Determination of Lead and Cadmium in Lipstick

By Steven Wilson, Louisiana State University

Date Started: 03/16/14

Date Finished: 04/10/14

Date Write-up Completed: 04/29/14

Abstract: Three samples of 5 different brands of lipsticks (n=15 total samples) were microwave

digested and analyzed, using flame atomic absorption spectroscopy, to determine the amount of

lead and cadmium present. The average lead and cadmium concentrations, in parts per million

(ppm), detected for each brand were as follows. Brand #1 (475 Mauve Me) contained .038+ .01

ppm cadmium and .66+ .02 ppm lead. Brand #2 (NYC Snowcone 411) contained .0222+ .002

ppm cadmium and .3+ .2 ppm lead. Brand #3 (025 Warm Brick) contained .007+ .01 ppm

cadmium and .4+ .2 ppm lead. Brand #4 (125 Pink Petal) contained .0253+ .006 ppm cadmium

and .64+ .04 ppm lead. Brand #5 (410 Volcanic) contained .009+ .001 ppm cadmium and .4+ .2

ppm lead. These values were then compared to other lipstick studies that tested for heavy metals,

particularly lead and cadmium.

Introduction: Lipstick is a popular cosmetic used by women throughout the world. An estimated

800-900 million lipsticks are sold worldwide each year, and 80% of women are purported to be

frequent users of lipstick (1) (2). Avon, the world’s biggest cosmetics company, sells 4 lipsticks

every second (2). Unbeknownst to the consumers, however, are the trace metals within these

lipstick products. Studies partaken by the Campaign for Safe Cosmetics (CSC), Food and Drug
Administration (FDA), and other researchers have found detectable amounts of lead, cadmium,

chromium, aluminum, nickel, and other metals in lipsticks (3) (4) (5) (6) (7). The CSC analyzed

33 brands of lipsticks and found that 61% of the tested lipsticks contained lead, with values

ranging from .03-.65 ppm; 33% of the lipsticks had lead concentrations in excess of .1 ppm, the

FDA’s limit for lead in candy (3). In 2007, the FDA tested 20 lipstick brands and found that all

the samples contained lead, with concentrations ranging from .09 to 3.06 ppm (4). As a follow up

to its 2007 study, the FDA partook in a colossal investigation of lead in lipstick, testing 400

brands for lead content (4). The lead concentrations ranged from .026-7.19 ppm, with an average

of 1.11 ppm (4).

In addition to the FDA and CSC, researchers in Iran and at the University of California

Berkley (UCB) tested 50 and 8 lipsticks (plus 24 lip glosses for 32 total samples), respectively,

for heavy metals (5) (6). The Iran study had a range of .08-5.2 ppm for lead and 4.08-60.20 ppm

for cadmium (5). The UCB study found detectable amounts of lead in 75% of the tested samples,

with an average concentration of .36 ppm; it also found an average cadmium concentration of

1.16 ppm (6). Another study, conducted by researchers at Government College University in

Pakistan, found lead and cadmium levels of .286-6.2384 ppm and .2-.5 ppm, respectively (7).

The high values of lead and cadmium found in these studies are harrowing because the

acceptable daily intake (ADI) values for lead and cadmium are only .95 and .38 micrograms per

day, with a public health goal target of .2 ppb and .04 ppb (lead and cadmium, respectively) (6).

Since lead is a known neurotoxin, and cadmium is a classified carcinogen, frequent use of

lipstick products could ultimately result in serious maladies (8) (9). To verify and substantiate

the presence of heavy metals in lipsticks (lead and cadmium), this study will use flame atomic

absorption spectroscopy (faas), along with nitric acid microwave digestion, to analyze five
different brands of lipsticks: 1) Maybelline’s Color Sensational Pink Petal #125, 2) L’Oreal’s

Coulor Riche Volcanic 411, 3) NYC’s 411 Snowcone, 4) Maybelline’s 475 Mauve Me, and 5)

Cover Girl’s 025 Warm Brick.

Method (Instrument Use): A Varian atomic absorption apparatus was used in conjunction with a

MARSX microwave (images shown below) to complete the experiment. To begin, a standard

amount of sample, 1-2 grams, is accurately weighed on an analytical balance and transferred to a

digestion tube. A diluted solution (1:100 dilution) of concentrated nitric acid (16.4 M) is then

added to the tube to commence the liquefaction of the sample. After the addition of nitric acid,

the digestion tubes are tightly screwed shut and taken to the MARSX microwave to complete the

sample digestion process. The microwave contains 6 spots for sample insertion and uses a high

temperature, typically 80-100 degrees Celsius, for a prolonged period of time, usually 10-30

minutes, to dissolve the solid into a liquid. With the sample fully liquefied, it is now ready for

analysis by means of faas with the Varian spectrometer (10).

The Varian atomic absorption apparatus consists of an air-acetylene gas tank, an

aspirator, a nebulizer, a flame, hollow cathode lamps (specific for each element), and a computer

program called spectraAA (11). Before sample measurements begin, an existing method for the

element to be analyzed is opened up in the spectraAA program. The hollow cathode lamp

corresponding to that element is then inserted into the lamp holder compartment of the Varian

spectrometer (11). After the lamp insertion, the optimize button is clicked on the spectraAA

program to bring the spectrometer to the proper wavelength: 228.8 nm for cadmium and 283.3

nm for lead (12). Once completed, the gas tank is turned on to supply the energy needed to ignite

the flame (11); the flame is then ignited by pressing the black button (has a picture of a flame
next to it) on the spectrometer. With the flame ignited, a blank is then used to zero out the

spectrometer (11) (13). The target samples are now ready for analysis.

Measurements from the Varian Atomic Absorption are obtained by placing the aspirator

within the liquid sample (usually in a cup) (11) (13). The aspirator sucks up the sample and sends

it into the nebulizer, which transforms the simple into an aerosol spray (fine mist) (11) (13) (14).

Next, the flame’s high temperature (2100-2400 degrees Celsius) atomizes the sample (turns them

into gaseous atoms) (11) (13) (14). The newly created atoms then absorb light at their

characteristic wavelength, which corresponds to the wavelength of the hollow cathode lamp (The

hollow cathode lamp is designed to set the spectrometer to the wavelength that represents each

element’s maximum absorbance.) (11) (13) (14). The detector measures this absorbance and

gives off an output signal that is transduced into a readable form on the computer spectraAA

program (11) (13) (14). The concentration of the sample can then be deduced from Beer’s Law,

which states that there is a linear relationship between the measured absorbance of a sample and

its concentration (14).

From the Beer’s Law absorbance-concentration relationship, several standards of different

concentrations (ppm) of lead and cadmium will be made, and subsequently have their absorbance

measured by the Varian spectrometer, to construct a linear standard calibration curve for each

element (14). The 15 samples of lipstick will then be analyzed to measure their absorbance

values. The concentration of lead and cadmium in each sample of lipstick will then be found by

solving the standard curve’s trendline equation, y=mx+b, for x, where y is the absorbance

reading of the lipstick sample, m is the slope of the trendline equation, x is the lipstick

sample’s concentration for either lead or cadmium, and b is the trendline equation’s y

intercept (14).
Figure 1: Beer’s Law (14)
Figure 2: MARSX digestion microwave

Figure 3: Varian spectrometer with aspirator shown (skinny wire) (15)

Figure 4: flame atomic absorption block diagram (13)

Figure 5: flame atomic absorption alternate block diagram (16)

Figure 6: Complete flame atomic absorption apparatus (hollow cathode lamps, spectraAA

program, spectrometer, and gas tank) (17)

Experimental Procedure:

1. Weigh 1-2 grams of lipstick sample

2. Create nitric acid stock solution (1:100 HNO3) and prepare lipstick
samples for microwave digestion

3. Perform microwave
digestion

4. Pour contents, while in a fume hood, into separate stock reagent

containers

5. Make standard solutions for cadmium and lead

6. Prepare spectrophotometer for analysis for each element's standard

solutions and lipstick samples

7. Analyze each element's solutions along with the lipstick

unknowns

8. Make standard calibration curves for each element

9. Find the concentration of each element in the lipstick samples

1) The amount of lipstick weighed for each brand is shown in the table below.

Lipstick Brand Amount weighed (g) with uncertainty (g)

1. 475 Mauve Me 1) 1.7886+ .0005 2) 1.1329+ .0005

3) 1.3633+ .0005
2. 411 Snowcone 1) 1.4537+ .0005 2) 1.2198+ .0005

3) 1.3590+ .0005
 3. 025 Warm Brick 1) 1.1137+ .0005 2) 1.108+ .0005

3) 1.5296+ .0005
4. 125 Pink Petal 1) 1.1445+ .0005 2) 1.1372+ .0005

3) 1.0761+ .0005
5. 410 Volcanic 1) 1.2919+ .0005 2) 1.4274+ .0005

3) 1.1339+ .0005

2) A 1000 ml nitric acid stock solution, 1:100 dilution, was made by placing 100 ml of

distilled water inside a 1000 ml volumetric flask followed by 10 ml of 16.4 M nitric acid

(Always add acid.). The flask was then filled to the calibration mark with distilled water.

After making the nitric acid stock solution, the lipstick samples were transferred to

digestion tubes, and approximately 10 ml of the nitric acid was added to each tube. The

tubes were then tightly closed with a wrench and taken to the MARSx microwave to

complete the digestion process.

3) Digestion was attempted 3 times with the MARSx microwave at the following

temperatures: 175, 80, and 100 degrees Celsius. The first digestion attempt had to be

stopped because of an insufficiently sealed digestion tube; this temperature was also

found to be too high for instrumental purposes, as noted by the teaching assistant. The

second digestion attempt at 80 degrees Celsius did not fully digest the samples, as solid

lipstick was still found in most of the digestion tubes. A third and final attempt at 100

degrees Celsius managed to liquefy enough of the lipstick samples so that analysis was

possible. For each digestion, the MARSx was operated according to the following

protocol. On the home screen, the edit button was selected, followed by create new

method. From the new user directory menu, the vessel type was selected (Omni XP 1500)
 along with the power (800 W, 100%), pressure (8000 psi), temperature (175, 80, 100 for

each attempt), and digestion time (10 minutes for ramping, 30 minutes at specified

temperature, and 10 minute cool down). (10)

4) After the microwave finished digesting the samples, the tubes were placed inside the

fume hood and opened; once all the pressurized gas fumes had disappeared, the digestion

tube contents were then filtered, using Whatman filter paper, into stock reagent bottles

and stored for later use.

5) Several standard solutions—0, .5, 1, 2, 3, 5, and 10 ppm—of both cadmium and lead

were made from respective 1000ppm stock solutions. The standards were made according

to the table below.

Standard Concentrations Amount of 1000 ppm lead/ Amount of distilled water

lead and cadmium (ppm) cadmium standard needed to add to reach 100 ml

(mLs) total volume (mLs)

0 0 100
.5 .05 99.95
1 .1 99.9
2 .2 99.8
3 .3 99.7
5 .5 99.5
10 1 99

6) The atomic absorption apparatus was setup to commence analysis by placing both a lead

and cadmium hollow cathode lamp inside the Varian spectrometer. Next, the air-
 acetylene gas tank was turned on to provide a fuel source for the flame (11) (13). The

standard solutions, as well as the unknown lipstick samples, were then poured into cups

and arranged in the following order: 1) 0ppm standards, 2).5 ppm standards, 3) 1ppm

standards, 4) 2 ppm standards, 5) 3ppm standards, 6) 5ppm standards, 7) 10 ppm

standards, and 8) unknowns (lipstick samples). Lastly, an already existing method for

lead and cadmium was opened in the spectraAA program (10).

7) The cadmium standard solutions were ran first, followed by the unknowns.

Measurements were taken by optimizing the cadmium lamp and then selecting calibration

on the spectraAA program. Distilled water was used for the instrument zero. After

successful blanking, the standard cadmium solutions were ran in sequential order and

immediately followed by the 15 lipstick samples. After all cadmium measurements had

been taken, this process was then repeated for lead.

8) A standard calibration curve was made for both lead and cadmium by plotting the

obtained absorbance readings vs the standard’s concentrations.

9) The concentration of cadmium and lead in the lipstick samples was found by solving the

corresponding standard curve trendline equations for x, with the y value being that

lipstick sample’s absorbance reading.

Results:

Table 3: Cadmium and Lead standard Absorbance readings

Cadmium Cadmium Lead standards Lead standards

 standards (ppm) standards (ppm) absorbance

absorbance readings

readings
0 -.003 0 .0019
.5 .0858 .5 .0101
1 .1702 1 .0193
2 .3211 2 .0363
3 .4569 3 .0536
5 .6724 5 .0885
10 .9765 10 .167

Graph 1: Cadmium Standards

Graph 2: Lead Standards

Table 4: Lipstick Sample Absorbance Readings for Cadmium and Lead

Cadmium Absorbance values Lead Absorbance values

a. 475 Mauve Me: 1) .0142 2) .015 a. 475 Mauve Me: 1) .0137 2) .0142

3) .0113 3) .0138
b. 411 Snowcone: 1) .0115 2) .011 b. 411 Snowcone: 1) .0036, 2) .01

3) .0108 3) .0118
c. 025 Warm Brick: 1) .0073 2) .0118 c. 025 Warm Brick: 1) .0085 2) .0135

3) .0072 3) .0066
d. 125 Pink Petal: 1) .0123 2) .0106 d. 125 Pink Petal: 1) .0134 2) .0142

3) .0118 3).0128
e. 410 Volcanic: 1) .0093 2) .0089 3) . e. 410 Volcanic: 1) .0078 2) .0125 3) .

009 0063

Table 5: Lipstick Sample concentrations

 Cadmium Average Cadmium Lead Average Lead

concentration concentration concentration(ppm) concentration

(ppm) (ppm) (ppm)

a. 475 Mauve Me: a. 475 Mauve Me: a. 475 Mauve Me: a. 475 Mauve Me:

1) .0426 2) .0481
.04+ .01 1) .6506 2) .6807 3) . .66+ .02
3) .0236
6566
b. 411 Snowcone: b. 411 Snowcone: b. 411 Snowcone: b. 411 Snowcone:

1) .0249 2) .0216
.022+ .002 1) .0421 2) .4277 3) . .3+ .2
3) .0203
5361
c. 025 Warm c. 025 Warm c. 025 Warm Brick: c. 025 Warm

Brick: 1) -.0026 2) . Brick: .007+ .02 Brick: .4+ .2

1) .3373 2) .6386 3) .
0269 3) -.0033
2229
d. 125 Pink Petal: d. 125 Pink Petal: d. 125 Pink Petal: d. 125 Pink Petal:

1) .0301 2) .0189
.025+ .005 1) .6325 2) .6807 3) . .64+ .04
3) .0269
5964
e. 410 Volcanic: 1) . e. 410 Volcanic: . e. 410 Volcanic: e. 410 Volcanic:

0104 2) .0078 3) . 009+ .001

1) .2952 2) .5783 3) . .4+ .2
0085
2048

Table 6: Detection Limits

Cadmium detection limit (ppb) Lead detection limit (ppb)

.8 15
(11) (11)
Graph 3: All 15 lipstick samples’ cadmium concentrations
Graph 4: All 15 lipstick samples’ lead concentrations

Discussion: Detectable amounts of both cadmium and lead were found in all 5 brands of

lipstick. The cadmium concentrations ranged from .007-.04 ppm (detection limit .8ppb and

range given used average concentrations), and the lead concentrations ranged from .3-.66

ppm (detection limit 15 ppb and range given used average concentrations) (11). Due to the

small amount of cadmium present in the lipsticks, the cadmium standard curve was adjusted

to only include up to the 3 ppm standard. The standard curves for each element were highly

linear, with R2 values of .99.

The lead concentrations were consistent, overlapped, with the CSC, UCB, Iran, and

Government College studies, but they were lower than the FDA’s average value of 1.11 ppm
(3) (4) (5) (6). Unlike lead, the cadmium values were significantly lower than the

aforementioned studies’ values of .2-.5 ppm (Government College researchers), 1.16 ppm

(UCB), and 4.08-60.20 ppm (Iran researchers) (5) (6) (7). These differences can likely be

attributed to poor sample digestion and the usage of a less sensitive analytical technique,

faas, instead of inductively coupled plasma mass spectrometry (ICP-MS) or graphite furnace

atomic absorption spectroscopy (11) (18). All of the studies that registered much higher

concentration values for lead and cadmium used ICP-MS for analysis (advantages shown in

the figures below), with the exceptions being the Iran and Government College studies

(graphite furnace and faas, respectively) (3) (4) (5) (6) (7). The superiority of ICP-MS was

clearly shown with the lipstick Pink Petal #125, the sample that registered the highest lead

concentration in the FDA’s 400 lipstick experiment (7.19 ppm) (4). Despite the low

concentrations for cadmium and lead, the experiment can be considered a success since it

proved that trace metals are in lipstick products.

 Figure 7: Detection limits for FAAS, Graphite Furnace, and ICP (shows the greater

sensitivity of ICP-MS) (11)

Figure 8: Comparison of analytical methods (Graphite Furnace and ICP-MS have

fewer interferences and better operational capabilities.) (11)

 Figure 9: Alternate analytical comparison diagram (18)

Conclusion: The trace metals cadmium and lead were detected in 5 different brands of

lipstick by means of faas. The cadmium concentration levels were lower than other

experimental results, but the lead concentration levels had greater overlap with other

experimental studies (3) (4) (5) (6) (7). Although faas did measure cadmium and lead in the

tested lipsticks, better results could have been obtained by using either ICP-MS or graphite

furnace atomic absorption (11) (18).

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