC and 0oC, but must not be
collected allowed to freeze. Semi-volatile organic samples have
in 40 mL VOA vials and are preserved with two drops a 14 day holding time to extraction and 28 days to
of H SO . Vials should be filled leaving no headspace
analysis. These samples are used for the determination
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of semi-volatiles and chlorophenols by EPA Method
and need to be kept at or below 6oC. Labels should be See project-specific SOP for proper purging of the
clearly marked with preservation and filtration. Sam- well. Radon samples are collected in a 125 mL glass
ples that have been properly preserved and stored bottle with a Teflon-lined cap. The sample is taken from
have a holding time of 28 days. TOC/DOC are a non-aerated connection to the well and should
analyzed by EPA Method 415.3 (TOC analyzer).
While dissolved inorganic carbon (DIC) is not
an organic carbon, it falls under this section as it
is analyzed with the DOC/TOC method.
Inorganic
carbon is defined as the carbon in any carbon-contain-
ing compound that purges from water that has been
acidified. This carbon purges as carbon dioxide (CO2)
and includes metal carbonates, metal bicarbonates,
and dissolved carbon dioxide. DIC samples are
filtered through a 0.45 μm pore diameter membrane
filter and collected in 40 mL VOA vials. Vials should
be filled leaving no headspace, however; these
samples are NOT preserved with acid. Vials should be
kept at or below 6oC. Samples that have been properly
sampled and stored have a holding time of 28 days.
DIC are analyzed by EPA Method 415.3 (TOC
analyzer).

Sample Handling for Radon

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 Jacqueline
Timmer
528 (GCMS).

SAMPLE ACCEPTANCE
Prior to sample delivery, samples should be en-
tered into the MBMG Groundwater Information
Center data entry portal (DATAGWIC). All data
col- lected in the field are entered, along with the
analytical services requested. All sites from which
samples are collected are assigned a GWIC
identification number (GWIC ID) which is used to
track every sample col- lected from that site
(contact GWIC staff for assistance to register your
site if it does not have a GWIC ID).
Each sample collected during a particular sampling
campaign is assigned a unique sample number by
the GWIC database (the GWIC sample ID). This
informa- tion is then passed on to the Laboratory
Information and Management System (LIMS by
Systat Software, Inc.). The group of samples is
assigned an order num- ber and the samples are
sequentially assigned a num- ber within the order.
The numbering scheme is YY- XXXXX-ZZZ,
where YY is the last two digits of the fiscal year,
XXXXX is a sequential number assigned to the
orders within a fiscal year, and ZZZ is a sequen-
tial sample number within the order.
Samples should be delivered to the MBMG Labo-
ratory, Natural Resources Building (NRB) room 103,

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 MBMG Open-File Report 729: Analytical Lab QA
Manual
located on the Montana Tech campus, 1300 W. Park
for analysis. The field identifier of the site location
St., Butte, MT 59701. MBMG Analytical Services
(GWIC ID), time and date of sampling, and identity of
are only available to researchers within the MBMG,
the sampler are all included.
researchers from other State and Federal agencies
collaborating on MBMG projects, or faculty and Organic samples do not go into LIMS and are
student researchers within the MUS system. Instruc- tracked using the GWIC sample ID within the given
tions for submitting samples are given at the time order number of a job. Job numbers are sequentially
sampling supplies are picked up. Field personnel are incremented.
made aware that the samples should arrive in a timely
manner, packed in coolers with ice to maintain a tem- When the samples are logged in, a separate label
perature of less than 4°C throughout the storage time, is affixed to the bottle indicating the GWIC sample
and protected from damage and freezing. Further, any ID. A sample log is generated from DATAGWIC
material shipped by common carrier must comply with and an extraction sheet is created in Excel. The
DOT rules regarding hazardous substances. When extraction sheet is used to document the date of each
shipping coolers, it is preferable to use coolers that step in the operation (extraction, evaporation, and
do not have a drain to avoid leakage from melting ice analysis).
during shipping. If the cooler has a drain, tape should
be placed over the drain on both the inside and the SAMPLE PREPARATION
outside to attempt to prevent leakage during shipping.
Inorganic
Samples requiring chain of custody documentation Determination of dissolved concentrations requires
must be delivered in person with a completed MBMG no additional preparation prior to introduction to the
COC Form, a chain of custody form identical to its instrument(s), other than dilution (when necessary).
Environmental Protection Agency (EPA) counterpart. The dilution schedule is based on the specific conduc-
The samples must be released into the custody of lab- tance of the sample and dilutions are performed by
oratory personnel by obtaining a signature from a lab- mass using disposable tubes and pipette tips.
oratory representative. The laboratory will retain the
white copy of the COC form and return the yellow and Radon samples need to dark-equilibrate prior to
pink copies to the submitter as proof of transfer. The analyzing. This simply consists of adding an aliquot
majority of MBMG programs/projects do not require of sample to the ‘cocktail’ and allowing it to sit in the
a COC; the information entered into DATAGWIC is instrument (in the dark) for 3 hours before starting
usually sufficient. Samplers should refer to the project analysis. Due to radon’s short half-life (3.8 days), this
SOP/SAP for specifics. 3 hour equilibration time needs to be taken into ac-
count when calculating the holding time.
SAMPLE LOGIN
Samples that are to be analyzed for water isotopes
Inorganic should be filtered in the field. If for some reason they
were not, and/or there is visible debris, they will need
After samples are received (and have been entered to be filtered in the laboratory prior to introduction to
into DATAGWIC and LIMS), they are sorted into sets the instrument.
of bottles corresponding to the samples within the
order. Labels with the LIMS order and sample number Total recoverable metals and trace elements re-
are attached and samples are stored in the designated, quire digestion in accordance with the specifications
refrigerated sample bank. The analytical parameter of EPA Method 200.2 (Sample Preparation Procedure
request is automatically populated in the LIMS and for Spectrochemical Determination of Total Recover-
the appropriate methods activated. able Elements). The same digestion is used for EPA
Method 200.7 (Determination of Metals and Trace
Organic Elements in Water and Wastes by Inductively Cou-
The organic login is also initiated electronically pled Plasma-Atomic Emission Spectrometry) and
in DATAGWIC. A job order is generated listing the EPA Method 200.8 (Determination of Trace
information about each sample that will be submitted Elements in Waters and Wastes by Inductively
Coupled Plas-
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 Jacqueline
ma-Mass
Timmer Spectrometry). The digestions are carried
out in a block digester using acid-washed disposable
poly-

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Manual
propylene tubes. In accordance to EPA Method 200.2, The only samples that are entered into long-term
a method blank, a laboratory control sample (LCS), storage are metals (FA and RA) samples. These sam-
a method duplicate, and a laboratory fortified sample
(spike) are included for each batch of 20 samples.

Organic
Water samples (1L, acidified with HCl)
containing semi-volatile organic compounds are
subjected to sol- id phase extraction (SPE) cartridges.
Once the sample has been ‘loaded’ on the cartridge,
the cartridges are dried by pulling air through them
with a vacuum.
The cartridges are then eluted with dichloromethane
and run through a drying cartridge of sodium sulfate.
Samples are then evaporated to 1.0 mL. The dichloro-
methane eluate is spiked with internal standards and
analyzed by Method 528.
Glassware, such as evaporator tubes, are washed in
a Labconco dishwasher, run through a second cycle on
a ‘rinse’ setting that has a 30 minute dry time, and
then rinsed with pesticide-grade acetone.

SHORT-TERM SAMPLE STORAGE

Inorganic
Acidified samples (FA and RA) for metals are
stored in the secure storage area in NRB 103A of the
Natural Resources Building.
Raw Unacidified (RU), Filtered Unacidified (FU),
and Filtered Acidified Nutrients samples are stored
under refrigeration at 4oC until analysis is complete.
Samples are stored in rooms 103A, 104A, and 106,
respectively. These samples may be retained for up
to 2 months beyond the method-specific holding time
before they are disposed of.

Organic
Preserved samples are stored (refrigerated at
4oC) in NRB 106. The entire aliquot of sample for
SVOC is used during extraction. Empty sample
bottles are rinsed and disposed of. DOC samples
have limited sample remaining after analyses due to
the number of replicates required by the method.
The remaining
sample is not suitable to analyze again due to the large
volume of headspace.

LONG-TERM STORAGE

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 Jacqueline
Timmer
ples are archived
for a period of 5 years in secure Other equipment is maintained in-house according to
storage in NRB 113. the manufacturer’s recommendations. Consumable
items, such as gas filters, are changed annually or
SAMPLE ANALYSIS
Samples are analyzed by EPA-approved
methods for parameters listed in table 2. Method
detection lim- its are determined quarterly.

DATA ACQUISITION AND

REPORTING
Methods are set up in instrument software such
that the reports are produced in formats compatible
with importation into spreadsheets. Data from every
instrument are exported to an Excel spreadsheet
where the data can then be imported into the LIMS
software. Quality assurance review is conducted to
ensure that QA samples (continuing calibration
verification, CCV; initial calibration verification,
ICV; LCS; blanks, etc.) meet acceptable recoveries
within the spreadsheet. In cases where analytical
runs have QA samples that are outside the
acceptable limits, samples are designated for
reanalysis.
Final qualified analytical results are exported to
the GWIC database by LIMS. Reports can be
obtained on the web at
http://mbmggwic.mtech.edu/. The user must know
the specific identifier number (GWIC ID) or the
location of the site to access the report.
Raw data files are archived electronically on
the MBMG lab server, which is backed up daily.

OUTSIDE EVALUATION
PROGRAMS
The MBMG Laboratory maintains certification
under the drinking water program administered by
the MTDPHHS Environmental Laboratory. The
laborato- ry also participates in the water supply
performance evaluation programs administered by
Environmental Resource Associates (ERA), and in
the United States Geological Survey (USGS)
Standard Reference Sam- ple Project (SRS).

PREVENTIVE MAINTENANCE
The analytical equipment employed by the
MBMG are given in table 2. The spectrometric
equipment items are covered under service contracts
(table 2).
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Table 2. Equipment routinely used by MBMG istered by the MTDPHHS. Laboratories that
Laboratory.
hold this certification have met strict quality
Instrument Service requirements and have the authority of the
Contract Thermo iCAP 6000 ICP-OES Yes MTDPHHS to analyze and submit data that
Thermo iCAP Q ICP-MS Yes can be used to determine compliance with
State and Federal regulations. Certification is
Metrohm 882 IC Plus Anion Chromatograph a Yes
maintained through the MTDPHHS Environ-
Metrohm 882 IC Plus Anion Chromatograph b Yes mental Laboratory for the analytes listed in
Metrohm 855 Robotic Titrator Yes table 3.
Thermo ISQ 7000 GC-MS Yes
Quality Control Protocol
Agilent 6890N GC/ECD No
Agilent 6890N/5973N GC/MS with SIM/SCAN No All analyses are subject to the quality
assurance guidelines of the EPA or USGS
Picarro L2130-i Isotopic Water Analyzer
method under which the samples are ana-
lyzed. Table 4 summarizes the QA samples
No Picarro G2131-i 13C High-Precision Isotopic that are included in every analytical proce-
Carbon Dioxide (CO2) analyzer No
13
dure and their respective acceptance criteria.
Costech Combustion Module (for C Second-source standards (purchased from a
analyses of solid samples) No
different vendor than those used to make the
Hidex 300SL Auto TDCR Radon Analyzer No calibration standards) are used as ICV in all
Hach DR 3800 Spectrophotometer No methods. Samples used as LCS originate with

sooner if use of the equipment is higher than normal.

Analytical balances are calibrated annually by Quality The MBMG Analytical Laboratory maintains
Control Services, Inc. of Portland, OR. certification under the drinking water program admin-

Waste Disposal
All wastes, including samples, standards, and
diluents are disposed of in accordance with the Chem-
ical Hygiene Plan for Laboratories (Montana Tech,
March 2010). Inorganic wastes are processed by
in-lab chemical management procedures consisting of
neutralization and addition of metal precipitants. The
liquid is decanted and analyzed prior to disposal in
the sanitary sewer. Solids are reposited in an
approved metal solid waste holding landfill. Organic
liquids are held in approved drums in a storage
facility until an annually scheduled pick-up by a
waste disposal com- pany occurs.

Chemical Inventory
The MBMG uses the Montana Tech campus
inven- tory database to track chemicals. All incoming
chemi- cals are bar coded and entered into the
database. When the material is used up, the bar coded
label is removed from the container and the reagent is
marked in the database as being disposed.

Certified Analytes
1
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 Jacqueline
the USGS Reference
Timmer Sample Program or ERA
Refer- ence Materials. The quality assurance review
process is carried out in a spreadsheet as discussed
above. The method detection limits (MDL) for the
spectroscopic methods are determined for every
analytical run and are summarized quarterly. The
estimated MDL and method reporting limit (MRL)
are then set as limits for reporting analytes in the
LIMS. For MBMG work, the MRL is considered to
be five times the MDL. Qualifi- ers are assigned to
reported concentrations in the final reports
according to QA guidelines of the EPA.
The parameters of pH, specific conductance, and
alkalinity are determined by automated methods;
therefore, it is not realistic to determine MDLs for
these analytes. The sensors are calibrated prior to
col- lection of data and rechecked after every 10
samples.

NOTE: It is important for samplers to

understand that the quality control protocol
discussed here is in reference to the laboratory and
the instrumentation used within it. Project-specific
QA/QC is defined within the SOP/SAP for each
project. This is where the sampler will find the
number/frequency of field blanks,
duplicate/triplicate samples, trip blanks, equip- ment
blanks, etc. that are required based on the specif- ic
project they are sampling for.

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Table 3. Analyte parameters and associated methods.

Method Method
Parameter EPA Method Detection Limit Units EPA Detection Limit Units
Inorganic: Metals and trace elements Method

Aluminum 200.7 0.049 mg/L 200.8 7.56 µg/L

Antimony 200.8 0.05 µg/L
Arsenic 200.8 0.06 µg/L
Barium 200.7 0.031 mg/L 200.8 0.08 µg/L
Beryllium mg/L 200.8 0.18 µg/L
Boron 200.7 0.032 mg/L 200.8 0.47 µg/L
Calcium 200.7 0.256 mg/L
Cadmium 200.8 0.05 µg/L
Chromium 200.7 0.032 mg/L 200.8 0.04 µg/L
Copper 200.7 0.036 mg/L 200.8 0.39 µg/L
Iron 200.7 0.043 mg/L 200.8 2.02 µg/L
Lead 200.8 0.15 µg/L
Magnesium 200.7 0.029 mg/L
Manganese 200.7 0.031 mg/L 200.8 0.05 µg/L
Molybdenum 200.7 0.031 mg/L 200.8 0.04 µg/L
Nickel 200.7 0.032 mg/L 200.8 0.11 µg/L
Potassium 200.7 0.315 mg/L
Selenium 200.8 0.1 µg/L
Silver 200.8 0.04 µg/L
Sodium 200.7 0.141 mg/L
Thallium 200.8 0.03 µg/L
Vanadium 200.7 0.06 mg/L 200.8 0.08 µg/L
Zinc 200.7 0.036 mg/L 200.8 0.11 µg/L
Inorganic: Anions
Bromide 300 0.01 mg/L
Chloride 300 0.1 mg/L
Fluoride 300 0.01 mg/L
Nitrite as N 300 0.01 mg/L
Nitrate as N 300 0.01 mg/L
Ortho-Phosphate as P 300 0.02 mg/L
Sulfate 300 0.5 mg/L
Inorganic: Other
pH 150.1
Alkalinity 310.1
Specific conductance 120.1
Organic
Pentachlorophenol 528.0 0.1 µg/L
modified
Dissolved / total carbon 0.25 mg/L
Organic 415.3

Other: Isotope
Radon 913.0 20.0 pCi/L
Stable water isotopes Picarro CRDS NA ‰

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 Jacqueline
Timmer

Table 4. Quality control check samples for analytical work.

QC CHECK TYPE EPA 200.7 EPA 200.8
Metals and Trace Elements Frequency Tolerance
Continuing Calibration Verification 10% ±10% ±10%
(CCV)
Continuing Calibration Blank (CCB) 10% <MDL No spec
Initial Calibration Verification (ICV) After Cal ±5% ±10%
Initial Calibration Blank After Cal <MDL <MDL
Linear Range Check Once per ±10% ±10%
Interference Check Sample- 24 hr No spec No spec
Interferents
Interference Check Sample-Analytes 24 hr No spec No spec
Laboratory Fortified Blankb 24 hr ±15% ±15%
Duplicate Sample 10% 20% RPD 20% RPD
Laboratory Fortified Matrixc 10% ±25% ±25%
Serial Dilution 10% ±10% ±10%
Laboratory Control Batch
Sample a <2.2MDL No spec
Laboratory Reagent Blank Batch
Sample
a

EPA CRDL 24 hr ±20%

Every
Internal Standards 60–125%

Anions EPA 300

Frequency Tolerance
Continuing Calibration Verification 10% ±10%
Continuing Calibration Blank 10% <MDL
Initial Calibration Verification After Cal ±10%
Initial Calibration Blank After Cal <MDL
Laboratory Fortified Blankb 24 hr. ±10%
Duplicate Sample 10% 10% RPD
Laboratory Fortified Matrixc 10% ±10%
Organic Pentachlorophenol Frequency Mid-Level Low Level
Continuing Calibration Check 10% ±50%
Continuing Calibration Blank 10% <MDL
Initial Calibration Verification After Cal ±15% ±30%
Surrogate
60–130%
Sampl
Every

a
Batch: 20 or fewer samples
b,c
Laboratory Fortified Blank and Matrix. Figure cited as deviation from 100% recovery

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