How to Avoid
Contamination When
Using ICP-MS
Inorganic Product Specialist
陳麗真 Jennifer Chen
Definition of Contamination
• An unwanted, detectable enhancement of
the background signal caused by an agent
which may interfere with the measurement
of an analyte of interest
Page 2
Do You Have a Contamination Problem?
¾ Reporting negative answers for blanks
¾ Run blanks and compare results
• Different sources of water
• Different sources of acids
• Different samples and sampling vessels
• Different analysts
¾ Run blanks exposed to laboratory
environment over time
• Checks cleanliness of laboratory environment
and the instrument
Page 3
Sources of Contamination (Sampling the Raw Sample)
¾ Sampling Equipment
¾ Sampling Environment
¾ Sample Bottles/Sample Storage
¾ Sample Transport
¾ Sampling Personnel
¾ Preservation Reagents
Page 4
Sources of Contamination (Post-sampling)
¾ Analytical Containers (flasks, pipettes,..)
¾ Storage Containers
¾ Lab Reagents (including lab pure water)
¾ Lab Environment
¾ Analyst
¾ Instrumentation (carry-over)
Page 5
Sources of Contamination - Glass Vessels and Volumetric Flasks
¾ NEVER USE THEM!!
¾ DO NOT USE for storage!
¾ DO NOT USE for dilutions!
¾ DO NOT USE for Preparing
Standards
¾ NEVER USE FOR DISSOLUTION
OR DIGESTION
USE A BALANCE TO MAKE STANDARDS
AND PERFORM DILUTIONS
Page 6
Sources of Contamination - Glass Pipettes
NEVER USE GLASS
PIPETTES!!
¾ Use Pipettors with disposable tips whenever
possible
¾ Use Separate Pipette Tips for Each Solution
¾ Take Care Not to Contaminate the Tips
During Use
¾ Pour Samples, Standards and Reagents Into
Secondary Containers Before Pipetting
Page 7
How clean are your pipettes?
2% Nitric acid run through 5ml pipets and scanned on ICPMS
Element Conc. PPB Detection limit Element Conc. PPB Detection limit
AG 2.33 0.0088 MN 1.72 0.012
AL 6.43 0.13 NA 19.1 0.6
BE 2.62 0.007 NI 0.96 0.18
BI 1.07 0.0006 PB 5.4 0.13
CA 18.8 2.9 SN 0.55 0.0033
CO 2.02 0.004 TH 0.24 0.0003
CR 0.91 0.28 TI 0.56 0.003
FE 1.62 0.75 TL 1.53 0.0075
MG 2.56 0.016 ZN 9 0.4
Page 8
Acceptable Levels of Contamination
¾ What do you want to get from your ICP-MS?
• The answer to this question determines the level
of acceptable contamination
• What level of contamination reduction is
necessary to achieve your analytical goals
¾ Detection limits are limited by contamination
• Routine analyses (i.e. Environmental)
• Clean - low level analyses (i.e. Semiconductor)
Page 9
Laboratory Pure Water
Water is the major component of aqueous
standards and samples. Its contribution to the overall quality of
the sample and standard is considerable.
Contaminants in water
• Dissolved, ionic solids eg. sodium chloride and calcium carbonate
present as minerals in water
• Dissolved non-ionic solids or pyrogens from organic matter formed as
a result of exposure to biologicals
• Particulate matter : Dirt, rust, sand, dust etc.
• Microbials : Bacteria, viruses, etc
Page 10
Laboratory Pure Water
RO SYSTEM
•Meets ASTM Type III water
standards
•Carbon filtration
•Reverse osmosis
•Meets ASTM Type I or Type II water
POLISHING SYSTEM standards
•Carbon filtration
•Deionization
•Organic adsorption
•Ultrafiltration
•Ultraviolet Exposure (ASTM Type I)
Page 11
ASTM Water Specifications
ASTM Type I II III IV
Total matter <0.1 0.1 1 2
(mg/L max.)
Specific Resist. 15-18 1 >1.0 0.2
(megohm, min)
pH NA NA 6.2-7.5 5-8
Min. color retention time of 60 60 10 10
KMnO4 mins
Soluble Silica ND ND 10ug/l high
Bacteria Count 0/ml 0/ml 10/ml 100/ml
Page 12
Routine Trace Metals Analysis - Work Station
¾ This Purifier Trace Metals Work Station is
designed specifically for the demands of
trace metals analysis of environmental
samples included EPA Method 1631
Mercury in Water
¾ Total exhaust vertical clean bench
provides a Class 100 particulate-free and
metal-free work environment
¾ All components in the HEPA-filtered air
stream are non-metallic including the
work area, which is PVC and tempered
safety glass
¾ Applications involving corrosive
chemicals such as acid digestions are
well-suited to this enclosure
¾ Provides personnel and product
protection from background
contamination
Page 13
Routine Analysis – Nebulizers and Spray Chambers
Sample Introduction
Common Materials
¾ Glass
¾ Quartz
O Nebulizers
¾ Ryton
O Spray
Chambers
17 abcti
Page 14
Routine Analysis – Nebulizers
¾ Cross - flow
¾ Meinhard
Page 15
Routine Analysis - Meinhard Nebulizer
¾ Cleaner solutions (Usually <1%
TDS)
¾ Best Precision and Detection
Limits
• 0.5% Precision
• D.L. 40 % lower than cross-
flow
¾ Can be run without pump (self-
aspiration)
¾ Susceptible to clogging
Page 16
Routine Analysis - Spray Chambers
¾ Scott - Type Double Pass Chamber
¾ Cyclonic Spray Chamber
¾ Baffled Cyclonic Spray Chamber
Page 17
Routine Analysis – Ryton Scott Style Spray Chamber
¾ Separates the small droplets
(<10 microns) from the larger
droplets Scott Spray Chamber
¾ Small droplets travel through
center tube, large droplet drop
out of center tube and into the
drain
¾ 2 - 4% efficient
¾ Durable and inert
¾ Cleaned with 10-20% warm not
boiling HNO3
18 HI
¾ Can run most any solvent
Page 18
Routine Analysis - Cyclonic Spray Chamber
¾ Very efficient Sample Introduction
• 40% higher efficiency
than a Scott-Type
¾ Excellent Rinse-out
¾ Detection limits improve by
a factor of 2 over a Scott-
Type
¾ Clean with hot mineral acids
¾ Precision worse than a
Scott-Type (1%)
17 abcti
Cyclonic Spray Chamber
Page 19
Routine Analysis - Baffled Cyclonic Spray Chamber
¾ Cyclonic spray chamber has fast
rinse out will little memory affects
¾ Baffle reduces effiency, but
increases precision and reduces
oxides
¾ Detection limit comparable with
Scott; maybe 10 % lower
¾ Allows for the running of volatile
solvents
Page 20
Routine Analysis - Acids and Standard Solutions
AAS grade acids and standard solutions contain impurities.
High purity acids and standard solutions must be used for ICP-MS.
¾ Fisher Scientific International Inc.
[Link]
¾ Cole Parmer
[Link]
¾ SPEX
[Link]
¾ High Purity Standard
[Link]
Page 21
Routine Analysis – Some Suggestions to Reduce/Avoid
Contamination
¾ Very difficult to determine 20 or more elements at ICP-MS detection
limits without contamination
¾ Do as much preparation in plastic or Teflon as possible
• Rinse with 1% nitric acid and keep nitric acid in them until
used
• Use once and discard or rinse with nitric acid (1%) or high
purity water and store until used
• Use Eppendorf® - type pipettes or automatic diluter
¾ Do dissolution in metal-free clean hood if contamination is a problem
¾ Use high purity acids when possible
¾ Best results when dilutions are done on a balance (weight/weight)
Page 22
Routine Analysis – Some Suggestions to Reduce/Avoid
Contamination
¾ Water – ASTM Type II (18 megohm) or better**
** ASTM Type I for Clean – Ultra low level analyses
¾ Acids, other reagents
• Cleanest are NH4OH and HNO3
• Dirtiest are HCl and NaOH
¾ Containers
• Glassware: B, Si, Na, and half the periodic table
• Polyethylene: Sn, Ba
• Teflon: Fe
• Polypropylene: best
Page 23
Clean - Class 100 Work Station
¾ 99.99% efficient HEPA filter
¾ Class 100 air (ISO Class 5
conditions)
¾ Corrosion-resistant PVC interior, air
foil and work surface
¾ Exterior of epoxy-coated steel and
aluminum
¾ Designed for ducting to the outside
¾ Tempered safety glass sides and
angled pivoting sash
¾ Filter condition indicator
¾ Fluorescent lighting
Particle-free Class 100 air (fewer than 100 particles 0.5 µm or larger per cubic foot of air)
Page 24
Clean Laboratory
• Environment of class 100 (less than 100 particles of 0.5
microns per m3)
• Walls, ceilings and floors sealed and dust free
• HEPA filters mounted in the ceiling
• No exposed metal parts
• All work performed under clean hood
• Exposure of Samples and Standards to air is limited
Page 25
PFA Volumetric Flasks and Pipette Tips
¾PFA Volumetric Flask
¾Contamination comes from the cap and mouth.
¾The mouth of volumetric flask is too small.
¾Solution touches the cap while mixing, this is unavoidable.
A wide mouth PFA bottle is recommended.
¾Pipette Tips
¾Most pipette tips have coating to allow better delivery of solution.
Can also contaminate solution!
¾Colorless polypropylene tips can be used for sampling of
standard solution, but not good for pure chemicals.
¾PFA tip is available from ESI.
¾Pipettors with a stainless steel plunger might be corroded by acid.
DON’T USE THEM!
Page 26
Impurities in Container Materials
Material Total No. of Total Major
Elements PPM Impurities
Polystyrene-PS 8 4 Na,Ti, Al
Teflon-TFE* 24 19 Ca,Pb,Fe,Cu
Teflon-FEP* 25 241 K,Ca,Mg
Polycarbonate-PC 10 85 Cl,Br,Al
Low Density PE-LDPE 18 23 Ca,Cl,K
Polypropylene-PP 21 519 Cl,Mg,Ca
Polymethyl Pentene-PMP 14 178 Ca,Mg,Zn
High Density PE-HDPE 22 654 Ca,Zn,Si
Borosilicate Glass 14 497 Si,B,Na
*TFE-Tetrafluoroethylene
*FEP=FluorinatedEthylenePropylene
Page 27
Cleaning Procedure
1. Soak in (1+1) HCl for one week.
2. Soak in (1+1) HNO3 for one week.
3. Heat with the chemical to be used for three hours
(under the boiling point of chemical)
4. Heat with UPW for three hours (under the boiling point).
pThis PFA bottle was
cleaned by the above
procedure.
pIt was used for pre-
concentration of HF.
pIt still took 14 runs to
eliminate the
contamination from the
bottle.
Page 28
Clean Acids and Standard Solutions
Two companies guaranty impurity level better than 10 ppt:
Tama Chemical
[Link]
Kanto Chemical
[Link]
AAS grade single standard solution contain impurities.
High purity standard solutions must be used for ICP-MS.
SPEX
[Link]
High Purity Standard
[Link]
Page 29
Clean Techniques – Analyst Procedures
• No jewelry, cosmetics or lotions
• Wear gloves, but No Powder
• Cover hair and mouth
• Protect samples and standards from dust,
airborne particles and fibers
Page 30
Conclusion
How do you determine how clean your lab is?
RUN A SERIES OF BLANKS!!!
Page 31
